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Sample records for liquid extraction ple

  1. Optimisation of pressurised liquid extraction (PLE) for rapid and efficient extraction of superficial and total mineral oil contamination from dry foods.

    Science.gov (United States)

    Moret, Sabrina; Scolaro, Marianna; Barp, Laura; Purcaro, Giorgia; Sander, Maren; Conte, Lanfranco S

    2014-08-15

    Pressurised liquid extraction (PLE) represents a powerful technique which can be conveniently used for rapid extraction of mineral oil saturated (MOSH) and aromatic hydrocarbons (MOAH) from dry foods with a low fat content, such as semolina pasta, rice, and other cereals. Two different PLE methods, one for rapid determination of superficial contamination mainly from the packaging, the other for efficient extraction of total contamination from different sources, have been developed and optimised. The two methods presented good performance characteristics in terms of repeatability (relative standard deviation lower than 5%) and recoveries (higher than 95%). To show their potentiality, the two methods have been applied in combination on semolina pasta and rice packaged in direct contact with recycled cardboard. In the case of semolina pasta it was possible to discriminate between superficial contamination coming from the packaging, and pre-existing contamination (firmly enclosed into the matrix). Copyright © 2014 Elsevier Ltd. All rights reserved.

  2. The loss of essential oil components induced by the Purge Time in the Pressurized Liquid Extraction (PLE) procedure of Cupressus sempervirens.

    Science.gov (United States)

    Dawidowicz, Andrzej L; Czapczyńska, Natalia B; Wianowska, Dorota

    2012-05-30

    The influence of different Purge Times on the effectiveness of Pressurized Liquid Extraction (PLE) of volatile oil components from cypress plant matrix (Cupressus sempervirens) was investigated, applying solvents of diverse extraction efficiencies. The obtained results show the decrease of the mass yields of essential oil components as a result of increased Purge Time. The loss of extracted components depends on the extrahent type - the greatest mass yield loss occurred in the case of non-polar solvents, whereas the smallest was found in polar extracts. Comparisons of the PLE method with Sea Sand Disruption Method (SSDM), Matrix Solid-Phase Dispersion Method (MSPD) and Steam Distillation (SD) were performed to assess the method's accuracy. Independent of the solvent and Purge Time applied in the PLE process, the total mass yield was lower than the one obtained for simple, short and relatively cheap low-temperature matrix disruption procedures - MSPD and SSDM. Thus, in the case of volatile oils analysis, the application of these methods is advisable. Copyright © 2012 Elsevier B.V. All rights reserved.

  3. Essential oils (EOs), pressurized liquid extracts (PLE) and carbon dioxide supercritical fluid extracts (SFE-CO2) from Algerian Thymus munbyanus as valuable sources of antioxidants to be used on an industrial level.

    Science.gov (United States)

    Bendif, Hamdi; Adouni, Khaoula; Miara, Mohamed Djamel; Baranauskienė, Renata; Kraujalis, Paulius; Venskutonis, Petras Rimantas; Nabavi, Seyed Mohammad; Maggi, Filippo

    2018-09-15

    The aim of this study was to demonstrate the potential of extracts from Algerian Thymus munbyanus as a valuable source of antioxidants for use on an industrial level. To this end, a study was conducted on the composition and antioxidant activities of essential oils (EOs), pressurized liquid extracts (PLE) and supercritical fluid extracts (SFE-CO 2 ) obtained from Thymus munbyanus subsp. coloratus (TMC) and subsp. munbyanus (TMM). EOs and SFE-CO 2 extracts were analysed by GC-FID and GC×GC-TOFMS revealing significant differences. A successive extraction of the solid SFE-CO 2 residue by PLE extraction with solvents of increasing polarity such as acetone, ethanol and water, was carried out. The extracts were evaluated for total phenolic content by Folin-Ciocalteu assay, while the antioxidant power was assessed by DPPH, FRAP, and ORAC assays. SFE-CO 2 extracts were also analysed for their tocopherol content. The antioxidant activity of PLE extracts was found to be higher than that of SFE-CO 2 extracts, and this increased with solvent polarity (water > ethanol > acetone). Overall, these results support the use of T. munbyanus as a valuable source of substances to be used on an industrial level as preservative agents. Copyright © 2018 Elsevier Ltd. All rights reserved.

  4. PLE in the analysis of plant compounds. Part I. The application of PLE for HPLC analysis of caffeine in green tea leaves.

    Science.gov (United States)

    Dawidowicz, Andrzej L; Wianowska, Dorota

    2005-04-29

    A broad spectrum of sample preparation methods is currently used for the isolation of pharmacologically active compounds from plant and herbal materials. The paper compares the effectiveness of infusion, microwave assisted solvent extraction (MASE), matrix solid-phase dispersion (MSPD) and pressurised liquid extraction (PLE) as sample preparation methods for the isolation of caffeine from green tea leaves. The effect of PLE variables, such as extraction temperature, pressure and time, on the yield of caffeine from the investigated matrix is discussed. The obtained results revealed that PLE, in comparison with other sample preparation methods applied, has significantly lower efficacy for caffeine isolation from green tea leaves. The evaluation of PLE conditions leads to the conclusion that elevated pressure applied in the PLE process is the factor hindering the extraction.

  5. PLE in the analysis of plant compounds. Part II: One-cycle PLE in determining total amount of analyte in plant material.

    Science.gov (United States)

    Dawidowicz, Andrzej L; Wianowska, Dorota

    2005-04-29

    Pressurised liquid extraction (PLE) is recognised as one of the most effective sample preparation methods. Despite the enhanced extraction power of PLE, the full recovery of an analyte from plant material may require multiple extractions of the same sample. The presented investigations show the possibility of estimating the true concentration value of an analyte in plant material employing one-cycle PLE in which plant samples of different weight are used. The performed experiments show a linear dependence between the reciprocal value of the analyte amount (E*), extracted in single-step PLE from a plant matrix, and the ratio of plant material mass to extrahent volume (m(p)/V(s)). Hence, time-consuming multi-step PLE can be replaced by a few single-step PLEs performed at different (m(p)/V(s)) ratios. The concentrations of rutin in Sambucus nigra L. and caffeine in tea and coffee estimated by means of the tested procedure are almost the same as their concentrations estimated by multiple PLE.

  6. Optimization of pressurized liquid extraction (PLE) of dioxin-furans and dioxin-like PCBs from environmental samples.

    Science.gov (United States)

    Antunes, Pedro; Viana, Paula; Vinhas, Tereza; Capelo, J L; Rivera, J; Gaspar, Elvira M S M

    2008-05-30

    Pressurized liquid extraction (PLE) applying three extraction cycles, temperature and pressure, improved the efficiency of solvent extraction when compared with the classical Soxhlet extraction. Polychlorinated-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and dioxin-like PCBs (coplanar polychlorinated biphenyls (Co-PCBs)) in two Certified Reference Materials [DX-1 (sediment) and BCR 529 (soil)] and in two contaminated environmental samples (sediment and soil) were extracted by ASE and Soxhlet methods. Unlike data previously reported by other authors, results demonstrated that ASE using n-hexane as solvent and three extraction cycles, 12.4 MPa (1800 psi) and 150 degrees C achieves similar recovery results than the classical Soxhlet extraction for PCDFs and Co-PCBs, and better recovery results for PCDDs. ASE extraction, performed in less time and with less solvent proved to be, under optimized conditions, an excellent extraction technique for the simultaneous analysis of PCDD/PCDFs and Co-PCBs from environmental samples. Such fast analytical methodology, having the best cost-efficiency ratio, will improve the control and will provide more information about the occurrence of dioxins and the levels of toxicity and thereby will contribute to increase human health.

  7. Quantification of four ionophores in soil, sediment and manure using pressurised liquid extraction

    DEFF Research Database (Denmark)

    Bak, Søren Alex; Hansen, Martin; Pedersen, Kenneth Munk

    2013-01-01

    A multi-residue pressurised liquid extraction (PLE) methodology has been established for the determination of the four ionophores: lasalocid, monensin, salinomycin and narasin in solid environmental matrices. The PLE methodology is combined with solid phase extraction as clean-up using liquid...

  8. Pressurized liquid extraction of ginger (Zingiber officinale Roscoe) with bioethanol:

    DEFF Research Database (Denmark)

    Hu, Jiajin; Guo, Zheng; Glasius, Marianne

    2011-01-01

    To develop an efficient green extraction approach for recovery of bioactive compounds from natural plants, we examined the potential of pressurized liquid extraction (PLE) of ginger (Zingiber officinale Roscoe) with bioethanol/water as solvents. The advantages of PLE over other extraction...... approaches, in addition to reduced time/solvent cost, the extract of PLE showed a distinct constituent profile from that of Soxhlet extraction, with significantly improved recovery of diarylheptanoids, etc. Among the pure solvents tested for PLE, bioethanol yield the highest efficiency for recovering most...... constituents of gingerol-related compounds; while for a broad concentration spectrum of ethanol aqueous solutions, 70% ethanol gave the best performance in terms of yield of total extract, complete constituent profile and recovery of most gingerol-related components. PLE with 70% bioethanol operated at 1500...

  9. Extraction of functional ingredients from spinach (Spinacia oleracea L.) using liquid solvent and supercritical CO₂ extraction.

    Science.gov (United States)

    Jaime, Laura; Vázquez, Erika; Fornari, Tiziana; López-Hazas, María del Carmen; García-Risco, Mónica R; Santoyo, Susana; Reglero, Guillermo

    2015-03-15

    In this work three different techniques were applied to extract dry leaves of spinach (Spinacia oleracea): solid-liquid extraction (SLE), pressurised liquid extraction (PLE) and supercritical fluid extraction (SFE) to investigate the influence of extraction solvent and technique on extracts composition and antioxidant activity. Moreover, the influence of carotenoids and phenolic compounds on the antioxidant and anti-inflammatory activities of spinach extracts was also studied. The higher concentrations of carotenoids and the lower content of phenolic compounds were observed in the supercritical CO₂ extracts; whereas water and/or ethanol PLE extracts presented low amounts of carotenoids and the higher concentrations of phenolic compounds. PLE extract with the highest content of phenolic compounds showed the highest antioxidant activity, although SFE carotenoid rich extract also showed a high antioxidant activity. Moreover, both extracts presented an important anti-inflammatory activity. PLE seems to be a good technique for the extraction of antioxidant and anti-inflammatory compounds from spinach leaves. Moreover, spinach phenolic compounds and carotenoids present a high antioxidant activity, whereas spinach carotenoids seem to show a higher anti-inflammatory activity than phenolic compounds. It is worth noting that of our knowledge this is the first time the anti-inflammatory activity of lipophilic extracts from spinach leaves is reported. © 2014 Society of Chemical Industry.

  10. Recovery of Steroidal Alkaloids from Potato Peels Using Pressurized Liquid Extraction

    Directory of Open Access Journals (Sweden)

    Mohammad B. Hossain

    2015-05-01

    Full Text Available A higher yield of glycoalkaloids was recovered from potato peels using pressurized liquid extraction (1.92 mg/g dried potato peels compared to conventional solid–liquid extraction (0.981 mg/g dried potato peels. Response surface methodology deduced the optimal temperature and extracting solvent (methanol for the pressurized liquid extraction (PLE of glycoalkaloids as 80 °C in 89% methanol. Using these two optimum PLE conditions, levels of individual steroidal alkaloids obtained were of 597, 873, 374 and 75 µg/g dried potato peel for α-solanine, α-chaconine, solanidine and demissidine respectively. Corresponding values for solid liquid extraction were 59%, 46%, 40% and 52% lower for α-solanine, α-chaconine, solanidine and demissidine respectively.

  11. Effect of pressurized liquids on extraction of antioxidants from Chlorella vulgaris.

    Science.gov (United States)

    Cha, Kwang Hyun; Kang, Suk Woo; Kim, Chul Young; Um, Byung Hun; Na, Ye Rim; Pan, Cheol-Ho

    2010-04-28

    Chlorella vulgaris is a green microalga that contains various antioxidants, such as carotenoids and chlorophylls. In this study, antioxidants from C. vulgaris were extracted using pressurized liquid extraction (PLE), which has been recently used for bioactive compound extraction. The antioxidant capacity of individual compounds in chlorella was determined by online HPLC ABTS(*+) analysis. According to the antioxidant analysis of total extracts, the extraction yield, radical scavenging activity, and phenolic compounds using PLE were relatively high compared to those obtained using maceration or ultrasound-assisted extraction. On the basis of online HPLC ABTS(*+) analysis, the 15 major antioxidants from chlorella extracts were identified as hydrophilic compounds, lutein and its isomers, chlorophylls, and chlorophyll derivatives. Using PLE at high temperature (85-160 degrees C) significantly increased antioxidant extraction from chlorella, improving the formation of hydrophilic compounds and yielding more antioxidative chlorophyll derivatives. Online HPLC ABTS(*+) analysis was a useful tool for the separation of main antioxidants from PLE extracts and allowed the simultaneous measurement of their antioxidant capacity, which clearly showed that PLE is an excellent method for extracting antioxidants from C. vulgaris.

  12. Recovery of anthocyanins from residues of Rubus fruticosus, Vaccinium myrtillus and Eugenia brasiliensis by ultrasound assisted extraction, pressurized liquid extraction and their combination.

    Science.gov (United States)

    Machado, Ana Paula Da Fonseca; Pereira, Ana Luiza Duarte; Barbero, Gerardo Fernández; Martínez, Julian

    2017-09-15

    This work investigated the extraction efficiency of polyphenols (anthocyanins) from blackberry, blueberry and grumixama residues using combined ultrasonic assisted extraction (UAE) and pressurized liquid extraction (PLE) (UAE+PLE). The performance of UAE+PLE was compared to those achieved by the isolated PLE and UAE methods and conventional Soxhlet extraction. The effects of the extraction methods and solvents (acidified water pH 2.0, ethanol+water 50% v/v and ethanol+water 70% ethanol v/v) on total phenolics content, anthocyanin composition and antioxidant capacity of extracts were investigated by a full factorial design. The extraction efficiency for total phenolics and antioxidant capacity in decreasing order was: UAE+PLE>PLE≈Soxhlet>UAE, and for anthocyanins it was: Soxhlet≈UAE>UAE+PLE>PLE, using hydroethanolic mixtures as solvents. Extractions with acidified water and ultrasound were not effective to recover phenolics. Two, four and fourteen anthocyanins were identified in the extracts from grumixama, blackberry and blueberry, respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

  13. Optimizing pressurized liquid extraction of microbial lipids using the response surface method.

    Science.gov (United States)

    Cescut, J; Severac, E; Molina-Jouve, C; Uribelarrea, J-L

    2011-01-21

    Response surface methodology (RSM) was used for the determination of optimum extraction parameters to reach maximum lipid extraction yield with yeast. Total lipids were extracted from oleaginous yeast (Rhodotorula glutinis) using pressurized liquid extraction (PLE). The effects of extraction parameters on lipid extraction yield were studied by employing a second-order central composite design. The optimal condition was obtained as three cycles of 15 min at 100°C with a ratio of 144 g of hydromatrix per 100 g of dry cell weight. Different analysis methods were used to compare the optimized PLE method with two conventional methods (Soxhlet and modification of Bligh and Dyer methods) under efficiency, selectivity and reproducibility criteria thanks to gravimetric analysis, GC with flame ionization detector, High Performance Liquid Chromatography linked to Evaporative Light Scattering Detector (HPLC-ELSD) and thin-layer chromatographic analysis. For each sample, the lipid extraction yield with optimized PLE was higher than those obtained with referenced methods (Soxhlet and Bligh and Dyer methods with, respectively, a recovery of 78% and 85% compared to PLE method). Moreover, the use of PLE led to major advantages such as an analysis time reduction by a factor of 10 and solvent quantity reduction by 70%, compared with traditional extraction methods. Copyright © 2010 Elsevier B.V. All rights reserved.

  14. The optimization of extraction of antioxidants from apple pomace by pressurized liquids.

    Science.gov (United States)

    Wijngaard, Hilde; Brunton, Nigel

    2009-11-25

    Pressurized liquid extraction (PLE) is a green extraction technique that can enhance extraction rates of bioactive compounds. PLE was used to extract antioxidants and polyphenols from industrially generated apple pomace at two different temperature ranges: 160 to 193 degrees C and 75 to 125 degrees C. Antioxidant activity (DPPH radical scavenging test), total phenol content and three individual polyphenol groups were determined. Response surface methodology was used to optimize the five response values. Maximum antioxidant activity was obtained at a temperature of 200 degrees C, but unwanted compounds such as hydroxymethylfurfural were formed. Therefore a lower temperature range between 75 and 125 degrees C is recommended. Using this temperature range, a maximum antioxidant activity was determined at 60% ethanol and 102 degrees C. By using PLE the antioxidant activity was increased 2.4 times in comparison to traditional solid-liquid extraction, and the technique may be a promising alternative to conventional techniques for extracting antioxidants.

  15. Quantification of four ionophores in soil, sediment and manure using pressurised liquid extraction

    DEFF Research Database (Denmark)

    Bak, Søren Alex; Hansen, Martin; Pedersen, Kenneth Munk

    2013-01-01

    A multi-residue pressurised liquid extraction (PLE) methodology has been established for the determination of the four ionophores: lasalocid, monensin, salinomycin and narasin in solid environmental matrices. The PLE methodology is combined with solid phase extraction as clean-up using liquid...... chromatography coupled to tandem mass spectrometry applying electrospray ionisation for detection. The samples were freeze-dried prior to extraction. The absolute recoveries for soil and sediment ranged from 71 to 123% (relative standard deviation (RSDs) below 16%) and in the range 94-133% (RSDs 9...

  16. Simultaneous analysis of organochlorinated pesticides (OCPs) and polychlorinated biphenyls (PCBs) from marine samples using automated pressurized liquid extraction (PLE) and Power Prep™ clean-up.

    Science.gov (United States)

    Helaleh, Murad I H; Al-Rashdan, Amal; Ibtisam, A

    2012-05-30

    An automated pressurized liquid extraction (PLE) method followed by Power Prep™ clean-up was developed for organochlorinated pesticide (OCP) and polychlorinated biphenyl (PCB) analysis in environmental marine samples of fish, squid, bivalves, shells, octopus and shrimp. OCPs and PCBs were simultaneously determined in a single chromatographic run using gas chromatography-mass spectrometry-negative chemical ionization (GC-MS-NCI). About 5 g of each biological marine sample was mixed with anhydrous sodium sulphate and placed in the extraction cell of the PLE system. PLE is controlled by means of a PC using DMS 6000 software. Purification of the extract was accomplished using automated Power Prep™ clean-up with a pre-packed disposable silica column (6 g) supplied by Fluid Management Systems (FMS). All OCPs and PCBs were eluted from the silica column using two types of solvent: 80 mL of hexane and a 50 mL mixture of hexane and dichloromethane (1:1). A wide variety of fish and shellfish were collected from the fish market and analyzed using this method. The total PCB concentrations were 2.53, 0.25, 0.24, 0.24, 0.17 and 1.38 ng g(-1) (w/w) for fish, squid, bivalves, shells, octopus and shrimp, respectively, and the corresponding total OCP concentrations were 30.47, 2.86, 0.92, 10.72, 5.13 and 18.39 ng g(-1) (w/w). Lipids were removed using an SX-3 Bio-Beads gel permeation chromatography (GPC) column. Analytical criteria such as recovery, reproducibility and repeatability were evaluated through a range of biological matrices. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. Optimization of Pressurized Liquid Extraction of Three Major Acetophenones from Cynanchum bungei Using a Box-Behnken Design

    Science.gov (United States)

    Li, Wei; Zhao, Li-Chun; Sun, Yin-Shi; Lei, Feng-Jie; Wang, Zi; Gui, Xiong-Bin; Wang, Hui

    2012-01-01

    In this work, pressurized liquid extraction (PLE) of three acetophenones (4-hydroxyacetophenone, baishouwubenzophenone, and 2,4-dihydroxyacetophenone) from Cynanchum bungei (ACB) were investigated. The optimal conditions for extraction of ACB were obtained using a Box-Behnken design, consisting of 17 experimental points, as follows: Ethanol (100%) as the extraction solvent at a temperature of 120 °C and an extraction pressure of 1500 psi, using one extraction cycle with a static extraction time of 17 min. The extracted samples were analyzed by high-performance liquid chromatography using an UV detector. Under this optimal condition, the experimental values agreed with the predicted values by analysis of variance. The ACB extraction yield with optimal PLE was higher than that obtained by soxhlet extraction and heat-reflux extraction methods. The results suggest that the PLE method provides a good alternative for acetophenone extraction. PMID:23203079

  18. Optimization of Pressurized Liquid Extraction of Three Major Acetophenones from Cynanchum bungei Using a Box-Behnken Design

    Directory of Open Access Journals (Sweden)

    Hui Wang

    2012-11-01

    Full Text Available In this work, pressurized liquid extraction (PLE of three acetophenones (4-hydroxyacetophenone, baishouwubenzophenone, and 2,4-dihydroxyacetophenone from Cynanchum bungei (ACB were investigated. The optimal conditions for extraction of ACB were obtained using a Box-Behnken design, consisting of 17 experimental points, as follows: Ethanol (100% as the extraction solvent at a temperature of 120 °C and an extraction pressure of 1500 psi, using one extraction cycle with a static extraction time of 17 min. The extracted samples were analyzed by high-performance liquid chromatography using an UV detector. Under this optimal condition, the experimental values agreed with the predicted values by analysis of variance. The ACB extraction yield with optimal PLE was higher than that obtained by soxhlet extraction and heat-reflux extraction methods. The results suggest that the PLE method provides a good alternative for acetophenone extraction.

  19. Optimization of pressurized liquid extraction by response surface methodology of Goji berry (Lycium barbarum L.) phenolic bioactive compounds.

    Science.gov (United States)

    Tripodo, Giusy; Ibáñez, Elena; Cifuentes, Alejandro; Gilbert-López, Bienvenida; Fanali, Chiara

    2018-01-03

    Pressurized liquid extraction (PLE) has been used for the first time in this work to extract phenolic compounds from Goji berries according to a multilevel factorial design using response surface methodology. The global yield (% w/dw, weight/dry-weight), total phenolic content (TPC), total flavonoid (TF) and antioxidant activity (determined via ABTS assay, expressed as TEAC value) were used as response variables to study the effects of temperature (50-180°C) and green solvent composition (mixtures of ethanol/water). Phenolic compounds characterization was performed by high performance liquid chromatography-diode array detector-tandem mass spectrometry (HPLC-DAD-MS/MS). The optimum PLE conditions predicted by the model were as follows: 180°C and 86% ethanol in water with a good desirability value of 0.815. The predicted conditions were confirmed experimentally and once the experimental design was validated for commercial fruit samples, the PLE extraction of phenolic compounds from three different varieties of fruit samples (Selvatico mongolo, Bigol, and Polonia) was performed. Nine phenolic compounds were tentatively identified in these extracts, including phenolic acids and their derivatives, and flavonols. The optimized PLE conditions were compared to a conventional solid-liquid extraction, demonstrating that PLE is a useful alternative to extract phenolic compounds from Goji berry. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. COMPARISONS OF SOXHLET EXTRACTION, PRESSURIZED LIQUID EXTRACTION, SUPERCRITICAL FLUID EXTRACTION, AND SUBCRITICAL WATER EXTRACTION FOR ENVIRONMENTAL SOLIDS: RECOVERY, SELECTIVITY, AND EFFECTS ON SAMPLE MATRIX. (R825394)

    Science.gov (United States)

    Extractions of a polycyclic aromatic hydrocarbon (PAH)-contaminated soil from a former manufactured gas plant site were performed with a Soxhlet apparatus (18 h), by pressurized liquid extraction (PLE) (50 min at 100°C), supercritical fluid extraction (SFE) (1 h at 150°...

  1. Pressurized liquid extraction of ginger (Zingiber officinale Roscoe) with bioethanol: an efficient and sustainable approach.

    Science.gov (United States)

    Hu, Jiajin; Guo, Zheng; Glasius, Marianne; Kristensen, Kasper; Xiao, Langtao; Xu, Xuebing

    2011-08-26

    To develop an efficient green extraction approach for recovery of bioactive compounds from natural plants, we examined the potential of pressurized liquid extraction (PLE) of ginger (Zingiber officinale Roscoe) with bioethanol/water as solvents. The advantages of PLE over other extraction approaches, in addition to reduced time/solvent cost, the extract of PLE showed a distinct constituent profile from that of Soxhlet extraction, with significantly improved recovery of diarylheptanoids, etc. Among the pure solvents tested for PLE, bioethanol yield the highest efficiency for recovering most constituents of gingerol-related compounds; while for a broad concentration spectrum of ethanol aqueous solutions, 70% ethanol gave the best performance in terms of yield of total extract, complete constituent profile and recovery of most gingerol-related components. PLE with 70% bioethanol operated at 1500 psi and 100 °C for 20 min (static extraction time: 5 min) is recommended as optimized extraction conditions, achieving 106.8%, 109.3% and 108.0% yield of [6]-, [8]- and [10]-gingerol relative to the yield of corresponding constituent obtained by 8h Soxhlet extraction (absolute ethanol as extraction solvent). Copyright © 2011 Elsevier B.V. All rights reserved.

  2. Determination of tributyltin (TBT) in marine sediment using pressurised liquid extraction-gas chromatography-isotope dilution mass spectrometry (PLE-GC-IDMS) with a hexane-tropolone mixture.

    Science.gov (United States)

    Konieczka, Piotr; Sejerøe-Olsen, Berit; Linsinger, Thomas P J; Schimmel, Heinz

    2007-06-01

    Extraction conditions for the determination of tributyltin (TBT) in sediment samples have been developed further. The analytical procedure is based on spiking with isotopically labelled analyte, pressurised liquid extraction (PLE) with a hexane/tropolone mixture, Grignard derivatization and quantification by GC-MS. It was applied to two unknown sediment samples as part of an intercomparison exercise of the Comité Consultatif pour la Quantité de Matière (CCQM). The detection limit was approximately 1.5 ng/g TBT as Sn, while the repeatability and intermediate precision (as the coefficient of variation) were 1.9% and 3.2%, respectively. The expanded uncertainty was 6.2% (coverage factor k = 2), and the accuracy was confirmed by measurement of a certified reference material.

  3. Determination of pharmaceuticals in environmental and biological matrices using pressurised liquid extraction--are we developing sound extraction methods?

    DEFF Research Database (Denmark)

    Runnqvist, Hannah; Bak, Søren Alex; Hansen, Martin

    2010-01-01

    Pressurised liquid extraction (PLE) is now a well established and extensively applied extraction technique in environmental analysis for pollutants such as persistent organic pollutants (POPs). During the past decade, an emerging group of environmentally interesting analytes are pharmaceuticals...

  4. Pressurized liquid extraction-assisted mussel cytosol preparation for the determination of metals bound to metallothionein-like proteins

    International Nuclear Information System (INIS)

    Santiago-Rivas, Sandra; Moreda-Pineiro, Antonio; Bermejo-Barrera, Pilar; Moreda-Pineiro, Jorge; Alonso-Rodriguez, Elia; Muniategui-Lorenzo, Soledad; Lopez-Mahia, Purificacion; Prada-Rodriguez, Dario

    2007-01-01

    The possibilities of pressurized liquid extraction (PLE) have been novelty tested to assist the cytosol preparation from wet mussel soft tissue before the determination of metals bound to metallothionein-like proteins (MLPs). Results obtained after PLE were compared with those obtained after a classical blending procedure for mussel cytosolic preparation. Isoforms MLP-1 (retention time of 4.1 min) and MLP-2 (retention time of 7.4 min) were separated by anion exchange high-performance liquid chromatography (HPLC) and the concentrations of Ba, Cu, Mn, Sr and Zn bound to MLP isoforms were directly measured by inductively coupled plasma-atomic emission spectrometry (ICP-OES) as a multi-element detector. The optimized PLE-assisted mussel cytosol preparation has consisted of one extraction cycle at room temperature and 1500 psi for 2 min. Since separation between the solid mussel residue and the extract (cytosol) is performed by the PLE system, the cytosol preparation method is faster than conventional cytosol preparation methods by cutting/blending using Ultraturrax or Stomacher devices

  5. Pressurised liquid extraction of flavonoids in onions. Method development and validation

    DEFF Research Database (Denmark)

    Søltoft, Malene; Christensen, J.H.; Nielsen, J.

    2009-01-01

    A rapid and reliable analytical method for quantification of flavonoids in onions was developed and validated. Five extraction methods were tested on freeze-dried onions and subsequently high performance liquid chromatography (HPLC) with UV detection was used for quantification of seven flavonoids...... extraction methods. However. PLE was the preferred extraction method because the method can be highly automated, use only small amounts of solvents, provide the cleanest extracts, and allow the extraction of light and oxygen-sensitive flavonoids to be carried out in an inert atmosphere protected from light......-step PLE method showed good selectivity, precision (RSDs = 3.1-11%) and recovery of the extractable flavonoids (98-99%). The method also appeared to be a multi-method, i.e. generally applicable to, e.g. phenolic acids in potatoes and carrots....

  6. Selective extraction of high-value phenolic compounds from distillation wastewater of basil (Ocimum basilicum L.) by pressurized liquid extraction.

    Science.gov (United States)

    Pagano, Imma; Sánchez-Camargo, Andrea Del Pilar; Mendiola, Jose Antonio; Campone, Luca; Cifuentes, Alejandro; Rastrelli, Luca; Ibañez, Elena

    2018-01-31

    During the essential oil steam distillation from aromatic herbs, huge amounts of distillation wastewaters (DWWs) are generated. These by-products represent an exceptionally rich source of phenolic compounds such as rosmarinic acid (RA) and caffeic acid (CA). Herein, the alternative use of dried basil DWWs (dDWWs) to perform a selective extraction of RA and CA by pressurized liquid extraction (PLE) employing bio-based solvent was studied. To select the most suitable solvent for PLE, the theoretical modelling of Hansen solubility parameters (HSP) was carried out. This approach allows reducing the list of candidate to two solvents: ethanol and ethyl lactate. Due to the composition of the sample, mixtures of water with those solvents were also tested. An enriched PLE extract in RA (23.90 ± 2.06 mg/g extract) with an extraction efficiency of 75.89 ± 16.03% employing a water-ethanol mixture 25:75 (% v/v) at 50°C was obtained. In the case of CA, a PLE extract with 2.42 ± 0.04 mg/g extract, having an extraction efficiency of 13.86 ± 4.96% using ethanol absolute at 50°C was achieved. DWWs are proposed as new promising sources of natural additives and/or functional ingredients for cosmetic, nutraceutical, and food applications. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Selective Extraction of Organic Contaminants from Soil Using Pressurised Liquid Extraction

    Directory of Open Access Journals (Sweden)

    Rozita Osman

    2013-01-01

    Full Text Available This study focuses on the application of sorbents in pressurised liquid extraction (PLE cell to establish a selective extraction of a variety of organic contaminants (polycyclic aromatic hydrocarbons (PAHs, chlorpyrifos, phenol, pentachlorophenol, and sterols from soil. The selectivity and efficiency of each sorbent depend on the properties of the material, extracting solvent, capacity factor, organic compounds of interest, and PLE operating parameters (temperature, pressure, and extraction time. Several sorbents (silica, alumina, and Florisil were evaluated and with the proper choice of solvents, polar and nonpolar compounds were successfully separated in two fractions. Nonpolar compounds (PAHs, chlorpyrifos, and pentachlorophenol were recovered in the first fraction using a polar sorbent such as Florisil or alumina, and n-hexane as eluting solvent, while more polar compounds (phenol and sterols were recovered in the second fraction using methanol. Silica (5 g was found to be effective for selective extraction with the satisfactory recoveries for all compounds (PAHs from 87.1–96.2%, chlorpyrifos 102.9%, sterols from 93.7–100.5%, phenol 91.9%, and pentachlorophenol 106.2%. The efficiency and precision of this extraction approach and the existing EPA Method 3545 were compared.

  8. Extraction of polycyclic aromatic hydrocarbons from smoked fish using pressurized liquid extraction with integrated fat removal

    DEFF Research Database (Denmark)

    Lund, Mette; Duedahl-Olesen, Lene; Christensen, Jan H.

    2009-01-01

    Quantification of polycyclic aromatic hydrocarbons (PAHs) in smoked fish products often requires multiple clean-up steps to remove fat and other compounds that may interfere with the chemical analysis. We present a novel pressurized liquid extraction (PLE) method that integrates exhaustive...

  9. Home-made online hyphenation of pressurized liquid extraction, turbulent flow chromatography, and high performance liquid chromatography, Cistanche deserticola as a case study.

    Science.gov (United States)

    Song, Qingqing; Li, Jun; Liu, Xiao; Zhang, Yuan; Guo, Liping; Jiang, Yong; Song, Yuelin; Tu, Pengfei

    2016-03-18

    Incompatibility between the conventional pressurized liquid extraction (PLE) devices and high performance liquid chromatography (HPLC) extensively hinders direct and green chemical analysis of herbal materials. Herein, a facile PLE module was configured, and then it was online hyphenated with HPLC via a turbulent flow chromatography (TFC) column. Regarding PLE module, a long PEEK tube (0.13 × 1000 mm) was employed to generate desired pressure (approximately 13.0 MPa) when warm acidic water (70 °C) was delivered as extraction solvent at a high flow rate (2.5 mL/min), and a hollow guard column (3.0 × 4.0 mm) was implemented to hold crude materials. Effluent was collected from the outlet of PEEK tube, concentrated, and subjected onto HPLC coupled with hybrid ion trap-time of flight mass spectrometer to assess the extraction efficiency and also to profile the chemical composition of Cistanche deserticola (CD) that is honored as "Ginseng of the desert". Afterwards, a TFC column was introduced to accomplish online transmission of low molecule weight components from PLE module to HPLC coupled with diode array detection, and two electronic 6-port/2-channel valves were in charge of alternating the whole system between extraction (0-3.0 min) and elution (3.0-35.0 min) phases. Quantitative method was developed and validated for simultaneous determination of eight primary phenylethanoid glycosides in CD using online PLE-TFC-HPLC. All findings demonstrated that the home-made platform is advantageous at direct chemical analysis, as well as time-, solvent-, and material-savings, suggesting a robust tool for chemical fingerprinting of herbs. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Extraction of bioactive carbohydrates from artichoke (Cynara scolymus L.) external bracts using microwave assisted extraction and pressurized liquid extraction.

    Science.gov (United States)

    Ruiz-Aceituno, Laura; García-Sarrió, M Jesús; Alonso-Rodriguez, Belén; Ramos, Lourdes; Sanz, M Luz

    2016-04-01

    Microwave assisted extraction (MAE) and pressurized liquid extraction (PLE) methods using water as solvent have been optimized by means of a Box-Behnken and 3(2) composite experimental designs, respectively, for the effective extraction of bioactive carbohydrates (inositols and inulin) from artichoke (Cynara scolymus L.) external bracts. MAE at 60 °C for 3 min of 0.3 g of sample allowed the extraction of slightly higher concentrations of inositol than PLE at 75 °C for 26.7 min (11.6 mg/g dry sample vs. 7.6 mg/g dry sample). On the contrary, under these conditions, higher concentrations of inulin were extracted with the latter technique (185.4 mg/g vs. 96.4 mg/g dry sample), considering two successive extraction cycles for both techniques. Both methodologies can be considered appropriate for the simultaneous extraction of these bioactive carbohydrates from this particular industrial by-product. To the best of our knowledge this is the first time that these techniques are applied for this purpose. Copyright © 2015 Elsevier Ltd. All rights reserved.

  11. Optimization of pressurized liquid extraction (PLE) for rapid determination of mineral oil saturated (MOSH) and aromatic hydrocarbons (MOAH) in cardboard and paper intended for food contact.

    Science.gov (United States)

    Moret, Sabrina; Sander, Maren; Purcaro, Giorgia; Scolaro, Marianna; Barp, Laura; Conte, Lanfranco S

    2013-10-15

    Packaging can represent a primary source of food contamination with mineral oil saturated hydrocarbons (MOSH) and aromatic hydrocarbons (MOAH), especially when recycled cardboard or mineral oil based printing inks are used. A pressurized liquid extraction (PLE) method, followed by on-line LC-GC analysis, has been optimized for rapid mineral oil determination in cardboard and paper samples. The proposed method involves extraction with hexane (2 cycles) at 60°C for 5 min, and allows for the processing of up to 6 samples in parallel with minimal sample manipulation and solvent consumption. It gave good repeatability (coefficient of variation lower than 5%) and practically quantitative extraction yield (less than 2% of the total contamination found in a third separate cycle). The method was applied to different cardboards and paper materials intended for food contact. Results obtained were similar to those obtained by applying classical solvent extraction with hexane/ethanol 1:1 (v/v) as described by Lorenzini et al. [20]. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. Miniaturised pressurised liquid extraction aromatic hydrocarbons from soil and sediment with subsequent large-volume injection-gas chromatography

    NARCIS (Netherlands)

    Ramos, L.; Vreuls, J.J.; Brinkman, U.A.T.

    2000-01-01

    Analyte extraction is the main limitation when developing at-line, or on-line, procedures for the preparation of (semi)solid environmental samples. Pressurised liquid extraction (PLE) is an analyte- and matrix-independent technique which provides cleaner extracts than the time-consuming classical

  13. A validated solid-liquid extraction method for the HPLC determination of polyphenols in apple tissues Comparison with pressurised liquid extraction.

    Science.gov (United States)

    Alonso-Salces, Rosa M; Barranco, Alejandro; Corta, Edurne; Berrueta, Luis A; Gallo, Blanca; Vicente, Francisca

    2005-02-15

    A solid-liquid extraction procedure followed by reversed-phase high-performance liquid chromatography (RP-HPLC) coupled with a photodiode array detector (DAD) for the determination of polyphenols in freeze-dried apple peel and pulp is reported. The extraction step consists in sonicating 0.5g of freeze-dried apple tissue with 30mL of methanol-water-acetic acid (30:69:1, v/v/v) containing 2g of ascorbic acid/L, for 10min in an ultrasonic bath. The whole method was validated, concluding that it is a robust method that presents high extraction efficiencies (peel: >91%, pulp: >95%) and appropriate precisions (within day: R.S.D. (n = 5) <5%, and between days: R.S.D. (n = 5) <7%) at the different concentration levels of polyphenols that can be found in apple samples. The method was compared with one previously published, consisting in a pressurized liquid extraction (PLE) followed by RP-HPLC-DAD determination. The advantages and disadvantages of both methods are discussed.

  14. Determination of carbohydrates in tobacco by pressurized liquid extraction combined with a novel ultrasound-assisted dispersive liquid-liquid microextraction method.

    Science.gov (United States)

    Cai, Kai; Hu, Deyu; Lei, Bo; Zhao, Huina; Pan, Wenjie; Song, Baoan

    2015-07-02

    A novel derivatization-ultrasonic assisted-dispersive liquid-liquid microextraction (UA-DLLME) method for the simultaneous determination of 11 main carbohydrates in tobacco has been developed. The combined method involves pressurized liquid extraction (PLE), derivatization, and UA-DLLME, followed by the analysis of the main carbohydrates with a gas chromatography-flame ionization detector (GC-FID). First, the PLE conditions were optimized using a univariate approach. Then, the derivatization methods were properly compared and optimized. The aldononitrile acetate method combined with the O-methoxyoxime-trimethylsilyl method was used for derivatization. Finally, the critical variables affecting the UA-DLLME extraction efficiency were searched using fractional factorial design (FFD) and further optimized using Doehlert design (DD) of the response surface methodology. The optimum conditions were found to be 44 μL for CHCl3, 2.3 mL for H2O, 11% w/v for NaCl, 5 min for the extraction time and 5 min for the centrifugation time. Under the optimized experimental conditions, the detection limit of the method (LODs) and linear correlation coefficient were found to be in the range of 0.06-0.90 μg mL(-1) and 0.9987-0.9999. The proposed method was successfully employed to analyze three flue-cured tobacco cultivars, among which the main carbohydrate concentrations were found to be very different. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Antioxidant White Grape Seed Phenolics: Pressurized Liquid Extracts from Different Varieties

    Directory of Open Access Journals (Sweden)

    Carmen Garcia-Jares

    2015-11-01

    Full Text Available Grape seeds represent a high percentage (20% to 26% of the grape marc obtained as a byproduct from white winemaking and keep a vast proportion of grape polyphenols. In this study, seeds obtained from 11 monovarietal white grape marcs cultivated in Northwestern Spain have been analyzed in order to characterize their polyphenolic content and antioxidant activity. Seeds of native (Albariño, Caiño, Godello, Loureiro, Torrontés, and Treixadura and non-native (Chardonnay, Gewurtzträminer, Pinot blanc, Pinot gris, and Riesling grape varieties have been considered. Low weight phenolics have been extracted by means of pressurized liquid extraction (PLE and further analyzed by LC-MS/MS. The results showed that PLE extracts, whatever the grape variety of origin, contained large amounts of polyphenols and high antioxidant activity. Differences in the varietal polyphenolic profiles were found, so a selective exploitation of seeds might be possible.

  16. Antioxidant White Grape Seed Phenolics: Pressurized Liquid Extracts from Different Varieties

    Science.gov (United States)

    Garcia-Jares, Carmen; Vazquez, Alberto; Lamas, Juan P.; Pajaro, Marta; Alvarez-Casas, Marta; Lores, Marta

    2015-01-01

    Grape seeds represent a high percentage (20% to 26%) of the grape marc obtained as a byproduct from white winemaking and keep a vast proportion of grape polyphenols. In this study, seeds obtained from 11 monovarietal white grape marcs cultivated in Northwestern Spain have been analyzed in order to characterize their polyphenolic content and antioxidant activity. Seeds of native (Albariño, Caiño, Godello, Loureiro, Torrontés, and Treixadura) and non-native (Chardonnay, Gewurtzträminer, Pinot blanc, Pinot gris, and Riesling) grape varieties have been considered. Low weight phenolics have been extracted by means of pressurized liquid extraction (PLE) and further analyzed by LC-MS/MS. The results showed that PLE extracts, whatever the grape variety of origin, contained large amounts of polyphenols and high antioxidant activity. Differences in the varietal polyphenolic profiles were found, so a selective exploitation of seeds might be possible. PMID:26783956

  17. Turning off flagellum rotation requires the pleiotropic gene pleD: pleA, pleC, and pleD define two morphogenic pathways in Caulobacter crescentus.

    OpenAIRE

    Sommer, J M; Newton, A

    1989-01-01

    We have identified mutations in three pleiotropic genes, pleA, pleC, and pleD, that are required for differentiation in Caulobacter crescentus. pleA and pleC mutants were isolated in an extensive screen for strains defective in both motility and adsorption of polar bacteriophage phi CbK; using temperature-sensitive alleles, we determined the time at which the two genes act. pleA was required for a short period at 0.7 of the swarmer cell cycle for flagellum biosynthesis, whereas pleC was requi...

  18. Optimisation of pressurised liquid extraction of antioxidants from black bamboo leaves.

    Science.gov (United States)

    Shang, Ya Fang; Kim, Sang Min; Um, Byung-Hun

    2014-07-01

    To develop an efficient green extraction approach for recovering bioactive compounds from natural plants, the potential of using pressurised liquid extraction (PLE) was examined on black bamboo (Phyllostachys nigra) leaves, with ethanol/water as solvents. The superheated PLE process showed a higher recovery of most constituents and antioxidative activity, compared to reflux extraction, with a significantly improved recovery of the total phenolic (TP) and flavonoid (TF) content and DPPH radical scavenging ability. For a broad range of ethanol aqueous solutions and temperatures, 50% EtOH and 200°C (static time: 25min) gave the best performance, in terms of the TP and TF (75% EtOH) content yield and DPPH scavenging ability (25% EtOH). Under the optimised extraction conditions, eight main antioxidative compounds were isolated and identified with HPLC-ABTS(+) assay guidance and assessed for radical scavenging activity. The superheated extraction process for black bamboo leaves enhanced the antioxidant properties by increasing the extraction of the phenolic components. Copyright © 2013 Elsevier Ltd. All rights reserved.

  19. Optimization of microwave-assisted extraction and pressurized liquid extraction of phenolic compounds from Moringa oleifera leaves by multiresponse surface methodology.

    Science.gov (United States)

    Rodríguez-Pérez, Celia; Gilbert-López, Bienvenida; Mendiola, Jose Antonio; Quirantes-Piné, Rosa; Segura-Carretero, Antonio; Ibáñez, Elena

    2016-07-01

    This work aims at studying the optimization of microwave-assisted extraction (MAE) and pressurized liquid extraction (PLE) by multi-response surface methodology (RSM) to test their efficiency towards the extraction of phenolic compounds from Moringa oleifera (M. oleifera) leaves. The extraction yield, total phenolic content (TPC), total flavonoid content (TF), DPPH scavenging method and trolox equivalent antioxidant capacity (TEAC) assay were considered as response variables while effects of extraction time, percentage of ethanol, and temperature were studied. Extraction time of 20 min, 42% ethanol and 158°C were the MAE optimum conditions for achieving extraction yield of 26 ± 2%, EC50 15 ± 2 μg/mL, 16 ± 1 Eq Trolox/100 g dry leaf, 5.2 ± 0.5 mg Eq quercetin/g dry leaf, and 86 ± 4 mg GAE/g dry leaf. Regarding PLE, the optimum conditions that allowed extraction yield of 56 ± 2%, EC50 21 ± 3 μg/mL, 12 ± 2 mmol Eq Trolox/100 g dry leaf, 6.5 ± 0.2 mg Eq quercetin/g dry leaf, and 59 ± 6 mg GAE/g dry leaf were 128°C, 35% of ethanol, and 20 min. PLE enabled the extraction of phenolic compounds with a higher number of hydroxyl-type substituents such as kaempferol diglycoside and its acetyl derivatives and those that are sensitive to high temperatures (glucosinolates or amino acids) while MAE allowed better recoveries of kaempferol, quercetin, and their glucosides derivatives. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Analytical method for the determination of trace levels of steroid hormones and corticosteroids in soil, based on PLE/SPE/LC-MS/MS.

    Science.gov (United States)

    Gineys, N; Giroud, B; Vulliet, E

    2010-07-01

    The aim of this study was to develop an efficient, sensitive and reliable analytical method for the determination of traces of steroid hormones (including oestrogen, androgens and progestagens) and corticosteroids in soil. A method of sample preparation involving pressurized liquid extraction (PLE) and solid-phase extraction (SPE) was developed for the determination of six steroids and five corticosteroids in soils, followed by analysis by liquid chromatography-tandem mass spectrometry. The conditions employed for PLE involved acetone/methanol (50:50) as the extracting solvent, a temperature of 80 degrees C, two cycles and a static time of 5 min. The extraction was followed by a SPE clean-up based on a polymeric phase. With use of protocol, a residual matrix effect was, however, highlighted. The limit of detection in soil was 0.08-0.89 ng/g for steroids and 0.09-2.84 ng/g for corticosteroids.

  1. A protocol for pressurized liquid extraction and processing methods to isolate modern and ancient bone cholesterol for compound-specific stable isotope analysis.

    Science.gov (United States)

    Laffey, Ann O; Krigbaum, John; Zimmerman, Andrew R

    2017-02-15

    Bone lipid compound-specific isotope analysis (CSIA) and bone collagen and apatite stable isotope ratio analysis are important sources of ecological and paleodietary information. Pressurized liquid extraction (PLE) is quicker and utilizes less solvent than traditional methods of lipid extraction such as soxhlet and ultrasonication. This study facilitates dietary analysis by optimizing and testing a standardized methodology for PLE of bone cholesterol. Modern and archaeological bones were extracted by PLE using varied temperatures, solvent solutions, and sample weights. The efficiency of PLE was assessed via quantification of cholesterol yields. Stable isotopic ratio integrity was evaluated by comparing isotopic signatures (δ 13 C and δ 18 O values) of cholesterol derived from whole bone, bone collagen and bone apatite. Gas chromatography/mass spectrometry (GC/MS) and gas chromatography isotope ratio mass spectrometry (GC/IRMS) were conducted on purified collagen and lipid extracts to assess isotopic responses to PLE. Lipid yield was optimized at two PLE extraction cycles of 75 °C using dichloromethane/methanol (2:1 v/v) as a solvent with 0.25-0.75 g bone sample. Following lipid extraction, saponification combined with the derivatization of the neutral fraction using trimethylsilylation yielded nearly twice the cholesterol of non-saponified or non-derivatized samples. It was also found that lipids extracted from purified bone collagen and apatite could be used for cholesterol CSIA. There was no difference in the bulk δ 13 C values of collagen extracted from bone with or without lipid. However, there was a significant depletion in 18 O of bone apatite due to lipid presence or processing. These results should assist sample selection and provide an effective, alternative extraction method for bone cholesterol that may be used for isotopic and paleodietary analysis. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  2. Pressurized liquid extraction of anthocyanins and biflavonoids from Schinus terebinthifolius Raddi: A multivariate optimization.

    Science.gov (United States)

    Feuereisen, Michelle M; Gamero Barraza, Mariana; Zimmermann, Benno F; Schieber, Andreas; Schulze-Kaysers, Nadine

    2017-01-01

    Response surface methodology was employed to investigate the effects of pressurized liquid extraction (PLE) parameters on the recovery of phenolic compounds (anthocyanins, biflavonoids) from Brazilian pepper (Schinus terebinthifolius Raddi) fruits. The effects of temperature, static time, and ethanol as well as acid concentration on the polyphenol yield were described well by quadratic models (p75°C), an artifact occurred and was tentatively identified as a diastereomer of I3',II8-binaringenin. Multivariate optimization led to high yields of phenolic compounds from the exocarp/drupes at 100/75°C, 10/10min, 54.5/54.2% ethanol, and 5/0.03% acetic acid. This study demonstrates that PLE is well suited for the extraction of phenolic compounds from S. terebinthifolius and can efficiently be optimized by response surface methodology. Copyright © 2016 Elsevier Ltd. All rights reserved.

  3. Determination of caffeoylquinic acids in feed and related products by focused ultrasound solid-liquid extraction and ultra-high performance liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Tena, M T; Martínez-Moral, M P; Cardozo, P W

    2015-06-26

    A method to determine caffeoylquinic acids (CQAs) in three sources (herbal extract, feed additive and finished feed) using for the first time focused ultrasound solid-liquid extraction (FUSLE) followed by ultra-high performance liquid chromatography (UPLC) coupled to quadrupole-time of flight mass spectrometry is presented. Pressurized liquid extraction (PLE) was also tested as extraction technique but it was discarded because cynarin was not stable under temperature values used in PLE. The separation of the CQAs isomers was carried out in only seven minutes. FUSLE variables such as extraction solvent, power and time were optimized by a central composite design. Under optimal conditions, FUSLE extraction was performed with 8mL of an 83:17 methanol-water mixture for 30s at a power of 60%. Only two extraction steps were found necessary to recover analytes quantitatively. Sensitivity, linearity, accuracy and precision were established. Matrix effect was studied for each type of sample. It was not detected for mono-CQAs, whereas the cynarin signal was strongly decreased due to ionization suppression in presence of matrix components; so the quantification by standard addition was mandatory for the determination of di-caffeoylquinic acids. Finally, the method was applied to the analysis of herbal extracts, feed additives and finished feed. In all samples, chlorogenic acid was the predominant CQA, followed by criptochlorogenic acid, neochlorogenic acid and cynarin. The method allows an efficient determination of chlorogenic acid with good recovery rates. Therefore, it may be used for screening of raw material and for process and quality control in feed manufacture. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. Pressurized liquid extracts from Spirulina platensis microalga. Determination of their antioxidant activity and preliminary analysis by micellar electrokinetic chromatography.

    Science.gov (United States)

    Herrero, Miguel; Ibáñez, Elena; Cifuentes, Alejandro; Señoráns, Javier

    2004-08-27

    In this work, different extracts from the microalga Spirulina platensis are obtained using pressurized liquid extraction (PLE) and four different solvents (hexane, light petroleum, ethanol and water). Different extraction temperatures (115 and 170 degrees C) were tested using extraction times ranging from 9 to 15 min. The antioxidant activity of the different extracts is determined by means of an in vitro assay using a free radical method. Moreover, a new and fast method is developed using micellar electrokinetic chromatography with diode array detection (MEKC-DAD) to provide a preliminary analysis on the composition of the extracts. This combined application (i.e., in vitro assays plus MEKC-DAD) allowed the fast characterization of the extracts based on their antioxidant activity and the UV-vis spectra of the different compounds found in the extracts. To our knowledge, this work shows for the first time the great possibilities of the combined use of PLE-in vitro assay-MEKC-DAD to investigate natural sources of antioxidants.

  5. Simultaneous quantification of major flavonoids in "Bawanghua", the edible flower of Hylocereus undatus using pressurised liquid extraction and high performance liquid chromatography.

    Science.gov (United States)

    Yi, Yan; Zhang, Qing-Wen; Li, Song-Lin; Wang, Ying; Ye, Wen-Cai; Zhao, Jing; Wang, Yi-Tao

    2012-11-15

    A pressurised liquid extraction (PLE) and high performance liquid chromatography (HPLC) method was developed for simultaneous quantification of six major flavonoids in edible flower of Hylocereus undatus. In order to achieve the baseline separation of two pairs of isomers, the HPLC conditions were optimised with different kind of reversed phase columns and mobile phase gradient programs. In addition, the solvent concentration, extraction temperature, extraction time and flush cycle for PLE were also optimised. Zorbax SB-C8 (100×2.1 mm, 1.8 μm) column was chosen with acetonitrile and water containing 0.1% trifluoroacetic acid as mobile phase, the six analytes were eluted with baseline separation. The calibration curves showed good linearity (r(2)>0.9994) with LODs and LOQs less than 0.90 and 3.60 ng respectively. The RSDs for intra- and inter-day repeatability was not more than 1.09% and 1.79% respectively. The overall recovery of the assay was 96.9-105.2%. The sample was stable for at least 12 h. The newly established method was successfully applied to quantify six flavonoids in different parts of "Bawanghua", and the commercial samples from different locations. Copyright © 2012 Elsevier Ltd. All rights reserved.

  6. Comparison of low-level polycyclic aromatic hydrocarbons in sediment revealed by Soxhlet extraction, microwave-assisted extraction, and pressurized liquid extraction

    International Nuclear Information System (INIS)

    Itoh, Nobuyasu; Numata, Masahiko; Aoyagi, Yoshie; Yarita, Takashi

    2008-01-01

    We analyzed polycyclic aromatic hydrocarbons (PAHs) present in lake sediment at low levels ( -1 ) by using Soxhlet extraction (Soxhlet), microwave-assisted extraction (MAE), and pressurized liquid extraction (PLE) in combination with gas chromatography and isotope-dilution mass spectrometry. Although all extraction techniques showed good repeatability for five target PAHs (relative standard deviation MAE > Soxhlet. Differences in the results originated mainly from differences in the extraction efficiencies of the techniques for native PAHs, because all techniques gave comparable recovery yields of corresponding 13 C-labeled PAHs ( 13 C-PAHs) (51-84%). Since non-negligible amounts of both native PAHs and 13 C-PAHs were re-adsorbed on matrix in MAE, not only recovery yields of 13 C-PAHs but also efficiencies of extraction of native PAHs should be examined to evaluate the appropriateness of any analytical procedures

  7. Pressurized liquid extracts from Spirulina platensis microalga Determination of their antioxidant activity and preliminary analysis by micellar electrokinetic chromatography

    OpenAIRE

    Herrero, Miguel; Ibáñez, Elena; Señorans, F. Javier; Cifuentes, Alejandro

    2004-01-01

    In this work, different extracts from the microalga Spirulina platensis are obtained using pressurized liquid extraction (PLE) and four different solvents (hexane, light petroleum, ethanol andwater). Different extraction temperatures (115 and 170 ◦C) were tested using extraction times ranging from 9 to 15 min. The antioxidant activity of the different extracts is determined by means of an in vitro assay using a free radical method. Moreover, a new and fast method is developed using m...

  8. MHD PbLi experiments in MaPLE loop at UCLA

    International Nuclear Information System (INIS)

    Courtessole, C.; Smolentsev, S.; Sketchley, T.; Abdou, M.

    2016-01-01

    Highlights: • The paper overviews the MaPLE facility at UCLA: one-of-a-few PbLi MHD loop in the world. • We present the progress achieved in development and testing of high-temperature PbLi flow diagnostics. • The most important MHD experiments carried out since the first loop operation in 2011 are summarized. - Abstract: Experiments on magnetohydrodynamic (MHD) flows are critical to understanding complex flow phenomena in ducts of liquid metal blankets, in particular those that utilize eutectic alloy lead–lithium as breeder/coolant, such as self-cooled, dual-coolant and helium-cooled lead–lithium blanket concepts. The primary goal of MHD experiments at UCLA using the liquid metal flow facility called MaPLE (Magnetohydrodynamic PbLi Experiment) is to address important MHD effects, heat transfer and flow materials interactions in blanket-relevant conditions. The paper overviews the one-of-a-kind MaPLE loop at UCLA and presents recent experimental activities, including the development and testing of high-temperature PbLi flow diagnostics and experiments that have been performed since the first loop operation in 2011. We also discuss MaPLE upgrades, which need to be done to substantially expand the experimental capabilities towards a new class of MHD flow phenomena that includes buoyancy effects.

  9. MHD PbLi experiments in MaPLE loop at UCLA

    Energy Technology Data Exchange (ETDEWEB)

    Courtessole, C., E-mail: cyril@fusion.ucla.edu; Smolentsev, S.; Sketchley, T.; Abdou, M.

    2016-11-01

    Highlights: • The paper overviews the MaPLE facility at UCLA: one-of-a-few PbLi MHD loop in the world. • We present the progress achieved in development and testing of high-temperature PbLi flow diagnostics. • The most important MHD experiments carried out since the first loop operation in 2011 are summarized. - Abstract: Experiments on magnetohydrodynamic (MHD) flows are critical to understanding complex flow phenomena in ducts of liquid metal blankets, in particular those that utilize eutectic alloy lead–lithium as breeder/coolant, such as self-cooled, dual-coolant and helium-cooled lead–lithium blanket concepts. The primary goal of MHD experiments at UCLA using the liquid metal flow facility called MaPLE (Magnetohydrodynamic PbLi Experiment) is to address important MHD effects, heat transfer and flow materials interactions in blanket-relevant conditions. The paper overviews the one-of-a-kind MaPLE loop at UCLA and presents recent experimental activities, including the development and testing of high-temperature PbLi flow diagnostics and experiments that have been performed since the first loop operation in 2011. We also discuss MaPLE upgrades, which need to be done to substantially expand the experimental capabilities towards a new class of MHD flow phenomena that includes buoyancy effects.

  10. Application of PLE for the determination of essential oil components from Thymus vulgaris L.

    Science.gov (United States)

    Dawidowicz, Andrzej L; Rado, Ewelina; Wianowska, Dorota; Mardarowicz, Marek; Gawdzik, Jan

    2008-08-15

    Essential plants, due to their long presence in human history, their status in culinary arts, their use in medicine and perfume manufacture, belong to frequently examined stock materials in scientific and industrial laboratories. Because of a large number of freshly cut, dried or frozen plant samples requiring the determination of essential oil amount and composition, a fast, safe, simple, efficient and highly automatic sample preparation method is needed. Five sample preparation methods (steam distillation, extraction in the Soxhlet apparatus, supercritical fluid extraction, solid phase microextraction and pressurized liquid extraction) used for the isolation of aroma-active components from Thymus vulgaris L. are compared in the paper. The methods are mainly discussed with regard to the recovery of components which typically exist in essential oil isolated by steam distillation. According to the obtained data, PLE is the most efficient sample preparation method in determining the essential oil from the thyme herb. Although co-extraction of non-volatile ingredients is the main drawback of this method, it is characterized by the highest yield of essential oil components and the shortest extraction time required. Moreover, the relative peak amounts of essential components revealed by PLE are comparable with those obtained by steam distillation, which is recognized as standard sample preparation method for the analysis of essential oils in aromatic plants.

  11. Application of response surface methodology to optimize pressurized liquid extraction of antioxidant compounds from sage (Salvia officinalis L.), basil (Ocimum basilicum L.) and thyme (Thymus vulgaris L.).

    Science.gov (United States)

    Hossain, M B; Brunton, N P; Martin-Diana, A B; Barry-Ryan, C

    2010-12-01

    The present study optimized pressurized liquid extraction (PLE) conditions using Dionex ASE® 200, USA to maximize the antioxidant activity [Ferric ion Reducing Antioxidant Power (FRAP)] and total polyphenol content (TP) of the extracts from three spices of Lamiaceae family (sage, basil and thyme). Optimal conditions with regard to extraction temperature (66-129 °C) and solvent concentration (32-88% methanol) were identified using response surface methodology (RSM). For all three spices, results showed that 129 °C was the optimum temperature with regard to antioxidant activity. Optimal methanol concentrations with respect to the antioxidant activity of sage and basil extracts were 58% and 60% respectively. Thyme showed a different trend with regard to methanol concentration and was optimally extracted at 33%. Antioxidant activity yields of the optimal PLE were significantly (p < 0.05) higher than solid/liquid extracts. Predicted models were highly significant (p < 0.05) for both total phenol (TP) and FRAP values in all the spices with high regression coefficients (R(2)) ranging from 0.651 to 0.999.

  12. A high-throughput method for the simultaneous determination of multiple mycotoxins in human and laboratory animal biological fluids and tissues by PLE and HPLC-MS/MS.

    Science.gov (United States)

    Cao, Xiaoqin; Wu, Shuangchan; Yue, Yuan; Wang, Shi; Wang, Yuting; Tao, Li; Tian, Hui; Xie, Jianmei; Ding, Hong

    2013-12-30

    A high-throughput method for the determination of 28 mycotoxins involving pressurised liquid extraction (PLE) coupled with liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has been optimised and validated for determination in various biological fluids and tissues of human and laboratory animals. High-throughput analysis was achieved using PLE pre-treatment and without the need for any cleanup. The extraction solvent was acetonitrile/water/acetic acid (80/19/1, v/v/v). The static extraction time was 5min. The extraction pressure and temperature were 1500psi and 140°C, respectively. The flush volume was 60%. The limits of detection, which were defined as CCα, varied from 0.01μg/kg (μg/L) to 0.69μg/kg (μg/L). The recoveries of spiked samples from 0.20μg/kg (μg/L) to 2μg/kg (μg/L) ranged from 71% to 100.5% with relative standard deviations of less than 17.5%, except FB1 and FB2 recoveries, which were lower than 60%. The method was successfully applied in real samples, and the data indicate that this technique is a useful analytical method for the determination of mycotoxins from humans and animals. To the best of our knowledge, this method is the first for the large-scale testing of multi-class mycotoxins in all types of biological fluids and tissues that uses PLE and HPLC-MS/MS. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. Total milk fat extraction and quantification of polar and neutral lipids of cow, goat, and ewe milk by using a pressurized liquid system and chromatographic techniques.

    Science.gov (United States)

    Castro-Gómez, M P; Rodriguez-Alcalá, L M; Calvo, M V; Romero, J; Mendiola, J A; Ibañez, E; Fontecha, J

    2014-11-01

    Although milk polar lipids such as phospholipids and sphingolipids located in the milk fat globule membrane constitute 0.1 to 1% of the total milk fat, those lipid fractions are gaining increasing interest because of their potential beneficial effects on human health and technological properties. In this context, the accurate quantification of the milk polar lipids is crucial for comparison of different milk species, products, or dairy treatments. Although the official International Organization for Standardization-International Dairy Federation method for milk lipid extraction gives satisfactory results for neutral lipids, it has important disadvantages in terms of polar lipid losses. Other methods using mixtures of solvents such as chloroform:methanol are highly efficient for extracting polar lipids but are also associated with low sample throughput, long time, and large solvent consumption. As an alternative, we have optimized the milk fat extraction yield by using a pressurized liquid extraction (PLE) method at different temperatures and times in comparison with those traditional lipid extraction procedures using 2:1 chloroform:methanol as a mixture of solvents. Comparison of classical extraction methods with the developed PLE procedure were carried out using raw whole milk from different species (cows, ewes, and goats) and considering fat yield, fatty acid methyl ester composition, triacylglyceride species, cholesterol content, and lipid class compositions, with special attention to polar lipids such as phospholipids and sphingolipids. The developed PLE procedure was validated for milk fat extraction and the results show that this method performs a complete or close to complete extraction of all lipid classes and in less time than the official and Folch methods. In conclusion, the PLE method optimized in this study could be an alternative to carry out milk fat extraction as a routine method. Copyright © 2014 American Dairy Science Association. Published by

  14. High Pressure Extraction of Antioxidants from Solanum stenotomun Peel

    Directory of Open Access Journals (Sweden)

    Enrique J. Martínez de la Ossa

    2013-03-01

    Full Text Available In the work described here, two techniques for the recovery of anthocyanins from potato peel were studied and compared. One of the techniques employed was supercritical fluid extraction (SFE with pure CO2 or with CO2 and ethanol as cosolvent and the other technique was pressurized liquid extraction (PLE, where the solvent used was ethanol in water acidified to pH 2.6. The effects of pressure and temperature were studied and the anthocyanin contents obtained were statistically analyzed. In SFE the use of low pressure (100 bar and high temperature (65 °C was desirable for the anthocyanin extraction. With PLE the anthocyanin contents are increased considerably, and the best yields were obtained at 100 bar and 80 °C. This result is in correspondence with antioxidant activity index values (1.66 obtained in a DPPH antioxidant activity assay. In the extracts obtained with PLE the phenolic compounds were also determined, but the main compounds presented in the extract are anthocyanins.

  15. Obtaining anthocyanin-rich extracts from frozen açai (Euterpe oleracea Mart. pulp using pressurized liquid extraction

    Directory of Open Access Journals (Sweden)

    Sylvia Carolina ALCÁZAR-ALAY

    Full Text Available Abstract Açai is considered a functional food, and in addition to being a source of energy and fiber, it is a valuable source of bioactive compounds such as anthocyanins, minerals and fatty acids. In the present work, antioxidant-rich extracts from açai pulp were obtained using pressurized liquid extraction (PLE. The effects of the independent variables, including solvent type (pure ethanol and ethanol/water (50:50 v/v, citric acid (0 and 0.3%, w/w, pressure (20 and 80 bar and temperature (30 and 60 °C were evaluated using a full factorial design. The extraction was affected primarily by the solvent type and the citric acid percentage. The results indicate that the maximum overall yield (X0 was 64± 9 (%, d.b. when the process was performed using ethanol (99.5% and citric acid (0.3% w/w. The maximum total anthocyanin content and anthocyanin recovered from the raw material were 7 ± 1 (mg anthocyanin/g extract, d.b. and 11 ± 2 (%, d.b., respectively.

  16. Chemical composition of mate tea leaves (Ilex paraguariensis): a study of extraction methods.

    Science.gov (United States)

    Assis Jacques, Rosângela; dos Santos Freitas, Lisiane; Flores Peres, Valéria; Dariva, Cláudio; de Oliveira, José Vladimir; Bastos Caramão, Elina

    2006-12-01

    The objective of this work was to investigate the extraction of Ilex paraguariensis leaves by means of three extraction techniques: pressurized liquid extraction (PLE, also called accelerated solvent extraction--ASE), maceration, and sonication. Samples of mate tea leaves were collected from an experiment conducted under agronomic control at Indfistria e Comércio de Erva-Mate Barão LTDA, Brazil. Six solvents with increasing polarities (n-hexane, toluene, dichloromethane, ethyl acetate, acetone, and methanol) were used in this investigation. Chemical analysis of the extracts was performed by GC coupled with a mass spectrometer detector. The identification and quantification were accomplished by coinjections of certified standards. The results showed that no significant differences in the qualities of the extracts were noticed regarding the extraction methods. On the other hand, the PLE technique was found to be more effective for the extractions of caffeine, phytol, palmitic, and stearic acid. The use of PLE led to a significant decrease in the total extraction time, amount of solvent consumption, and manipulation of samples compared to maceration and ultrasound-assisted extraction methods.

  17. Sequential high pressure extractions applied to recover piceatannol and scirpusin B from passion fruit bagasse.

    Science.gov (United States)

    Viganó, Juliane; Aguiar, Ana C; Moraes, Damila R; Jara, José L P; Eberlin, Marcos N; Cazarin, Cinthia B B; Maróstica, Mário R; Martínez, Julian

    2016-07-01

    Passion fruit seeds are currently discarded on the pulp processing but are known for their high piceatannol and scirpusin B contents. Using pressurized liquid extraction (PLE), these highly valuable phenolic compounds were efficiently extracted from defatted passion fruit bagasse (DPFB). PLE was performed using mixtures of ethanol and water (50 to 100% ethanol, w/w) as solvent, temperatures from 50 to 70°C and pressure at 10MPa. The extraction methods were compared in terms of the global yield, total phenolic content (TPC), piceatannol content and the antioxidant capacity of the extracts. The DPFB extracts were also compared with those from non-defatted passion fruit bagasse (nDPFB). Identification and quantification of piceatannol were performed using UHPLC-MS/MS. The results showed that high TPC and piceatannol content were achieved for the extracts obtained from DPFB through PLE at 70°C and using 50 and 75% ethanol as the solvent. The best PLE conditions for TPC (70°C, 75% ethanol) resulted in 55.237mgGAE/g dried and defatted bagasse, whereas PLE at 70°C and 50% ethanol achieved 18.590mg of piceatannol/g dried and defatted bagasse, and such yields were significantly higher than those obtained using conventional extraction techniques. The antioxidant capacity assays showed high correlation with the TPC (r>0.886) and piceatannol (r>0.772). The passion fruit bagasse has therefore proved to be a rich source of piceatannol and PLE showed high efficiency to recover phenolic compounds from defatted passion fruit bagasse. Copyright © 2016 Elsevier Ltd. All rights reserved.

  18. Extraction and analysis of intact glucosinolates--a validated pressurized liquid extraction/liquid chromatography-mass spectrometry protocol for Isatis tinctoria, and qualitative analysis of other cruciferous plants.

    Science.gov (United States)

    Mohn, Tobias; Cutting, Brian; Ernst, Beat; Hamburger, Matthias

    2007-09-28

    Glucosinolates have attracted significant interest due to the chemopreventive properties of some of their transformation products. Numerous protocols for the extraction and analysis of glucosinolates have been published, but limited effort has been devoted to optimize and validate crucial extraction parameters and sample preparation steps. We carried out a systematic optimization and validation of a quantitative assay for the direct analysis of intact glucosinolates in Isatis tinctoria leaves (woad, Brassicaceae). Various parameters such as solvent composition, particle size, temperature, and number of required extraction steps were optimized using pressurized liquid extraction (PLE). We observed thermal degradation of glucosinolates at temperatures above 50 degrees C, and loss of >60% within 10min at 100 degrees C, but no enzymatic degradation in the leaf samples at ambient temperature. Excellent peak shape and resolution was obtained by reversed-phase chromatography on a Phenomenex Aqua column using 10mM ammonium formate as ion-pair reagent. Detection was carried out by electrospray ionisation mass spectrometry in the negative ion mode. Analysis of cruciferous vegetables and spices such as broccoli (Brassica oleracea L. var. italica), garden cress (Lepidium sativum L.) and black mustard (Sinapis nigra L.) demonstrated the general applicability of the method.

  19. Development of a high performance liquid chromatography method and a liquid chromatography-tandem mass spectrometry method with pressurized liquid extraction for simultaneous quantification and confirmation of cyromazine, melamine and its metabolites in foods of animal origin

    International Nuclear Information System (INIS)

    Yu Huan; Tao Yanfei; Chen Dongmei; Wang Yulian; Liu Zhaoying; Pan Yuanhu; Huang Lingli; Peng Dapeng; Dai Menghong; Liu Zhenli; Yuan Zonghui

    2010-01-01

    Simple and sensitive methods have been developed for simultaneous detection of cyromazine, melamine and their metabolites (ammeline, ammelide and cyanuric acid) in samples of animal origins. These include a high performance liquid chromatography (HPLC) method and a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method and are useful in regular monitoring and in toxicity studies of these molecules. Representative samples used in this study include muscles and livers of swine, bovine, sheep and chicken, kidneys of swine, bovine and sheep, and milk powder. A new sample preparation procedure with pressurized liquid extraction (PLE) at 1400 psi and 70 deg. C was investigated. Quantification of these five compounds by HPLC was achieved using an APS-2 column with UV detection at 230 nm. Limit of detection (LOD) was at 10 μg kg -1 , and limit of quantification (LOQ) was at 40 μg kg -1 . Recoveries of the five analytes in spiked samples ranged from 72.2% to 115.4% with RSD less than 12%. Confirmatory analysis of the analytes was performed using LC-MS/MS in selected reaction monitoring (SRM) mode. The LOD and LOQ were 5 μg kg -1 and 15 μg kg -1 , respectively. This is the first simultaneous analysis of cyromazine, melamine, ammeline, ammelide and cyanuric acid residues in complex tissue samples using PLE and HPLC. It is expected that these methods will find many practical applications in evaluating the safety of cyromazine, melamine and their metabolites.

  20. Evaluation of Carbohydrates in Natural and Cultured Cordyceps by Pressurized Liquid Extraction and Gas Chromatography Coupled with Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Jia Guan

    2010-06-01

    Full Text Available Free and polymeric carbohydrates in Cordyceps, a valued edible mushroom and well-known traditional Chinese medicine, were determined using stepwise pressurized liquid extraction (PLE extraction and GC-MS. Based on the optimized PLE conditions, acid hydrolysis and derivatization, ten monosaccharides, namely rhamnose, ribose, arabinose, xylose, mannose, glucose, galactose, mannitol, fructose and sorbose in 13 samples of natural and cultured Cordyceps were qualitatively and quantitatively analyzed and compared with myo-inositol hexaacetate as internal standard. The results showed that natural C. sinensis contained more than 7.99% free mannitol and a small amount of glucose, while its polysaccharides were usually composed of mannose, glucose and galactose with a molar ratio of 1.00:16.61~3.82:1.60~1.28. However, mannitol in cultured C. sinensis and cultured C. militaris were less than 5.83%, and free glucose was only detected in a few samples, while their polysaccharides were mainly composed of mannose, glucose and galactose with molar ratios of 1.00:3.01~1.09:3.30~1.05 and 1.00:2.86~1.28:1.07~0.78, respectively. Natural and cultured Cordyceps could be discriminated by hierarchical clustering analysis based on its free carbohydrate contents.

  1. Use of micro-emulsions in liquid-liquid extraction

    International Nuclear Information System (INIS)

    Komornicki, Jacques

    1982-01-01

    As liquid-liquid extraction of metallic cations is an important method of separation and concentration of metals present in diluted aqueous solutions, and as the extraction rate is limited by one or several steps of matter transfer at the liquid-liquid interface, the extraction kinetics can be improved by creating a wide surface interface and by allowing an increased reactivity between species. In this research thesis, the author aims at determining to which extent systems of interface with a wide surface obtained by using for example amphiphile molecules to create micro-emulsions, can be used as reaction media for physical-chemical processes of liquid-liquid extraction. He also aims at identifying their applicability limitations and problems which might arise with their application. The author notably focuses of the liquid-liquid extraction of metallic cations exhibiting particularly slow extraction kinetics

  2. Green Extraction of Antioxidants from Different Varieties of Red Grape Pomace

    Directory of Open Access Journals (Sweden)

    María José Otero-Pareja

    2015-05-01

    Full Text Available The extraction yield, phenolic content, anthocyanin content and antioxidant activity of extracts from different varieties of red grapes, Cabernet Sauvignon, Merlot, Petit Verdot, Syrah, Tempranillo and Tintilla, using pressurized green solvents have been analyzed. Two techniques were studied and compared: supercritical fluid extraction (SFE with CO2 + 20% ethanol and pressurized liquid extraction (PLE with either ethanol, water or an ethanol/water mixture as the extraction solvents. The Petit Verdot variety allowed the highest global and phenolic yield, and antioxidant activity. The best conditios for PLE obtained from the experimental design and kinetic study were 50% ethanol/water as the pressurized solvent at 90 bar, 120 °C, a flow rate of 5 g/min and, an extraction time of 90 min. A statistical analysis of variance has been performed and it was found that temperature is the only variable that has a statistical influence on the extraction yield. The antioxidant activity levels of the extracts are very promising and they are similar to those obtained with the antioxidant tocopherol.

  3. Green extraction of antioxidants from different varieties of red grape pomace.

    Science.gov (United States)

    Otero-Pareja, María José; Casas, Lourdes; Fernández-Ponce, María Teresa; Mantell, Casimiro; Martínez de la Ossa, Enrique J

    2015-05-26

    The extraction yield, phenolic content, anthocyanin content and antioxidant activity of extracts from different varieties of red grapes, Cabernet Sauvignon, Merlot, Petit Verdot, Syrah, Tempranillo and Tintilla, using pressurized green solvents have been analyzed. Two techniques were studied and compared: supercritical fluid extraction (SFE) with CO2 + 20% ethanol and pressurized liquid extraction (PLE) with either ethanol, water or an ethanol/water mixture as the extraction solvents. The Petit Verdot variety allowed the highest global and phenolic yield, and antioxidant activity. The best conditios for PLE obtained from the experimental design and kinetic study were 50% ethanol/water as the pressurized solvent at 90 bar, 120 °C, a flow rate of 5 g/min and, an extraction time of 90 min. A statistical analysis of variance has been performed and it was found that temperature is the only variable that has a statistical influence on the extraction yield. The antioxidant activity levels of the extracts are very promising and they are similar to those obtained with the antioxidant tocopherol.

  4. Implementasi Pendekatan Personal Learning Environtments (PLE dalam Praktikum Fisika

    Directory of Open Access Journals (Sweden)

    Paramita Ayuningtyas

    2017-06-01

    Full Text Available Abstract The background of this quasy experimental research is the lack of students’ independency in carrying out experiments, the low integration of information technology to explore student ability, also PLE approach that has not been widely implemented in learning. The purpose of this research, which is implemented PLE approach in the physics experiment to increase: independent and experiment abilities also the skill to make experiment report of high school student. The research was conducted from April until May 2015 at senior high school at Yogyakarta. The results of the research show that implementation PLE in the experiment: affect students in the determine the converging lens focus; in adjust theory and experimental purpose; and to conclude the experimental process and report. Keywords: Personal Learning Environtments, physics experiment, independent. Abstrak Penelitian eksperimen ini dilatarbelakangi kekurang mandirian siswa berpraktikum, kurang maksimalnya peran teknologi informasi untuk menggali potensi siswa, serta pendekatan PLE yang belum banyak diimplementasikan di pembelajaran. Sedangkan tujuan penelitian ini yaitu mengimplementasikan pendekatan PLE pada praktikum fisika untuk meningkatkan kemandirian, kemampuan praktikum serta keterampilan membuat laporan praktikum fisika pada siswa SMA. Penelitian dilakukan bulan April hingga Mei 2015 di SMA Negeri 3 Yogyakarta. Hasil penelitian menunjukkan implementasi PLE dalam praktikum: mempengaruhi kemampuan siswa menentukan fokus lensa cembung; menghubungkan dasar teori dengan tujuan praktikum; dan menyimpulkan hasil praktikum (proses maupun laporan. Kata kunci: Personal Learning Environtments, praktikum fisika, kemandirian.

  5. 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....

  6. May I Suggest? Comparing Three PLE Recommender Strategies

    Science.gov (United States)

    Modritscher, Felix; Krumay, Barbara; El Helou, Sandy; Gillet, Denis; Nussbaumer, Alexander; Albert, Dietrich; Dahn, Ingo; Ullrich, Carsten

    2011-01-01

    Personal learning environment (PLE) solutions aim at empowering learners to design (ICT and web-based) environments for their learning activities, mashing-up content and people and apps for different learning contexts. Widely used in other application areas, recommender systems can be very useful for supporting learners in their PLE-based…

  7. May I Suggest? Comparing Three PLE Recommender Strategies

    Directory of Open Access Journals (Sweden)

    Felix Mödritscher

    2011-11-01

    Full Text Available Personal learning environment (PLE solutions aim at empowering learners to design (ICT and web-based environments for their learning activities, mashingup content and people and apps for different learning contexts. Widely used in other application areas, recommender systems can be very useful for supporting learners in their PLE-based activities, to help discover relevant content, peers sharing similar learning interests or experts on a specific topic. In this paper we examine the utilization of recommender technology for PLEs. However, being confronted by a variety of educational contexts we present three strategies for providing PLE recommendations to learners. Consequently, we compare these recommender strategies by discussing their strengths and weaknesses in general.

  8. Polybrominated diphenyl ethers (PBDEs) contents in house and car dust of Portugal by pressurized liquid extraction (PLE) and gas chromatography-mass spectrometry (GC-MS).

    Science.gov (United States)

    Cunha, S C; Kalachova, K; Pulkrabova, J; Fernandes, J O; Oliveira, M B P P; Alves, A; Hajslova, J

    2010-03-01

    Dust is the repository of various compounds including flame retardants. In this study an analytical method based on PLE extraction and gas chromatography-mass spectrometry was selected for the analysis of 16 PBDEs congeners in house and car dust samples collected in Portugal. The analytical performance of the method was validated using standard reference material (SRM); values from 90% to 109% and from 2% to 11% were obtained for recovery and precision, respectively. The PBDE congeners distribution in whole and sieved fractions of the dust samples, as well as influence of the source on the levels of these contaminants, were obtained. The wide range of PBDEs contents found in the dust samples indicates heterogeneous levels of contamination in these matrices. The clearest feature of the results obtained was that Deca-BDE was the main PBDE in both house and car dust samples. The total PBDEs measured in house dust (ranging from 34 to 1928 ng g(-1)) was lower than those found in car dust (ranging from 193 to 22955 ng g(-1)). However, house dust provides a major contribution to human exposure due to the time spent there, much higher than in cars. Copyright (c) 2009 Elsevier Ltd. All rights reserved.

  9. Multi-residue determination of the sorption of illicit drugs and pharmaceuticals to wastewater suspended particulate matter using pressurised liquid extraction, solid phase extraction and liquid chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Baker, David R; Kasprzyk-Hordern, Barbara

    2011-11-04

    Presented is the first comprehensive study of drugs of abuse on suspended particulate matter (SPM) in wastewater. Analysis of SPM is crucial to prevent the under-reporting of the levels of analyte that may be present in wastewater. Analytical methods to date analyse the aqueous part of wastewater samples only, removing SPM through the use of filtration or centrifugation. The development of an analytical method to determine 60 compounds on SPM using a combination of pressurised liquid extraction, solid phase extraction and liquid chromatography coupled with tandem mass spectrometry (PLE-SPE-LC-MS/MS) is reported. The range of compounds monitored included stimulants, opioid and morphine derivatives, benzodiazepines, antidepressants, dissociative anaesthetics, drug precursors, and their metabolites. The method was successfully validated (parameters studied: linearity and range, recovery, accuracy, reproducibility, repeatability, matrix effects, and limits of detection and quantification). The developed methodology was applied to SPM samples collected at three wastewater treatment plants in the UK. The average proportion of analyte on SPM as opposed to in the aqueous phase was 10% with regard to methadone, EDDP, EMDP, BZP, fentanyl, nortramadol, norpropoxyphene, sildenafil and all antidepressants (dosulepin, amitriptyline, nortriptyline, fluoxetine and norfluoxetine). Consequently, the lack of SPM analysis in wastewater sampling protocol could lead to the under-reporting of the measured concentration of some compounds. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Pressurized liquid extraction using water/isopropanol coupled with solid-phase extraction cleanup for industrial and anthropogenic waste-indicator compounds in sediment

    Science.gov (United States)

    Burkhardt, M.R.; ReVello, R.C.; Smith, S.G.; Zaugg, S.D.

    2005-01-01

    A broad range of organic compounds is recognized as environmentally relevant for their potential adverse effects on human and ecosystem health. This method was developed to better determine the distribution of 61 compounds that are typically associated with industrial and household waste as well as some that are toxic and known (or suspected) for endocrine-disrupting potential extracted from environmental sediment samples. Pressurized liquid extraction (PLE) coupled with solid-phase extraction (SPE) was used to reduce sample preparation time, reduce solvent consumption to one-fifth of that required using dichloromethane-based Soxhlet extraction, and to minimize background interferences for full scan GC/MS analysis. Recoveries from spiked Ottawa sand, commercially available topsoil, and environmental stream sediment, fortified at 4-720 ??g per compound, averaged 76 ?? 13%. Initial method detection limits for single-component compounds ranged from 12.5 to 520 ??g/kg, based on 25 g samples. Results from 103 environmental sediment samples show that 36 out of 61 compounds (59%) were detected in at least one sample with concentrations ranging from 20 to 100,000 ??g/kg. The most frequently detected compound, beta-sitosterol, a plant sterol, was detected in 87 of the 103 (84.5%) environmental samples with a concentration range 360-100,000 ??g/kg. Results for a standard reference material using dichloromethane Soxhlet-based extraction are also compared. ?? 2004 Published by Elsevier B.V.

  11. Comparative Study of Green Sub- and Supercritical Processes to Obtain Carnosic Acid and Carnosol-Enriched Rosemary Extracts with in Vitro Anti-Proliferative Activity on Colon Cancer Cells

    Directory of Open Access Journals (Sweden)

    Andrea del Pilar Sánchez-Camargo

    2016-12-01

    Full Text Available In the present work, four green processes have been compared to evaluate their potential to obtain rosemary extracts with in vitro anti-proliferative activity against two colon cancer cell lines (HT-29 and HCT116. The processes, carried out under optimal conditions, were: (1 pressurized liquid extraction (PLE, using an hydroalcoholic mixture as solvent at lab-scale; (2 Single-step supercritical fluid extraction (SFE at pilot scale; (3 Intensified two-step sequential SFE at pilot scale; (4 Integrated PLE plus supercritical antisolvent fractionation (SAF at pilot scale. Although higher extraction yields were achieved by using PLE (38.46% dry weight, this extract provided the lowest anti-proliferative activity with no observed cytotoxic effects at the assayed concentrations. On the other hand, extracts obtained using the PLE + SAF process provided the most active rosemary extracts against both colon cancer cell lines, with LC50 ranging from 11.2 to 12.4 µg/mL and from 21.8 to 31.9 µg/mL for HCT116 and HT-29, respectively. In general, active rosemary extracts were characterized by containing carnosic acid (CA and carnosol (CS at concentrations above 263.7 and 33.9 mg/g extract, respectively. Some distinct compounds have been identified in the SAF extracts (rosmaridiphenol and safficinolide, suggesting their possible role as additional contributors to the observed strong anti-proliferative activity of CA and CS in SAF extracts.

  12. Alternative oil extraction methods from Echium plantagineum L. seeds using advanced techniques and green solvents.

    Science.gov (United States)

    Castejón, Natalia; Luna, Pilar; Señoráns, Francisco J

    2018-04-01

    The edible oil processing industry involves large losses of organic solvent into the atmosphere and long extraction times. In this work, fast and environmentally friendly alternatives for the production of echium oil using green solvents are proposed. Advanced extraction techniques such as Pressurized Liquid Extraction (PLE), Microwave Assisted Extraction (MAE) and Ultrasound Assisted Extraction (UAE) were evaluated to efficiently extract omega-3 rich oil from Echium plantagineum seeds. Extractions were performed with ethyl acetate, ethanol, water and ethanol:water to develop a hexane-free processing method. Optimal PLE conditions with ethanol at 150 °C during 10 min produced a very similar oil yield (31.2%) to Soxhlet using hexane for 8 h (31.3%). UAE optimized method with ethanol at mild conditions (55 °C) produced a high oil yield (29.1%). Consequently, advanced extraction techniques showed good lipid yields and furthermore, the produced echium oil had the same omega-3 fatty acid composition than traditionally extracted oil. Copyright © 2017 Elsevier Ltd. All rights reserved.

  13. As, Cd, Cr, Ni and Pb pressurized liquid extraction with acetic acid from marine sediment and soil samples

    International Nuclear Information System (INIS)

    Moreda-Pineiro, Jorge; Alonso-Rodriguez, Elia; Lopez-Mahia, Purificacion; Muniategui-Lorenzo, Soledad; Prada-Rodriguez, Dario; Moreda-Pineiro, Antonio; Bermejo-Barrera, Adela; Bermejo-Barrera, Pilar

    2006-01-01

    Rapid leaching procedures by Pressurized Liquid Extraction (PLE) have been developed for As, Cd, Cr, Ni and Pb leaching from environmental matrices (marine sediment and soil samples). The Pressurized Liquid Extraction is completed after 16 min. The released elements by acetic acid Pressurized Liquid Extraction have been evaluated by inductively coupled plasma-optical emission spectrometry. The optimum multi-element leaching conditions when using 5.0 ml stainless steel extraction cells, were: acetic acid concentration 8.0 M, extraction temperature 100 deg. C, pressure 1500 psi, static time 5 min, flush solvent 60%, two extraction steps and 0.50 g of diatomaceous earth as dispersing agent (diatomaceous earth mass/sample mass ratio of 2). Results have showed that high acetic acid concentrations and high extraction temperatures increase the metal leaching efficiency. Limits of detection (between 0.12 and 0.5 μg g -1 ) and repeatability of the over-all procedure (around 6.0%) were assessed. Finally, accuracy was studied by analyzing PACS-2 (marine sediment), GBW-07409 (soil), IRANT-12-1-07 (cambisol soil) and IRANT-12-1-08 (luvisol soil) certified reference materials (CRMs). These certified reference materials offer certified concentrations ranges between 2.9 and 26.2 μg g -1 for As, from 0.068 to 2.85 μg g -1 for Cd, between 26.4 and 90.7 μg g -1 for Cr, from 9.3 to 40.0 μg g -1 for Ni and between 16.3 and 183.0 μg g -1 for Pb. Recoveries after analysis were between 95.7 and 105.1% for As, 96.2% for Cd, 95.2 and 100.6% for Cr, 95.7 and 103% for Ni and 94.2 and 105.5% for Pb

  14. Pressurized liquid extraction-gas chromatography-mass spectrometry analysis of fragrance allergens, musks, phthalates and preservatives in baby wipes.

    Science.gov (United States)

    Celeiro, Maria; Lamas, J Pablo; Garcia-Jares, Carmen; Llompart, Maria

    2015-03-06

    Baby wipes and wet toilet paper are specific hygiene care daily products used on newborn and children skin. These products may contain complexes mixtures of harmful chemicals. A method based on pressurized liquid extraction (PLE) followed by gas chromatography-mass spectrometry (GC-MS) has been developed for the simultaneous determination of sixty-five chemical compounds (fragrance allergens, preservatives, musks, and phthalates) in wipes and wet toilet paper for children. These compounds are legislated in Europe according Regulation EC No 1223/2009, being twelve of them banned for their use in cosmetics, and one of them, 3-iodo-2-propynyl butylcarbamate (IPBC), is banned in products intended for children under 3 years. Also, propyl-, and butylparaben will be prohibited in leave-on cosmetic products designed for application on the nappy area of children under 3 years from April 2015. PLE is a fast, simple, easily automated technique, which permits to integrate a clean-up step during the extraction process reducing analysis time and stages. The proposed PLE-based procedure was optimized on real non-spiked baby wipe samples by means of experimental design to study the influence on extraction of parameters such as extraction solvent, temperature, extraction time, and sorbent type. Under the selected conditions, the method was validated showing satisfactory linearity, and intra-day, and inter-day precision. Recoveries were between 80-115% for most of the compounds with relative standard deviations (RSD) lower than 15%. Finally, twenty real samples were analyzed. Thirty-six of the target analytes were detected, highlighting the presence of phenoxyethanol in all analyzed samples at high concentration levels (up to 0.8%, 800μgg(-1)). Methyl paraben (MeP), and ethyl paraben (EtP) were found in 40-50% of the samples, and the recently banned isobutyl paraben (iBuP) and isopropyl paraben (iPrP), were detected in one and seven samples, respectively, at concentrations between

  15. May I Suggest? Comparing Three PLE Recommender Strategies

    OpenAIRE

    Mödritscher, Felix; Krumay, Barbara; El Helou, Sandy; Gillet, Denis; Nussbaumer, Alexander; Albert, Dietrich; Dahn, Ingo; Ullrich, Carsten

    2011-01-01

    Personal learning environment (PLE) solutions aim at empowering learners to design (ICT and web-based) environments for their learning activities, mashingup content and people and apps for different learning contexts. Widely used in other application areas, recommender systems can be very useful for supporting learners in their PLE-based activities, to help discover relevant content, peers sharing similar learning interests or experts on a specific topic. In this paper we examine the utilizat...

  16. Liquid-liquid extraction in flow analysis: A critical review

    Energy Technology Data Exchange (ETDEWEB)

    Silvestre, Cristina I.C.; Santos, Joao L.M. [REQUIMTE, Servico de Quimica-Fisica, Faculdade de Farmacia, Universidade do Porto, R. Anibal Cunha, 164, 4099-030 Porto (Portugal); Lima, Jose L.F.C., E-mail: limajlfc@ff.up.pt [REQUIMTE, Servico de Quimica-Fisica, Faculdade de Farmacia, Universidade do Porto, R. Anibal Cunha, 164, 4099-030 Porto (Portugal); Zagatto, Elias A.G. [Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, P.O. Box 96, Piracicaba 13400-970 (Brazil)

    2009-10-12

    Liquid-liquid extractions (LLE) are a common sample pre-treatment in many analytical applications. This review aims at providing a critical overview of the distinct automated continuous flow-based approaches that were developed for liquid-liquid extraction with the purpose of pre-concentration and/or separation of multiple analytes, such as ultra-trace metal and metalloid species, phenolic compounds, surfactants, pharmaceuticals, etc., hyphenated with many detection technique such as UV/vis spectrophotometry, atomic spectrometric detection systems and luminescent detectors, including distinct extraction strategies and applications like single and multiple extraction schemes, wetting film extraction, supported liquid membrane extraction, back extraction, closed-loop systems and the utilisation of zone sampling, chromatomembranes and iterative reversal techniques. The analytical performance of the developed flow-based LLE methods and the influence of flow manifold components such as the segmenter, extraction coil and phase separator, is emphasised and object of discussion. An overall presentation of each system components, selectivity, advantages and shortcomings is carried out and exemplified with selected applications.

  17. The use of ultrasonic instrumentation in liquid/liquid extraction plant

    International Nuclear Information System (INIS)

    Asher, R.C.; Bradshaw, L.; Tolchard, A.C.

    1984-01-01

    Ultrasonic instruments can be used to determine many of the parameters of interest in a liquid/liquid extraction plant, eg liquid levels, the position of interfaces between immiscible liquids and the concentration of solutions. The determinations can often be made non-invasively. A number of instruments developed for a liquid/liquid extraction plant used for nuclear fuel reprocessing is described. These instruments have a wider application in liquid/liquid extraction plant in general. (author)

  18. Salting-out homogenous extraction followed by ionic liquid/ionic liquid liquid-liquid micro-extraction for determination of sulfonamides in blood by high performance liquid chromatography.

    Science.gov (United States)

    Liu, Zhongling; Yu, Wei; Zhang, Hanqi; Gu, Fanbin; Jin, Xiangqun

    2016-12-01

    Salting-out homogenous extraction followed by ionic liquid/ionic liquid dispersive liquid-liquid micro-extraction system was developed and applied to the extraction of sulfonamides in blood. High-performance liquid chromatography was applied to the determination of the analytes. The blood sample was centrifuged to obtain the serum. After the proteins in the serum were removed in the presence of acetonitrile, ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate, dipotassium hydrogen phosphate, ionic liquid 1-Hexyl-3-methylimidazolium hexafluorophosphate were added into the resulting solution. After the resulting mixture was ultrasonically shaken and centrifuged, the precipitate was separated. The acetonitrile was added in the precipitate and the analytes were extracted into the acetonitrile phase. The parameters affecting the extraction efficiency, such as volume of ionic liquid, amount of dipotassium hydrogen phosphate, volume of dispersant, extraction time and temperature were investigated. The limits of detection of sulfamethizole (STZ), sulfachlorpyridazine (SCP), sulfamethoxazole (SMX) and Sulfisoxazole (SSZ) were 4.78, 3.99, 5.21 and 3.77μgL -1 , respectively. When the present method was applied to the analysis of real blood samples, the recoveries of analytes ranged from 90.0% to 113.0% and relative standard deviations were lower than 7.2%. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. LIQUID-LIQUID EXTRACTION COLUMNS

    Science.gov (United States)

    Thornton, J.D.

    1957-12-31

    This patent relates to liquid-liquid extraction columns having a means for pulsing the liquid in the column to give it an oscillatory up and down movement, and consists of a packed column, an inlet pipe for the dispersed liquid phase and an outlet pipe for the continuous liquid phase located in the direct communication with the liquid in the lower part of said column, an inlet pipe for the continuous liquid phase and an outlet pipe for the dispersed liquid phase located in direct communication with the liquid in the upper part of said column, a tube having one end communicating with liquid in the lower part of said column and having its upper end located above the level of said outlet pipe for the dispersed phase, and a piston and cylinder connected to the upper end of said tube for applying a pulsating pneumatic pressure to the surface of the liquid in said tube so that said surface rises and falls in said tube.

  20. Membrane assisted liquid-liquid extraction of cerium

    International Nuclear Information System (INIS)

    Soldenhoff, K.M.

    2000-02-01

    Membrane assisted liquid-liquid extraction of cerium was investigated, with emphasis placed on the study of the reaction chemistry and the kinetics of non-dispersive solvent extraction and stripping with microporous membranes. A bulk liquid membrane process was developed for the purification of cerium(IV) from sulfate solutions containing other rare earth elements. The cerium process was studied in both a flat sheet contained liquid membrane configuration and with hollow fibre contactors. Di-2-ethylhexyl phosphoric acid (DEHPA) was identified as a suitable extractant for cerium(IV) from sulfuric acid solution, with due consideration of factors such as extraction ability, resistance to degradation, solvent selectivity and potential for sulfate transfer into a strip solution. A detailed study of the extraction of cerium(IV) with DEHPA defined the extraction reaction chemistry. The Ce/DEHPA/sulfate system was also investigated with a flat sheet bulk liquid membrane configuration, using both sulfuric and hydrochloric acid as receiver solutions. These tests identified that hydrophobic membranes provide better mass transfer for extraction and hydrophilic membranes are better for stripping. The presence of an impurity, mono 2-ethylhexyl phosphoric acid (MEHPA), was found to have a dramatic accelerating effect on the rate of the chemical extraction reaction. This was attributed to its higher interfacial activity and population compared to DEHPA, and the fact that MEHPA was also found to be an active carrier for cerium(IV). The mass transfer rate of membrane assisted extraction and stripping of cerium, using hydrophobic and hydrophilic microporous membranes, respectively, was investigated using a modified Lewis-type cell. It was quantitatively demonstrated that the extraction process was mainly controlled by membrane diffusion and the stripping process was controlled by the chemical reaction rate, with membrane diffusion becoming important at low distribution coefficients

  1. May I suggest? Three PLE recommender strategies in comparison

    OpenAIRE

    Mödritscher, Felix; Krumay, Barbara; El Helou, Sandy; Gillet, Denis; Nussbaumer, Alexander; Albert, Dietrich; Dahn, Ingo; Ullrich, Carsten

    2011-01-01

    Personal learning environment (PLE) solutions aim at empowering learners to design (ICT and web-based) environments for their activities in different learning contexts and even for transitions between these contexts. Hereby, recommender systems which are highly successful in other application areas comprise one relevant technology for supporting learners in PLE-based activities. In this paper we examine the utilization of recommender technology for PLEs. However, being confronted by a variety...

  2. Determination of pharmaceuticals in sewage sludge by pressurized liquid extraction (PLE) coupled to liquid chromatography-tandem mass spectrometry (LC-MS/MS).

    Science.gov (United States)

    Radjenović, J; Jelić, A; Petrović, M; Barceló, D

    2009-03-01

    In this study, we aimed at optimizing a sensitive and reliable method for a simultaneous determination of 31 pharmaceuticals belonging to predominant therapeutic classes identified in different types of sewage sludge proceeding from conventional and advanced wastewater treatment. Freeze-dried sewage sludge was extracted by pressurized liquid extraction technique using accelerated solvent extractor Dionex 300. In order to minimize interferences with matrix components and to preconcentrate target analytes, solid phase extraction was introduced in the method as a clean-up step. The entire method was validated for linearity, precision, accuracy, and method detection limits (MDLs). The method turned out to be specific, sensitive, and reliable for the analysis of sludge of different composition, type, and retention time in the process. The developed sample preparation protocol and previously published method for LC-MS/MS analysis (Gros et al., Talanta 70:678-690, 2006) were successfully applied to monitor the target pharmaceuticals in different types of sewage sludge, i.e., primary sludge, secondary sludge, treated sludge, and sludge proceeding from pilot-scale membrane bioreactors (MBRs) operating in parallel to the conventional activated sludge treatment. Among the investigated pharmaceuticals, 20 were detected in the sludge proceeding from full-scale installations, whereas the MBR sludge concentrations were below MDLs for several compounds. The highest concentrations were recorded for treated and primary sludge. For example, the mean concentration of ibuprofen in the digested sludge was 299.3 +/- 70.9 ng g(-1) dw, whereas in the primary sludge, it was enriched up to 741.1 ng g(-1) dw. Other pharmaceuticals detected at relatively high concentrations were diclofenac, erythromycin, glibenclamide, ketoprofen, ofloxacin, azithromycin (up to 380.7, 164.2, 190.7, 336.3, 454.7, 299.6 ng g(-1) dw in the primary sludge, respectively), gemfibrozil, loratidine, and fluoxetine (up

  3. Liquid-liquid extraction of plutonium(IV) in monoamide - ammonium ionic liquid mixture

    International Nuclear Information System (INIS)

    Rout, Alok; Venkatesan, K.A.; Antony, M.P.

    2016-01-01

    Room temperature ionic liquid (RTIL) can be regarded as a sustainable alternative to the conventional molecular diluent, n-dodecane (n-DD), in solvent extraction process. Replacement of volatile organic solvents by RTILs in solvent extraction could lead to inherently safer processes. As far as the cation is concerned, most of the studies reported in literature are focused on imidazolium-based ionic liquids. In contrast to imiadazolium ionic liquids, quarternary ammonium ionic liquids like trioctylmethylammonium chloride (Aliquat 336), trioctylmethylammonium nitrate etc., do not exhibit any cation exchange with the metal ions from aqueous phase during extraction. However, there is no report available in literature that emphasizes the application of trioctylmethylammonium bis(trifluoromethane-sulfonyl)imide ((N_1_8_8_8)(NTf_2)) ionic liquid, for the extraction of Pu(IV). In this paper, we report the advantages of using the ionic liquid, trioctylmethylammonium bis(trifluoromethanesulfonyl)imide ((N_1_8_8_8)(NTf_2)), as diluent, for the extraction of plutonium(IV) in DHOA/(N_1_8_8_8)(NTf_2)

  4. SISAK liquid-liquid extraction experiments with preseparated 257Rf

    International Nuclear Information System (INIS)

    Omtvedt, Jon Petter; Alstad, J.; Breivik, H.; Dyve, J.E.; Eberhardt, K.; Folden III, C.M.; Ginter, T.; Gregorich, K.E.; Hult, E.A.; Johansson, M.; Kirbach, U.W.; Lee, D.M.; Mendel, M.; Nahler, A.; Ninov, V.; Omtvedt, L.A.; Patin, J.B.; Skarnemark, G.; Stavsetra, L.; Sudowe, R.; Wiehl, N.; Wierczinski, B.; Wilk, P.A.; Zielinski, P.M.; Kratz, J.V.; Trautmann, N.; Nitsche, H.; Hoffman, D.C.

    2002-01-01

    The SISAK liquid-liquid extraction system was used to extract 4.0-s 257Rf. The 257Rf was produced in the reaction 208Pb(50Ti, 1n)257Rf with 237-MeV beam energy on target, separated in the Berkeley Gas-filled Separator (BGS) and transferred to a gas jet using the Recoil Transfer Chamber (RTC). The activity delivered by the gas jet was dissolved in 6-M HNO3 and Rf was extracted into 0.25-M dibutyl-phosphoric acid in toluene. This was the first time a transactinide, i.e., an element with Z >= 104, was extracted and unequivocally identified by the SISAK system. Thus, this pilot experiment demonstrates that the fast liquid-liquid extraction system SISAK, in combination with liquidscintillation detectors, can be used for investigating the chemical properties of the transactinides. The extraction result is in accordance with the behaviour shown by the Rf group IV homologues Zr and Hf

  5. Lessons Learnt from and Sustainability of Adopting a Personal Learning Environment & Network (Ple&N)

    Science.gov (United States)

    Tsui, Eric; Sabetzadeh, Farzad

    2014-01-01

    This paper describes the feedback from the configuration and deployment of a Personal Learning Environment & Network (PLE&N) tool to support peer-based social learning for university students and graduates. An extension of an earlier project in which a generic and PLE&N was deployed for all learners, the current PLE&N is a…

  6. SISAK liquid-liquid extraction experiments with preseparated {sup 257}Rf

    Energy Technology Data Exchange (ETDEWEB)

    Omtvedt, Jon Petter; Alstad, J.; Breivik, H. [University of Oslo, Department of Chemistry, Oslo (NO)] (and others)

    2002-06-01

    The SISAK liquid-liquid extraction system was used to extract 4.0-s {sup 257}Rf. The {sup 257}Rf was produced in the reaction {sup 208}Pb({sup 50}Ti, 1n){sup 257}Rf with 237-MeV beam energy on target, separated in the Berkeley Gas-filled Separator (BGS) and transferred to a gas jet using the Recoil Transfer Chamber (RTC). The activity delivered by the gas jet was dissolved in 6-M HNO{sub 3} and Rf was extracted into 0.25-M dibutyl-phosphoric acid in toluene. This was the first time a transactinide, i.e., an element with Z{>=}104, was extracted and unequivocally identified by the SISAK system. Thus, this pilot experiment demonstrates that the fast liquid-liquid extraction system SISAK, in combination with liquid-scintillation detectors, can be used for investigating the chemical properties of the transactinides. The extraction result is in accordance with the behaviour shown by the Rf group IV homologues Zr and Hf. (author)

  7. PLE-based instruction concept

    Science.gov (United States)

    Javorcik, Tomas

    2017-11-01

    The paper is aimed at the description of a PLE (Personal Learning Environment)-based teaching model suitable for implementation in the instruction of upper primary school students. The paper describes the individual stages of the model and its use of ICT (Information and Communication Technologies) tools. The Personal Learning Environment is a form of instruction which allows for the meaningful use of information and communication technologies (including mobile technologies) in their entirety.

  8. Liquid-Liquid Extraction in Systems Containing Butanol and Ionic Liquids – A Review

    OpenAIRE

    Kubiczek Artur; Kamiński Władysław

    2017-01-01

    Room-temperature ionic liquids (RTILs) are a moderately new class of liquid substances that are characterized by a great variety of possible anion-cation combinations giving each of them different properties. For this reason, they have been termed as designer solvents and, as such, they are particularly promising for liquid-liquid extraction, which has been quite intensely studied over the last decade. This paper concentrates on the recent liquid-liquid extraction studies involving ionic liqu...

  9. Personal Learning Environments (PLE) in the Academic Achievement of University Students

    Science.gov (United States)

    Gallego, Maria Jesus; Gamiz, Vanesa Maria

    2014-01-01

    The main purpose of this research is to analyze the elements that compose the PLE of pre-service teachers and to determine whether the composition of these environments is related to academic achievement in a course on Information and Communication Technologies in Education. The hypothesis is that a PLE with more components is related to a higher…

  10. Kinetic of liquid-liquid extraction for uranyl nitrate and actinides (III) and lanthanides (III) nitrates by amide extractants

    International Nuclear Information System (INIS)

    Toulemonde, V.; CEA Centre d'Etudes de la Vallee du Rhone, 30 -Marcoule

    1995-01-01

    The kinetics of liquid-liquid extraction by amide extractants have been investigated for uranyl nitrate (monoamide extractants), actinides (III) and lanthanides (III) nitrates (diamide extractants). The transfer of the metallic species from the aqueous phase to the organic phase was studied using two experimental devices: ARMOLLEX (Argonne Modified Lewis cell for Liquid Liquid Extraction) and RSC (Rotating Stabilized Cell). The main conclusions are: for the extraction of uranyl nitrate by DEHDMBA monoamide, the rate-controlling step is the complexation of the species at the interface of the two liquids. Thus, an absorption-desorption (according to Langmuir theory) reaction mechanism was proposed; for the extraction of actinides (III) and lanthanides (III) nitrates in nitric acid media by DMDBTDMA diamide, the kinetic is also limited by interfacial reactions. The behavior of Americium and Europium is very similar as fare as their reaction kinetics are concerned. (author)

  11. The Influence of Extractant TOA, Stirring Time on the Extraction ProcessLiquid-liquid, and Liquid Membrane on the Liquid Wastes Containing Cd

    International Nuclear Information System (INIS)

    Prayitno; Djoko-Sardjono; Nurimaniwati; Adhe-Helmayani

    2000-01-01

    The influence of extractant and stirring time on the reduction componentcadmium on liquid wastes has been investigated. The method of experimentalused the extraction with liquid membrane emulsion. The parameters to beinvestigated were extractant amount tri-n octylamine (TOA), duration ofstirring time. In this investigated, extractant amount was varied from 5 to25 % (v/v) TOA, duration of stirring time varied from 5 to minutes. Theresult of experimental can be concluded that the best condition obtained forreducing cadmium component was on extractant amount 20 % (v/v) TOA, stirringtime 25 minutes. The best condition for reducing the cadmium component wasefficiency factor 98.35%. (author)

  12. Plate performance in liquid-liquid extraction

    International Nuclear Information System (INIS)

    Wadkins, R.P.

    1984-01-01

    The relative effectiveness of perforated, nozzle, and burred plates from a capacity and extraction standpoint were studied in a pulsed liquid-liquid extraction system. The experiments were conducted in a 3.8 x 10 -2 m diameter column using a mixture of aluminum nitrate, nitric acid, and uranyl nitrate as the aqueous phase, and tributyl phosphate dissolved in AMSCO 125-90 W as the organic phase. The uranium was extracted from the aqueous phase to the organic phase. A standard cartridge was made for each type of plate and consisted of an assembly of plates spaced 5.08 x 10 -2 m apart. Each plate had 3.2 x 10 -3 m holes spaced on 6.1 x 10 -3 -m centers, and contained 23% free area. 16 references, 4 figures, 1 table

  13. Pressurized liquid extraction-gas chromatography-mass spectrometry for confirming the photo-induced generation of dioxin-like derivatives and other cosmetic preservative photoproducts on artificial skin.

    Science.gov (United States)

    Alvarez-Rivera, Gerardo; Llompart, Maria; Garcia-Jares, Carmen; Lores, Marta

    2016-04-01

    The stability and photochemical transformations of cosmetic preservatives in topical applications exposed to UV-light is a serious but poorly understood problem. In this study, a high throughput extraction and selective method based on pressurized liquid extraction (PLE) coupled to gas chromatography-mass spectrometry (GC-MS) was validated and applied to investigate the photochemical transformation of the antioxidant butylated hydroxytoluene (BHT), as well as the antimicrobials triclosan (TCS) and phenyl benzoate (PhBz) in an artificial skin model. Two sets of photodegradation experiments were performed: (i) UV-Irradiation (8W, 254nm) of artificial skin directly spiked with the target preservatives, and (ii) UV-irradiation of artificial skin after the application of a cosmetic cream fortified with the target compounds. After irradiation, PLE was used to isolate the target preservatives and their transformation products. The follow-up of the photodegradation kinetics of the parent preservatives, the identification of the arising by-products, and the monitorization of their kinetic profiles was performed by GC-MS. The photochemical transformation of triclosan into 2,8-dichloro-dibenzo-p-dioxin (2,8-DCDD) and other dioxin-like photoproducts has been confirmed in this work. Furthermore, seven BHT photoproducts, and three benzophenones as PhBz by-products, have been also identified. These findings reveal the first evidences of cosmetic ingredients phototransformation into unwanted photoproducts on an artificial skin model. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Kinetic of liquid-liquid extraction for uranyl nitrate and actinides (III) and lanthanides (III) nitrates by amide extractants; Cinetique d`extraction liquide-liquide du nitrate d`uranyle et des nitrates d`actinides (III) et de lanthanides (III) par des extractants a fonction amide

    Energy Technology Data Exchange (ETDEWEB)

    Toulemonde, V [CEA Centre d` Etudes Nucleaires de Saclay, 91 -Gif-sur-Yvette (France); [CEA Centre d` Etudes de la Vallee du Rhone, 30 -Marcoule (France). Dept. d` Exploitation du Retraitement et de Demantelement

    1995-12-20

    The kinetics of liquid-liquid extraction by amide extractants have been investigated for uranyl nitrate (monoamide extractants), actinides (III) and lanthanides (III) nitrates (diamide extractants). The transfer of the metallic species from the aqueous phase to the organic phase was studied using two experimental devices: ARMOLLEX (Argonne Modified Lewis cell for Liquid Liquid Extraction) and RSC (Rotating Stabilized Cell). The main conclusions are: for the extraction of uranyl nitrate by DEHDMBA monoamide, the rate-controlling step is the complexation of the species at the interface of the two liquids. Thus, an absorption-desorption (according to Langmuir theory) reaction mechanism was proposed; for the extraction of actinides (III) and lanthanides (III) nitrates in nitric acid media by DMDBTDMA diamide, the kinetic is also limited by interfacial reactions. The behavior of Americium and Europium is very similar as fare as their reaction kinetics are concerned. (author). 89 refs.

  15. Typography of Jože Plečnik

    Directory of Open Access Journals (Sweden)

    Klementina Možina

    2013-09-01

    Full Text Available ABSTRACTPurpose: This paper focuses on the typographic analysis of a small fairy tale book Makalonca designed by Plečnik, and on the analysis of its two reprints, which were unfortunately found to be inferior to the original design.Methodology/approach: The differences and inconsistencies between the original and the two reprints of Makalonca were studied in details by the means of a comparative analysis.Results: The architecture of Jože Plečnik (1872–1957 is well known throughout Europe, while his graphic design and typography are less known. During the Second World War he made all the decorations, vignettes and initials for the fairy tales and elaborated the graphic design for the book which was published in two different bindings – hardcover and paperback. Two paperback reprints were subsequently published as well, the first one a year after the architect’s death in 1958 and the second one in 1988, commemorating the centenary of the fairytales. In both reprints it was stressed that the graphic design remained the same as it was done by Plečnik. On the contrary, both reprints are deformations of the original. Not only that they are different in the book and layout size and typefaces, one even differs in the type style and type size of the body text. Moreover, there are also many other differences within the rest of the text, thus representing a great loss for the Slovenian cultural heritage.Research limitation: The research was hampered by difficulties in the accessibility and authentication of historical data of printing in Slovenia.Originality/practical implications: This is the first detailed typographic research of a smaller part of Plečnik’s graphic design. The typographic analysis and research results can be of use at the preparation of facsimile or authentic reprints important for our cultural heritage.

  16. Separation of Asphaltenes by Polarity using Liquid-Liquid Extraction

    DEFF Research Database (Denmark)

    Andersen, Simon Ivar

    1997-01-01

    In order to investigate the nature of petroleum asphaltenes in terms of polarity a process was developed using initial liquid-liquid extraction of the oil phase followed by precipitation of the asphaltenes using n-heptane. The liquid-liquid extraction was performed using toluene-methanol mixtures...... phase. The asphaltenes were analysed using FTir, Elemental analysis, and HPLC-SEC with a diode array detector. With increasing content of toluene in the methanol the molecular weight distribution of the asphaltenes significantly move to higher molecular weights. The content of nitrogen and sulfur...

  17. Liquid-Liquid Extraction in Systems Containing Butanol and Ionic Liquids – A Review

    Directory of Open Access Journals (Sweden)

    Kubiczek Artur

    2017-03-01

    Full Text Available Room-temperature ionic liquids (RTILs are a moderately new class of liquid substances that are characterized by a great variety of possible anion-cation combinations giving each of them different properties. For this reason, they have been termed as designer solvents and, as such, they are particularly promising for liquid-liquid extraction, which has been quite intensely studied over the last decade. This paper concentrates on the recent liquid-liquid extraction studies involving ionic liquids, yet focusing strictly on the separation of n-butanol from model aqueous solutions. Such research is undertaken mainly with the intention of facilitating biological butanol production, which is usually carried out through the ABE fermentation process. So far, various sorts of RTILs have been tested for this purpose while mostly ternary liquid-liquid systems have been investigated. The industrial design of liquid-liquid extraction requires prior knowledge of the state of thermodynamic equilibrium and its relation to the process parameters. Such knowledge can be obtained by performing a series of extraction experiments and employing a certain mathematical model to approximate the equilibrium. There are at least a few models available but this paper concentrates primarily on the NRTL equation, which has proven to be one of the most accurate tools for correlating experimental equilibrium data. Thus, all the presented studies have been selected based on the accepted modeling method. The reader is also shown how the NRTL equation can be used to model liquid-liquid systems containing more than three components as it has been the authors’ recent area of expertise.

  18. Use of ethyl lactate to extract bioactive compounds from Cytisus scoparius: Comparison of pressurized liquid extraction and medium scale ambient temperature systems.

    Science.gov (United States)

    Lores, Marta; Pájaro, Marta; Álvarez-Casas, Marta; Domínguez, Jorge; García-Jares, Carmen

    2015-08-01

    An important trend in the extraction of chemical compounds is the application of new environmentally friendly, food grade solvents. Ethyl lactate (ethyl 2-hydroxypropanoate), produced by fermentation of carbohydrates, is miscible with both hydrophilic and hydrophobic compounds being a potentially good solvent for bioactive compounds. Despite its relatively wide use as a general solvent, the utilization of ethyl lactate as an extraction solvent has only recently been considered. Here, we evaluate the possible use of ethyl lactate to extract phenolic compounds from wild plants belonging to Cytisus scoparius, and we compare the characteristics of the extracts obtained by Pressurized Solvent Extraction (the total phenolics content, the antioxidant activity and the concentration of the major polyphenols) with those of other extracts obtained with methanol. In order to explore the industrial production of the ethyl lactate Cytisus extract, we also evaluate medium scale ambient temperature setups. The whole plant and the different parts (flowers, branches, and seed pods) were evaluated separately as potential sources of polyphenols. All extracts were analyzed by LC-MS/MS for accurate identification of the major polyphenols. Similar phenolic profiles were obtained when using ethyl lactate or methanol. The main bioactives found in the Cytisus extract were the non-flavonoid phenolic compounds caffeic and protocatechuic acids and 3,4-dihydroxybenzaldehyde; the flavonoids rutin, kaempferol and quercetin; the flavones chrysin, orientin and apigenin; and the alkaloid lupanine. Regarding the comparison of the extraction systems, although the performance of the PLE was much better than that of the ambient-temperature columns, the energy consumption was also much higher. Ethyl lactate has resulted an efficient extraction solvent for polyphenols from C. scoparius, yielding extracts with high levels of plant phenolics and antioxidant activity. The antimicrobial activity of these

  19. Reduction of Hexavalent Chromium Using Sorbaria sorbifolia Aqueous Leaf Extract

    Directory of Open Access Journals (Sweden)

    Shashi Prabha Dubey

    2017-07-01

    Full Text Available Aqueous plant leaves extract (PLE of an abundant shrub, Sorbaria sorbifolia, was explored for the reduction of hexavalent chromium, Cr(VI, to trivalent chromium, Cr(III. The effect of contact time, pH, PLE quantity, ionic strength, hardness, temperature and effective initial Cr(VI ion concentration were tested; Cr(VI reduction followed the pseudo-first order rate kinetics and maximum reduction was observed at pH 2. Significantly, Cr(VI reduction efficacies varied from 97 to 66% over the pH range of 2 to 10, which bodes well for PLE to be used for the reduction of Cr(VI also at a higher pH. PLE-mediated Cr(VI reduction displays considerable efficiency at various ionic strengths; however, hardness strongly affects the reduction ability. Higher temperature significantly enhances the Cr(VI reduction. This study reveals the potential use of PLE as a green reducing agent in aqueous extract for the efficient reduction of Cr(VI to Cr(III.

  20. Transuranium element purification by liquid-liquid extraction

    International Nuclear Information System (INIS)

    Madic, C.; Koehly, G.

    1976-01-01

    In the transuranium element production, the liquid-liquid extraction purification is presented. The affinity of TBP and trilaurylammonium nitrate for these elements is given. Exemples of NP/Pu, Pu/Np, U/Pu, Am/Cm, Am and Cm/Ln separation are presented [fr

  1. Selective Activation of N,N'-Diacyl Rhodamine Pro-fluorophores Paired with Releasing Enzyme, Porcine Liver Esterase (PLE).

    Science.gov (United States)

    Abney, Kristopher K; Ramos-Hunter, Susan J; Romaine, Ian M; Godwin, J Shawn; Sulikowski, Gary A; Weaver, Charles David

    2018-04-21

    This study reports the synthesis and testing of a family of rhodamine pro-fluorophores and an enzyme capable of converting pro-fluorophores to Rhodamine 110. We prepared a library of simple N,N'-diacyl rhodamines and investigated Porcine Liver Esterase (PLE) as an enzyme to activate rhodamine-based pro-fluorophores. A PLE-expressing cell line generated an increase in fluorescence rapidly upon pro-fluorophore addition demonstrating the rhodamine pro-fluorophores are readily taken up and fluorescent upon PLE-mediated release. Rhodamine pro-fluorophore amides trifluoroacetamide (TFAm) and proponamide (PAm) appeared to be the best substrates using a cell-based assay using PLE expressing HEK293. Our pro-fluorophore series showed diffusion into live cells and resisted endogenous hydrolysis. The use of our engineered cell line containing the exogenous enzyme PLE demonstrated the rigorousness of amide masking when compared to cells not containing PLE. This simple and selective pro-fluorophore rhodamine pair with PLE offers the potential to be used in vitro and in vivo fluorescence based assays. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. An inkjet-printed microfluidic device for liquid-liquid extraction.

    Science.gov (United States)

    Watanabe, Masashi

    2011-04-07

    A microfluidic device for liquid-liquid extraction was quickly produced using an office inkjet printer. An advantage of this method is that normal end users, who are not familiar with microfabrication, can produce their original microfluidic devices by themselves. In this method, the printer draws a line on a hydrophobic and oil repellent surface using hydrophilic ink. This line directs a fluid, such as water or xylene, to form a microchannel along the printed line. Using such channels, liquid-liquid extraction was successfully performed under concurrent and countercurrent flow conditions. © The Royal Society of Chemistry 2011

  3. 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...

  4. Ionic Liquids as Extraction Media for Metal Ions

    Science.gov (United States)

    Hirayama, Naoki

    In solvent extraction separation of metal ions, recently, many researchers have investigated possible use of hydrophobic ionic liquids as extraction media instead of organic solvents. Ionic liquids are salts of liquid state around room temperature and can act not only as solvents but also as ion-exchangers. Therefore, the extraction mechanism of metal ions into ionic liquids is complicated. This review presents current overview and perspective on evaluation of nature of hydrophobic ionic liquids as extraction media for metal ions.

  5. Quality Parameters of Curcuma Longa L. Extracts by Supercritical Fluid Extraction (SFE) and Ultrasonic Assisted Extraction (UAE)

    International Nuclear Information System (INIS)

    Zaibunnisa Abdul Haiyee; Siti Hafsah Mohd Shah; Khudzir Ismail; Nooraain Hashim; Wan Iryani Wan Ismail

    2016-01-01

    Turmeric is one of the prominently use herbal plants due to its diverse beneficial effects especially in Indian medicine. The rhizome part of the turmeric contains valuable compounds which have been said to owe its antimicrobial effects, anti-cancer, anti-inflammatory and enhance wound healing. Due to its short-life span and perishable properties, the conversion of the rhizome into turmeric extract is desirable. Several methods have been used for extraction such as Soxhlet extraction and pressurized liquid extraction (PLE). However, these techniques are tedious, laborious, time consuming and involves the usage of toxic organic solvent, of which safeness of the end product is doubtful. In this study, a rapid, reliable and green extraction method of supercritical fluid extraction (SFE) and ultrasonic assisted extraction (UAE) were used. SFE without modifier has resulted in 0.0006 mg/ 100 g of curcuminoids concentration and 5.62 % of yield (dry weight basis). UAE using ethanol was able to produce significantly the highest yield (6.40 %, dry weight basis) and the highest curcuminoids concentration (0.1020 mg/ 100 g). However, SFE was able to produce extract that contain significantly higher major volatile compounds; tumerone, ar-turmerone and curlone. Therefore, this study proves that both extraction methods were able to produce high quality turmeric extract. (author)

  6. Enhanced biological activities of gamma-irradiated persimmon leaf extract.

    Science.gov (United States)

    Cho, Byoung-Ok; Nchang Che, Denis; Yin, Hong-Hua; Jang, Seon-Il

    2017-09-01

    The aim of this study was to compare the anti-oxidative and anti-inflammatory activities of gamma-irradiated persimmon leaf extract (GPLE) with those of non-irradiated persimmon leaf extract (PLE). Ethanolic extract of persimmon leaf was exposed to gamma irradiation at a dose of 10 kGy. After gamma irradiation, the color of the extract changed from dark brown to light brown. The anti-oxidative and anti-inflammatory activities of GPLE and PLE were assessed from: total polyphenol and total flavonoid contents; 2,2-diphenyl-1-picrylhydrazyl (DPPH) assay; 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) assay, and levels of pro-inflammatory mediators such as nitric oxide (NO), prostaglandin E2 (PGE2), tumor necrosis factor alpha (TNF-α) and interleukin-6 (IL-6). The total polyphenol contents of GPLE and PLE were determined to be 224.44 ± 1.54 and 197.33 ± 5.81 mg gallic acid equivalents (GAE)/g, respectively, and the total flavonoid contents of GPLE and PLE were 206.27 ± 1.15 and 167.60 ± 2.00 mg quercetin equivalents (QUE)/g, respectively. The anti-oxidant activities of GPLE and PLE as measured by DPPH assays were 338.33 ± 30.19 μg/ml (IC50) and 388.68 ± 8.45 μg/ml (IC50), respectively, and those measured by ABTS assays were 510.49 ± 15.12 μg/ml (IC50) and 731.30 ± 10.63 μg/ml (IC50), respectively. IC50 is the inhibitor concentration that reduces the response by 50%. GPLE strongly inhibited the production of NO, PGE2 and IL-6 compared with PLE in lipopolysaccharide-stimulated RAW264.7 macrophages. Furthermore, GPLE significantly inhibited the production of TNF-α and IL-6 cytokines compared with PLE in phorbol 12-myristate 13-acetate (PMA) plus A23187-stimulated HMC-1 human mast cells. These results indicate that gamma irradiation of PLE can enhance its anti-oxidative and anti-inflammatory activities through elevation of the phenolic contents. Therefore, gamma-irradiated PLE has potential for use in the food and cosmetic

  7. PLE CATALYZED HYDROLYZES OF ALPHA-SUBSTITUTED ALPHA-HYDROXY ESTERS - THE INFLUENCE OF THE SUBSTITUENTS

    NARCIS (Netherlands)

    MOORLAG, H; KELLOGG, RM

    1991-01-01

    The enzymatic hydrolyses of a variety of alpha-substituted mandelic and lactic esters using pig liver esterase (PLE) have been investigated. High to moderate enantioselectivity was found for various alpha-substituted mandelic esters, whereas PLE showed low to no enantioselectivity for

  8. Ionizable polyethers as specific metal ion carriers in liquid-liquid extraction and liquid membrane separations

    International Nuclear Information System (INIS)

    Walkowiak, W.; Charewicz, W.A.; Bartsch, R.A.; Ndip, G.M.

    1988-01-01

    Consideration is given to results of investigations into competitive extraction and penetration through a liquid membrane of alkali and alkaline earth cations from aqueous solutions by a series of lipophilic and ionizable acyclic polyethers of various molecular structure. It is shown that specificity and selectiviy of cation carriers in liquid-liquid extraction and liquid membrane separation depend on molecular structure of acyclic polyethers

  9. E-PLE: an Algorithm for Image Inpainting

    Directory of Open Access Journals (Sweden)

    Yi-Qing Wang

    2013-12-01

    Full Text Available Gaussian mixture is a powerful tool for modeling the patch prior. In this work, a probabilisticview of an existing algorithm piecewise linear estimation (PLE for image inpainting is presentedwhich leads to several theoretical and numerical improvements based on an effective use ofGaussian mixture.

  10. Determination of Niacinamide in Lotions and Creams Using Liquid-Liquid Extraction and High-Performance Liquid Chromatography

    Science.gov (United States)

    Usher, Karyn M.; Simmons, Carolyn R.; Keating, Daniel W.; Rossi, Henry F., III

    2015-01-01

    Chemical separations are an important part of an undergraduate chemistry curriculum. Sophomore students often get experience with liquid-liquid extraction in organic chemistry classes, but liquid-liquid extraction is not as often introduced as a quantitative sample preparation method in honors general chemistry or quantitative analysis classes.…

  11. Graphic Design in Jože Plečnik’s Fairytales Makalonca

    Directory of Open Access Journals (Sweden)

    Klementina Možina

    2011-11-01

    Full Text Available This paper focuses on a small fairytale book Makalonca, which was completelydesigned by Jože Plečnik.The Slovenian architecture by Jože Plečnik (1872–1957 is well known in Europe,while his work in the area of graphic design and typography is less known. Duringthe Second World War, he made all the decorations, vignettes and initial letters forthe fairytales, and elaborated graphic design for the book published in two differentbindings – hardcover and paperback. Two paperback reprints were subsequentlypublished as well. In both reprints it was stressed that the graphic design remainedthe same as done by Plečnik. Instead, both reprints are actually deformations of theoriginal. As a consequence, the Slovenian cultural heritage has lost a great deal.

  12. Microsystems for liquid-liquid extraction of radionuclides in the analytical protocols

    International Nuclear Information System (INIS)

    Helle, Gwendolyne

    2014-01-01

    Radiochemical analyses are necessary to numerous steps for nuclear wastes management and for the control of the environment. An analytical protocol generally includes different steps of chemical separations which are lengthy, manual and complicated to implement because of their confinement in glove boxes and because of the hostile chemical and radiochemical media. Thus there is a huge importance to propose innovative and robust solutions to automate these steps but also to reduce the volumes of the radioactive and chemical wastes at the end of the analytical cycle. One solution consists in the miniaturization of the analyses through the use of lab-on-chip. The objective of this thesis work was to propose a rational approach to the conception of separative microsystems for the liquid-liquid extraction of radionuclides. To achieve this, the hydrodynamic behavior as well as the extraction performances have been investigated in one chip for three different chemical systems: Eu(III)-HNO 3 /DMDBTDMA, Eu(III)-AcO(H,Na)-HNO 3 /HDEHP and U(VI)-HCl/Aliquat336. A methodology has been developed for the implementation of the liquid-liquid extraction in micro-system for each chemical system. The influence of various geometric parameters such as channel length or specific interfacial area has been studied and the comparison of the liquid-liquid extraction performances has led to highlight the influence of the phases viscosities ratio on the flows. Thanks to the modeling of both hydrodynamics and mass transfer in micro-system, the criteria related to physical and kinetic properties of the chemical systems have been distinguished to propose a rational conception of tailor-made chips. Finally, several examples of the liquid-liquid extraction implementation in micro-system have been described for analytical applications in the nuclear field: U/Co separation by Aliquat336, Eu/Sm separation by DMDBTDMA or even the coupling between a liquid-liquid extraction chip and the system of

  13. Systeme im Einsatz. Lernmanagement, Kompetenzmanagement und PLE

    NARCIS (Netherlands)

    Kalz, Marco; Schön, Sandra; Lindner, Martin; Roth, Detlev; Baumgartner, Peter

    2011-01-01

    Kalz, M., Schön, S., Lindner, M., Roth, D., & Baumgartner, P. (2011). Systeme im Einsatz. Lernmanagement, Kompetenzmanagement und PLE. In M. Ebner, & S. Schön (Eds.), L3T - Lerhbuch für Lernen und Lehren mit Technologie (pp. 111-118). Graz, Austria: Uni Graz. Available at

  14. Kinetics of glycoalkaloid hydrolysis and solanidine extraction in liquid-liquid systems

    Directory of Open Access Journals (Sweden)

    Stanković Mihajlo Z.

    2002-01-01

    Full Text Available The kinetics of glycoalkaloid hydrolysis and solanidine extraction in Analyzed in this study. obtained from dried and milled potato haulm to to which hydrochlotic acid was added is the first liquid phase, while chloroform trichloroethylene or carbon tetrachlondeisthe second organic, liquid phase. The purpose of this paper was to combine the processes of glycoalkaloid hydrolysis to solanidine and solanidine extraction into one step, and to find the optimal liquid-liquid system for such a process.

  15. Primary metals extraction by liquid membranes

    International Nuclear Information System (INIS)

    Subramanian, K.N.

    1980-01-01

    The extraction of copper and uranium by liquid membranes is presented. The recovery of uranium from wet process phosphoric acid is described. The development of this process has progressed through three stages, firstly the chemistry of uranium extraction as it pertains to liquid membrane systems. This was followed by continuous extraction tests on fresh black acid and on aged acid. Results on a 1 litre/minute pilot plant demonstrated that the process could be operated with a minimum of feed pretreatment and about 90% of uranium could be extracted. The extraction of copper from copper leach liquors is also described. (U.K.)

  16. Liquid-liquid extraction kinetics of uranyl nitrate and actinides (III)-lanthanides nitrates by extractants with amide function

    International Nuclear Information System (INIS)

    Toulemonde, V.

    1995-01-01

    Nowadays, the most important part of electric power is generated by fission energy. But spent fuels have then to be reprocessed. The production of these reprocessed materials separately and with a high purity level is done according to a liquid-liquid extraction process (Purex process) with the use of tributyl phosphate as solvent. Optimization studies concerning the extracting agent have been undertaken. This work gives the results obtained for the uranyl nitrate and the actinides (III)-lanthanides (III) nitrates extraction by extractants with amide function (monoamide for U(VI) and diamide for actinides (III) and lanthanides (III)). The extraction kinetics have been studied in the case of a metallic specie transfer from the aqueous phase towards the organic phase. The experiments show that the nitrates extraction kinetics is limited by the complexation chemical reaction of the species at the interface between the two liquids. An adsorption-desorption interfacial reactional mechanism (Langmuir theory) is proposed for the uranyl nitrate. (O.M.)

  17. Liquid-liquid extraction by reversed micelles in biotechnological processes

    Directory of Open Access Journals (Sweden)

    Kilikian B. V.

    2000-01-01

    Full Text Available In biotechnology there is a need for new purification and concentration processes for biologically active compounds such as proteins, enzymes, nucleic acids, or cells that combine a high selectivity and biocompatibility with an easy scale-up. A liquid-liquid extraction with a reversed micellar phase might serve these purposes owing to its capacity to solubilize specific biomolecules from dilute aqueous solutions such as fermentation and cell culture media. Reversed micelles are aggregates of surfactant molecules containing an inner core of water molecules, dispersed in a continuous organic solvent medium. These reversed micelles are capable of selectively solubilizing polar compounds in an apolar solvent. This review gives an overview of liquid-liquid extraction by reversed micelles for a better understanding of this process.

  18. Effects of black hoof medicinal mushroom, phellinus linteus (Agaricomycetes), polysaccharide extract in streptozotocin-induced diabetic rats

    NARCIS (Netherlands)

    Yamaç, Mustafa; Zeytinoğlu, Melih; Şentürk, Hakan; Kartkaya, Kazim; Kanbak, Göngör; Bayramoğlu, Gökhan; Oğlakci, Ayşegül; Griensven, van Leo J.L.D.

    2016-01-01

    In this article we report the healing effects of a Phellinus linteus fruiting body hot water extract (PLE) in streptozotocin (STZ)–induced diabetic rats. PLE was given before and after STZ. The preprotective, protective, and postprotective effects of PLE on STZ-induced oxidative stress were

  19. The method for simultaneous extraction and back extraction in liquid three-phase system and equipment for simultaneous extraction and back extraction in liquid three-phase system

    International Nuclear Information System (INIS)

    Palyska, W.; Chmielewski, A.G.

    1992-01-01

    The method for simultaneous extraction and back extraction in liquid three-phase system has been worked out. The equipment designed for that process has been also subject of the patent. The interesting component is extracted first to intermediate phase consists of magnetic solvent keeping two extracting phases separately. The intermediate magnetic liquid has been kept in its position using a stable magnet maintained on the surface of the extraction vessel. Then the component pass from intermediate phase to the third phase as a result of back extraction. Mixing in the extraction and back extraction zones is organized by means of rotating shaft going along the whole apparatus. The extraction and back extraction processes occur simultaneously as a result of continuous flow of solvent in their zones. The single extraction back extraction facilities can be joined in larger batteries. 3 figs

  20. Hydrogen extraction from liquid lithium-lead alloy by gas-liquid contact method

    International Nuclear Information System (INIS)

    Xie Bo; Weng Kuiping; Hou Jianping; Yang Guangling; Zeng Jun

    2013-01-01

    Hydrogen extraction experiment from liquid lithium-lead alloy by gas-liquid contact method has been carried out in own liquid lithium-lead bubbler (LLLB). Experimental results show that, He is more suitable than Ar as carrier gas in the filler tower. The higher temperature the tower is, the greater hydrogen content the tower exports. Influence of carrier gas flow rate on the hydrogen content in the export is jagged, no obvious rule. Although the difference between experimental results and literature data, but it is feasible that hydrogen isotopes extraction experiment from liquid lithium-lead by gas-liquid contact method, and the higher extraction efficiency increases with the growth of the residence time of the alloy in tower. (authors)

  1. Separation of rare earths by liquid-liquid extraction

    International Nuclear Information System (INIS)

    Helgorsky, M.; Leveque, M.

    1978-01-01

    The elements of the rare earth family are characterised by very similar chemical properties connected with their special electronic structure. The purification of the rare earths sold by RHONE-POULENC is now done by the liquid-liquid extraction technique. The development of different extracting agents and also counter-current techniques have led to solvent extraction replacing the other fractionation techniques because of its efficiency and low cost. There are usually several possible solutions to the main problem of choosing the extracting agent and its mode of use. The difficulty is to find the most economical one taking account of the thermodynamic and hydrodynamic constraints of the solvent. It is shown how ideas about the separation have changed over the course of the development of the uses of the rare earths, ending finally in an integrated scheme that makes RHONE-POULENC a world leader of manufacturers of separated rare earths [fr

  2. AFM fluid delivery/liquid extraction surface sampling/electrostatic spray cantilever probe

    Science.gov (United States)

    Van Berkel, Gary J.

    2015-06-23

    An electrospray system comprises a liquid extraction surface sampling probe. The probe comprises a probe body having a liquid inlet and a liquid outlet, and having a liquid extraction tip. A solvent delivery conduit is provided for receiving solvent liquid from the liquid inlet and delivering the solvent liquid to the liquid extraction tip. An open liquid extraction channel extends across an exterior surface of the probe body from the liquid extraction tip to the liquid outlet. An electrospray emitter tip is in liquid communication with the liquid outlet of the liquid extraction surface sampling probe. A system for analyzing samples, a liquid junction surface sampling system, and a method of analyzing samples are also disclosed.

  3. Can the Integration of a PLE in an E-Portfolio Platform Improve Generic Competences?

    Science.gov (United States)

    Galván-Fernández, Cristina; Rubio-Hurtado, María José; Martínez-Olmo, Francesc; Rodríguez-Illera, José Luis

    2017-01-01

    The study analyzes the improvement in generic competences through e-portfolio/PLE platform and didactic planning. The new version of the platform, Digital Folder, contains utilities for students and teachers and some PLE components that help the learning process through e-portfolios. Didactic planning is compared for students from the University…

  4. Polymorphous light eruption (PLE) and a new potent antioxidant and UVA-protective formulation as prophylaxis.

    Science.gov (United States)

    Hadshiew, I M; Treder-Conrad, C; v Bülow, R; Klette, E; Mann, T; Stäb, F; Moll, I; Rippke, F

    2004-08-01

    Polymorphous light eruption (PLE) is the most common photodermatosis. While its etiology still remains elusive, pathogenesis seems to involve UVA-induced oxidative stress and subsequent deregulation of antioxidative immune responses. Only few and often ineffective prophylactic and therapeutic measures exist to date. In our randomized, double-blind, placebo-controlled clinical study, we compared the efficacy of a new topical formulation, consisting of 0.25%alpha-glucosylrutin (AGR) (a natural, modified flavonoid), 1% tocopheryl acetate (vitamin E) and a broad-spectrum, highly UVA-protective sunscreen (SPF 15) in a hydrodispersion gel vehicle, to a sunscreen-only gel and vehicle. Thirty patients with a history of PLE were pretreated with either the above formulation, a similar preparation (with the same concentration for vitamin E and AGR, but a different UV filter system), placebo or a SPF 15 sunscreen-only gel, 30 min prior to daily photoprovocation with UVA irradiations of 60-100 J/cm(2) to 5 x 5 cm(2) areas on the upper arms. After 4 days, results revealed a statistically highly significant difference (PPLE. While only one patient developed clinical signs of PLE with accompanying itch in the area treated with the new antioxidant UV-protective gel formulation, 62.1% of the placebo-treated areas and 41.3% of the sunscreen-only treated areas showed mild to moderate signs of PLE. Combining a potent antioxidant with a broad-spectrum, highly UVA-protective sunscreen is far more effective in preventing PLE than sunscreen alone or placebo and should thus be employed as the prophylaxis of choice for PLE.

  5. Glycerol-based deep eutectic solvents as extractants for the separation of MEK and ethanol via liquid-liquid extraction

    NARCIS (Netherlands)

    Rodriguez, N.R.; Ferré Güell, J.; Kroon, M.C.

    2016-01-01

    Four different glycerol-based deep eutectic solvents (DESs) were tested as extracting agents for the separation of the azeotropic mixture {methyl ethyl ketone + ethanol} via liquid-liquid extraction. The selected DESs for this work were: glycerol/choline chloride with molar ratios (4:1) and (2:1),

  6. Liquid-liquid extraction and separation studies of uranium(VI)

    International Nuclear Information System (INIS)

    Langade, A.D.; Shinde, V.M.

    1980-01-01

    Separation of uranium(VI) from iron(III), molybdenum(VI), vanadium(V), bismuth(III), zirconium(IV) and thorium(IV) is achieved by liquid-liquid extraction with 4-methyl-3-pentene-2-one (mesityl oxide; MeO) from sodium salicylate media (0.1M, pH 6.0). The extracted species is UO 2 (HO.C 6 H 4 COO) 2 .2MeO. A procedure for separating 50 μg of uranium from mg amounts of the other metals is described. (author)

  7. Ionic liquid based dispersive liquid-liquid microextraction for the extraction of pesticides from bananas.

    Science.gov (United States)

    Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Asensio-Ramos, María; Rodríguez-Delgado, Miguel Angel

    2009-10-23

    This paper describes a dispersive liquid-liquid microextraction (DLLME) procedure using room temperature ionic liquids (RTILs) coupled to high-performance liquid chromatography with diode array detection capable of quantifying trace amounts of eight pesticides (i.e. thiophanate-methyl, carbofuran, carbaryl, tebuconazole, iprodione, oxyfluorfen, hexythiazox and fenazaquin) in bananas. Fruit samples were first homogenized and extracted (1g) with acetonitrile and after suitable evaporation and reconstitution of the extract in 10 mL of water, a DLLME procedure using 1-hexyl-3-methylimidazolium hexafluorophosphate ([C(6)MIM][PF(6)]) as extraction solvent was used. Experimental conditions affecting the DLLME procedure (sample pH, sodium chloride percentage, ionic liquid amount and volume of disperser solvent) were optimized by means of an experimental design. In order to determine the presence of a matrix effect, calibration curves for standards and fortified banana extracts (matrix matched calibration) were studied. Mean recovery values of the extraction of the pesticides from banana samples were in the range of 69-97% (except for thiophanate-methyl and carbofuran, which were 53-63%) with a relative standard deviation lower than 8.7% in all cases. Limits of detection achieved (0.320-4.66 microg/kg) were below the harmonized maximum residue limits established by the European Union (EU). The proposed method, was also applied to the analysis of this group of pesticides in nine banana samples taken from the local markets of the Canary Islands (Spain). To the best of our knowledge, this is the first application of RTILs as extraction solvents for DLLME of pesticides from samples different than water.

  8. Hybrid Multiphase CFD Solver for Coupled Dispersed/Segregated Flows in Liquid-Liquid Extraction

    Directory of Open Access Journals (Sweden)

    Kent E. Wardle

    2013-01-01

    Full Text Available The flows in stage-wise liquid-liquid extraction devices include both phase segregated and dispersed flow regimes. As a additional layer of complexity, for extraction equipment such as the annular centrifugal contactor, free-surface flows also play a critical role in both the mixing and separation regions of the device and cannot be neglected. Traditionally, computional fluid dynamics (CFD of multiphase systems is regime dependent—different methods are used for segregated and dispersed flows. A hybrid multiphase method based on the combination of an Eulerian multifluid solution framework (per-phase momentum equations and sharp interface capturing using Volume of Fluid (VOF on selected phase pairs has been developed using the open-source CFD toolkit OpenFOAM. Demonstration of the solver capability is presented through various examples relevant to liquid-liquid extraction device flows including three-phase, liquid-liquid-air simulations in which a sharp interface is maintained between each liquid and air, but dispersed phase modeling is used for the liquid-liquid interactions.

  9. Synergistic extraction of europium(III) in ammonium ionic liquid

    International Nuclear Information System (INIS)

    Rout, Alok; Venkatesan, K.A.; Antony, M.P.

    2016-01-01

    Room temperature ionic liquids have been receiving increased attention for possible applications in the area of nuclear fuel reprocessing and waste management due to their fascinating properties such as good ionicity, high solvation capability, properties tunable etc. Most of the studies in the literature on the extraction of metal ions with molecular extractants dissolved in ionic liquid diluents are making use of the hydrophobic ionic liquids containing imidazolium cations such as the 1-alkyl-3-methylimidazolium ion. From an environmental point of view, such ionic liquids are not suitable as the primary mode of the metal extraction is by cation exchange mechanism wherein ionic liquid cation is lost to the aqueous phase leading to aqueous contamination and issue of recyclability of organic phase. However, there are some hydrophobic ionic liquids such as trioctylmethylammonium chloride ((N 1888 )(Cl)), and trihexyl(tetradecyl)phoshonium chloride (Cyphos IL 101) that exhibit no cation exchange in the aqueous phase during extraction. In this context, the extraction behavior of europium(III) using a neutral extractant, octyl, phenyl-N.N-diisobutylmethylcarbamoylphophinoxide (CMPO) and/or an acidic extractant bis(ethylhexyl)phosphoric acid (D2EHPA) dissolved in the ammonium ionic liquid diluent, trioctylmethylammonium bis(trifluoromethanesulfonyl)imide, (N 1888 )(NTf 2 ). The extraction behavior of CMPO (or D2EHPA)/(N 1888 )((Tf 2 ) system was investigated as a function of different extraction parameters such as feed acidity, extractant concentration, equilibration time etc.

  10. Solid-Liquid Separation Properties of Thermoregulated Dicationic Ionic Liquid as Extractant of Dyes from Aqueous Solution

    Directory of Open Access Journals (Sweden)

    Rui Lv

    2018-01-01

    Full Text Available Two thermoregulated dicationic ionic liquids were synthesized and applied for effective extraction of the common dye malachite green oxalate (MG. The extraction parameters such as amount of ionic liquids, pH of water phase, extraction time, cooling time, and centrifugal time on the extraction efficiency were investigated systematically. It revealed that the dye has been successfully extracted into the ionic liquids, with high extraction efficiency higher than 98%, and recovery of 98.2%–100.8%, respectively. Furthermore, these ionic liquids can be recycled easily after elution. The reusable yields were 87.1% and 88.7%. The extraction of the dye into the thermoregulated ionic liquid provides a method of minimizing pollution of waste water potentially.

  11. Extraction by means of emulsified liquid membranes; Extraction par membranes liquides emulsionnees (MLE)

    Energy Technology Data Exchange (ETDEWEB)

    Pareau, D.; Stambouli, M. [Ecole Centrale de Paris, 75 (France)

    2006-12-15

    It is an alternative of the liquid-liquid extraction process where extraction and stripping are simultaneously carried out. The stripping solution is dispersed in the solvent in micro-droplets. This emulsion, stabilised by a surface-active agent, is then dispersed in the liquid to be treated and, during that step, the metal is transferred to the stripping solution, moving through the solvent which operates as an organic membrane. The paper describes in detail the mechanism of the process, its advantages and its disadvantages. Its field of applications is wide, but only a few units are now industrially in operation, most of them exists only at the pilot scale. It is particularly adapted for the treatment of effluents with a very low content in metallic impurities. As examples, the paper describes the recovery of zinc from viscose plant effluents (Lenzing plant, Austria) and the removal of free cyanide ions and cyanide metallic complexes (pilot scale). (authors)

  12. Personal Learning Environments (PLE in the Bachelor’s Degree in Elementary Education at the University of Granada

    Directory of Open Access Journals (Sweden)

    Eduardo Chaves-Barboza

    2017-12-01

    Full Text Available This paper studies the devices that university students in teacher education incorporate into their personal learning environments (PLE. It also examines the time that students dedicate to activities related to ICT, the factors that encourage or frustrate the incorporation of tools to students’ PLE, and the characteristics that this population desires for a PLE. For this, a questionnaire has been applied using Likert scales in a sample of 668 students divided into 15 groups, enrolled in the Elementary Education Bachelor’s degree program, at the University of Granada, Spain. The data were analyzed using descriptive and inferential statistics (with 95% confidence interval. Also, correlation tests (Kendall coefficient τ and analysis of variance (test of Kruskal-Wallis H were employed. The results showed that laptops and smartphones are the most accessible devices for students. The findings also showed that students spend little time to visiting university platforms, they prefer PLE tools to be productive and to allow them to connect with others, and they want PLE to be interactive, customizable and useful.

  13. Application of liquid-liquid extraction in uranium hydrometallurgy (Paper No. : V-1)

    Energy Technology Data Exchange (ETDEWEB)

    Murthy, T K.S.; Koppiker, K S

    1979-01-01

    Uranium recovery from the ores is carried out exclusively by hydrometallurgical techniques. The initial solubilisation of uranium is achieved by either sodium carbonate or sulphuric acid leaching, the latter being more common. Further purification and upgrading of uranium from the sulphate liquors is carried out by an ion-exchange process. Solid resin type anion exchangers or liquid ion-exchangers are employed. The processing of uranium liquors is, perhaps, the first major application of liquid-liquid extraction in metal recovery. Organophosphoric acids were initially used but later the long-chain aliphatic amines have superseded them. The amine extraction system has been widely studied and several variations are now known. Chloride, nitrate, carbonate or sulphate or acid stripping can be used for getting back the uranium into the aqueous phase. Combination of ion exchange (resin type) and solvent extraction processes called Eluex processes are developed for special applications. Studies have also been made of solvent extraction of uranium from leach pulps instead of clear liquors. Tributylphosphate has found wide application in the refining of uranium concentrates to meet the stringent needs of nuclear purity. liquid-liquid extraction is, perhaps, the only successful technique for the recovery of uranium, as by-product, from wet-process phosphoric acid. This has opened up a new source of uranium.

  14. Reprints of Jože Plečnik’s Fairytales Makalonca

    Directory of Open Access Journals (Sweden)

    Klementina Možina

    2012-12-01

    Full Text Available This paper focuses on a small fairytale book entitled Makalonca, completely designed by Jože Plečnik, and its two reprints, which were unfortunately found inferior to the original design.The Slovenian architecture by Jože Plečnik (1872–1957 is well known in Europe, while his work in the area of graphic design and typography is less known. During the Second World War he made all the decorations, vignettes and initial letters for fairytales and elaborated graphic design for the book. Two paperback reprints were subsequently published as well; one a year after the architect’s death in 1958 and another in 1988, commemorating the centenary of the fairytales.In both reprints it was stressed that the graphic design remained the same as done by Plečnik. However, both reprints are deformations of the original. Not only are they different in book and layout size, typefaces, one even in the type style and type size of the body text, but there are also many other differences to be found within the rest of the text. In consequence, the Slovenian cultural heritage has lost a great deal.

  15. Application of solid-liquid extraction separation in analytical chemistry: Pt. 1

    International Nuclear Information System (INIS)

    Xu Zulan; Dai Lixin

    1985-01-01

    Low m.p. waxes as solid solvents for solid-liquid extraction separation are advanced. Uranium in aqueous phase is extracted by homogeneous organic phase which is composed of waxes and various kinds of extractants. Various parameters of this extraction separation method are studied and compared with one of liquid-liquid extraction. The characteristic of wax as solvent, speciality and applicability of solid-liquid extraction separation method are evaluated

  16. Uranium Extraction From Artificial Liquid Waste Using Continuous Extraction Liquid membrane Technique

    International Nuclear Information System (INIS)

    Rusdianasari; Buchari

    2002-01-01

    The continuous extraction of uranium from artificial liquid waste by emulsion liquid membrane was carried out using one stage mixer-settler. This emulsion liquid membrane containing di-2-ethylhexylphosphoric acid (D2EHPA) and tri-n-buthyl phosphate (TBP) as carrier were carried out using one stage mixer-settler. The optimum condition gave the ratio of emulsion velocity to the feed velocity 1:4 and steady state reached after five minutes. The optimum condition was obtained at the 90.91 % of uranium recovered from raffinate, using EDTA as the masking agent with concentration 5x10 - 2 M . The total concentration of carrier was 3% with ratio D2EHPA and TBP 3:1. The emulsion liquid membrane has high relative selectivity after steady state with separation factors were α U , N i= 115,43 and α U , Fe 328,55. The result of experiment showed that emulsion liquid membrane containing D2EHPA and TBP as carrier have good performance for continuous system

  17. The pedagogical practices of a teacher of Portuguese Foreign Language (PLE in immersion and non-immersion context

    Directory of Open Access Journals (Sweden)

    Nildicéia Aparecida Rocha

    2016-05-01

    Full Text Available The aim of this paper is to present a reflection on the specifics of teaching Portuguese as a Foreign Language (PLE both in the context of immersion and outside it, from the observations carried out in two stages: first, the practice of a teacher PLE will be described in immersion situation at a university in the state of São Paulo, Brazil; and then practice the same teacher in a course of PLE out of the immersion context, at a university in Spain, in a provincial capital. In this sense, the teaching practice will be analyzed from a teacher of PLE in immersion situation and beyond when the didactic and pedagogical treatment of the inseparable relationship between language and culture within an intercultural communicative approach. It is a qualitative research in which it is a case of state, showing the practice of one teacher (research subjects in two socio-historically different contexts, but with the same approach. The survey results indicate that the teacher's practice in non-immersion context had to be re-signified to enable PLE learning in such a context. In fact, the teacher had to redefine their practice and deconstruct a belief and turn to the theory, according to their didactic and pedagogical and linguistic concerns, finding that the examination of social, historical and cultural data should always be the guiding and / or determinants as regards the teaching of a foreign language, in particular PLE out of immersion.

  18. PLE-wu, a new member of piggyBac transposon family from insect, is active in mammalian cells.

    Science.gov (United States)

    Wu, Chunxiao; Wang, Shu

    2014-10-01

    piggyBac, a highly active transposon in insect and mammalian cells, is a very useful tool in genome manipulation. A new piggyBac-like element (PLE), named PLE-wu, was identified from a mutant baculovirus cultured in sf9 insect cells. This new transposon is 2931 bp in length and encodes two active forms of transposase, a 708-amino acid-long transposase and a short 576-residue-long transposase translated from a downstream in-frame initiation codon. PLE-wu has asymmetric terminal structures, containing 6-bp inverted terminal repeats, 32-bp imperfect inverted and direct sub-terminal repeats. Similar to piggyBac, PLE-wu exhibits traceless excision activity in both insect and mammalian cells, restoring the original TTAA target sequence upon excision. It also retains the insertion activity in mammalian cells with a plasmid to chromosome transposition rate about 10-fold higher than random integration. Plasmid rescue assays revealed that the TTAA target sequence was duplicated at the junctions of the insertion site. Deletion of the terminal sequences including the sub-terminal repeats decreased the transposition activity of the 708-residue-long transposase, while the transposition activity of the short form of transposase was not affected. With its low sequence similarity to piggyBac, PLE-wu will contribute to the understanding the mechanism of PLE transposition, as well as design of new transposon systems with higher activity. Copyright © 2014 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

  19. SYNTHESE D’EXTRACTANTS ACIDES HEXADECYL- ET DECYLAMINOBIMETHYLENEDIPHOSPHONIQUES APPLICATION A L’EXTRACTION LIQUIDE-LIQUIDE DE Ni (II

    Directory of Open Access Journals (Sweden)

    M.A DIDI

    2007-06-01

    Après purification puis caractérisation des produits, nous avons réalisé divers tests d’extraction liquide - liquide de Ni (II en milieu sulfaté. Le temps d’équilibre déterminé par étude cinétique a été fixé à 40 minutes. Les paramètres changeant tels la température ( T = 20°C, 30°C et 50°C, le rapport du nombre de moles (n extractant / n métal (Q =1 à 6 et le rapport des volumes (Vaq / Vorg= 1, 2, 3 et 4 ont permis de maximiser le rendement d’extraction qui est de 46% avec le HABMP et de 44% pour le DADMP et ceci pour des extractions à un seul plateau.

  20. Ionic liquids used in extraction and separation of metal ions

    International Nuclear Information System (INIS)

    Shen Xinghai; Xu Chao; Liu Xinqi; Chu Taiwei

    2006-01-01

    Ionic liquids as green solvents now have become a research hotspot in the field of separation of metal ions by solvent extraction. Experimental results of extraction of various metal ions with ionic liquids as solvents, including that of alkali metals, alkaline earths, transition metals rare earths and actinides are introduced. The extraction of uranium, plutonium and fission products that are involved in spent nuclear fuel reprocessing is also reviewed. The possible extraction mechanisms are discussed. Finally, the prospect of replacement of volatile and/or toxic organic solvents with environmentally benign ionic liquids for solvent extraction and the potency of applications of ionic liquids in solvent extraction are also commented. (authors)

  1. Novel thiosalicylate-based ionic liquids for heavy metal extractions

    Energy Technology Data Exchange (ETDEWEB)

    Leyma, Raphlin; Platzer, Sonja [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, A-1090 Vienna (Austria); Jirsa, Franz [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, A-1090 Vienna (Austria); Department of Zoology, University of Johannesburg, PO Box 524, Auckland Park, 2006, Johannesburg (South Africa); Kandioller, Wolfgang, E-mail: wolfgang.kandioller@univie.ac.at [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, A-1090 Vienna (Austria); Krachler, Regina; Keppler, Bernhard K. [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, A-1090 Vienna (Austria)

    2016-08-15

    Highlights: • Six thiosalicylate-based ammonium and phosphonium ionic liquids (ILs) were newly synthesized. • ILs showed good extraction of cadmium, copper, and zinc. • Phosphonium ILs showed better extraction efficiencies than their ammonium counterparts. - Abstract: This study aims to develop novel ammonium and phosphonium ionic liquids (ILs) with thiosalicylate (TS) derivatives as anions and evaluate their extracting efficiencies towards heavy metals in aqueous solutions. Six ILs were synthesized, characterized, and investigated for their extracting efficacies for cadmium, copper, and zinc. Liquid-liquid extractions of Cu, Zn, or Cd with ILs after 1–24 h using model solutions (pH 7; 0.1 M CaCl{sub 2}) were assessed using flame atomic absorption spectroscopy (F-AAS). Phosphonium-based ILs trihexyltetradecylphosphonium 2-(propylthio)benzoate [P{sub 66614}][PTB] and 2-(benzylthio)benzoate [P{sub 66614}][BTB] showed best extraction efficiency for copper and cadmium, respectively and zinc was extracted to a high degree by [P{sub 66614}][BTB] exclusively.

  2. Growth of TiC films by Pulsed Laser Evaporation (PLE) and characterization by XPS and AES

    International Nuclear Information System (INIS)

    Rist, O.; Murray, P.T.

    1991-01-01

    Thin films of TiC with a thickness of some 100 nm have been grown on Si(100) substrates by Pulsed Laser Evaporation (PLE). Advantages of PLE in comparison with more conventional growth methods e.g. PVD or CVD are reported. The feasibility of growing stoichiometric thin films of TiC by PLE was investigated. These films produced have been analysed in situ by X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES). XPS results and Auger sputter depht profiles indicate that the films grown between RT and 500degC are stoichiometric TiC. Film/substrate interdiffusion is observed at 600degC substrate temperature and higher. (orig.)

  3. Plečnik’s concept of planning the rehabilitation of Ljubljana

    Directory of Open Access Journals (Sweden)

    Andreja Jan

    2001-01-01

    Full Text Available Most of Plečnik’s work was achieved in the strict urban core, mainly on the edge joining the historical medieval core with the new city. Plečnik gradually created a composition of places surrounding the old city that became important connecting elements between the medieval and modern city, at that time in its first development surge. From his work it is clear that he achieved his imaginary city gradually and methodically, with architectural emphasis and based on ties between particular key places in the city. He recognised these key spaces in the city, tied them together with axes and merged them into the present urban tissue.

  4. Metal extraction by solid-liquid agglomerates

    International Nuclear Information System (INIS)

    Fuller, E.F.

    1980-01-01

    Dissolved metal values are extracted from a liquid e.g. uranium from phosphoric acid by contacting the liquid with agglomerates for a time to load the agglomerate with the metal value, separating the loaded agglomerates from the liquid phase and stripping the metal value from the loaded agglomerate. The agglomerate may be made by combining finely divided solid particles with a binding liquid to form a paste, adding a suspending liquid to form a mixture, the suspending liquid and binding liquid being immiscible in each other and the solid particles being insoluble in the suspending liquid and shearing the mixture to form the agglomerate. (author)

  5. Alkylsulfate-based ionic liquids in the liquid–liquid extraction of aromatic hydrocarbons

    International Nuclear Information System (INIS)

    García, Silvia; Larriba, Marcos; García, Julián; Torrecilla, José S.; Rodríguez, Francisco

    2012-01-01

    Highlights: ► Values of α 2,1 for the four R-SO 4 ionic liquids are higher than those of sulfolane. ► Values of D 2 for all the ionic liquids are lower than those of sulfolane. ► Values of D 2 for [emim][C 2 H 5 SO 4 ] are the highest among the R-SO 4 ionic liquids. - Abstract: The (liquid + liquid) equilibrium data (LLE) for the extraction of toluene from heptane with different ionic liquids (ILs) based on the alkylsulfate anion (R-SO 4 ) was determined at T = 313.2 K and atmospheric pressure. The effect of more complex R-SO 4 anions on capacity of extraction and selectivity in the liquid–liquid extraction of toluene from heptane was studied. The ternary systems were formed by {heptane + toluene + 1,3-dimethylimidazolium methylsulfate ([mmim][CH 3 SO 4 ]), 1-ethyl-3-methylimidazolium hydrogensulfate ([emim][HSO 4 ]), 1-ethyl-3-methylimidazolium methylsulfate ([emim][CH 3 SO 4 ]), or 1-ethyl-3-methylimidazolium ethylsulfate ([emim][C 2 H 5 SO 4 ])}. The degree of quality of the experimental LLE data was ascertained by applying the Othmer–Tobias correlation. The phase diagrams for the ternary systems were plotted, and the tie lines correlated with the NRTL model compare satisfactorily with the experimental data.

  6. Cone-shaped membrane liquid phase micro extraction

    International Nuclear Information System (INIS)

    Hong, Heng See; Sanagi, M.M.; Ibrahim, W.A.W.; Naim, A.A.

    2008-01-01

    A novel sample pre-treatment technique termed cone-shaped membrane liquid phase micro extraction (CSM-LPME) was developed and combined with micro-liquid chromatography (micro-LC) for the determination of selected pesticides in water samples. Several important extraction parameters such as types of extraction solvent, agitation rate, pH value, total exposure time and effect of salt and humic acids were investigated and optimized. Enrichment factors of >50 folds were easily achieved within 20 min of extraction. The new developed method demonstrated an excellent performance in terms of speed, cost effectiveness, reproducibility, as well as exceptional low detection limits. Current work provides a great interest to further investigate on the applicability of the CSM-LPME technique in analytical chemistry and explores the possibility of replacing conventional extraction techniques such as soxhlet, solid phase extraction (SPE) and solid phase micro extraction (SPME). (author)

  7. Pesticide extraction from table grapes and plums using ionic liquid based dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Herrera-Herrera, Antonio V; Rodríguez-Delgado, Miguel Angel

    2009-12-01

    Room temperature ionic liquids (RTILs) have been used as extraction solvents in dispersive liquid-liquid microextraction (DLLME) for the determination of eight multi-class pesticides (i.e. thiophanate-methyl, carbofuran, carbaryl, tebuconazole, iprodione, oxyfluorfen, hexythiazox, and fenazaquin) in table grapes and plums. The developed method involves the combination of DLLME and high-performance liquid chromatography with diode array detection. Samples were first homogenized and extracted with acetonitrile. After evaporation and reconstitution of the extract in water containing sodium chloride, a quick DLLME procedure that used the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate ([C(6)MIM][PF(6)]) and methanol was developed. The RTIL dissolved in a very small volume of acetonitrile was directed injected in the chromatographic system. The comparison between the calibration curves obtained from standards and from spiked sample extracts (matrix-matched calibration) showed the existence of a strong matrix effect for most of the analyzed pesticides. A recovery study was also developed with five consecutive extractions of the two types of fruits spiked at three concentration levels. Mean recovery values were in the range of 72-100% for table grapes and 66-105% for plum samples (except for thiophanate-methyl and carbofuran, which were 64-75% and 58-66%, respectively). Limits of detection (LODs) were in the range 0.651-5.44 microg/kg for table grapes and 0.902-6.33 microg/kg for plums, representing LODs below the maximum residue limits (MRLs) established by the European Union in these fruits. The potential of the method was demonstrated by analyzing 12 commercial fruit samples (six of each type).

  8. Design of guanidinium ionic liquid based microwave-assisted extraction for the efficient extraction of Praeruptorin A from Radix peucedani.

    Science.gov (United States)

    Ding, Xueqin; Li, Li; Wang, Yuzhi; Chen, Jing; Huang, Yanhua; Xu, Kaijia

    2014-12-01

    A series of novel tetramethylguanidinium ionic liquids and hexaalkylguanidinium ionic liquids have been synthesized based on 1,1,3,3-tetramethylguanidine. The structures of the ionic liquids were confirmed by (1)H NMR spectroscopy and mass spectrometry. A green guanidinium ionic liquid based microwave-assisted extraction method has been developed with these guanidinium ionic liquids for the effective extraction of Praeruptorin A from Radix peucedani. After extraction, reversed-phase high-performance liquid chromatography with UV detection was employed for the analysis of Praeruptorin A. Several significant operating parameters were systematically optimized by single-factor and L9 (3(4)) orthogonal array experiments. The amount of Praeruptorin A extracted by [1,1,3,3-tetramethylguanidine]CH2CH(OH)COOH is the highest, reaching 11.05 ± 0.13 mg/g. Guanidinium ionic liquid based microwave-assisted extraction presents unique advantages in Praeruptorin A extraction compared with guanidinium ionic liquid based maceration extraction, guanidinium ionic liquid based heat reflux extraction and guanidinium ionic liquid based ultrasound-assisted extraction. The precision, stability, and repeatability of the process were investigated. The mechanisms of guanidinium ionic liquid based microwave-assisted extraction were researched by scanning electron microscopy and IR spectroscopy. All the results show that guanidinium ionic liquid based microwave-assisted extraction has a huge potential in the extraction of bioactive compounds from complex samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Ionic-liquid-impregnated resin for the microwave-assisted solid-liquid extraction of triazine herbicides in honey.

    Science.gov (United States)

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

    2015-09-01

    Microwave-assisted ionic-liquid-impregnated resin solid-liquid extraction was developed for the extraction of triazine herbicides, including cyanazine, metribuzin, desmetryn, secbumeton, terbumeton, terbuthylazine, dimethametryn, and dipropetryn in honey samples. The ionic-liquid-impregnated resin was prepared by immobilizing 1-hexyl-3-methylimidazolium hexafluorophosphate in the microspores of resin. The resin was used as the extraction adsorbent. The extraction and enrichment of analytes were performed in a single step. The extraction time can be shortened greatly with the help of microwave. The effects of experimental parameters including type of resin, type of ionic liquid, mass ratio of resin to ionic liquid, extraction time, amount of the impregnated resin, extraction temperature, salt concentration, and desorption conditions on the extraction efficiency, were investigated. A Box-Behnken design was applied to the selection of the experimental parameters. The recoveries were in the range of 80.1 to 103.4% and the relative standard deviations were lower than 6.8%. The present method was applied to the analysis of honey samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. The plant microtubule-associated protein AtMAP65-3/PLE is essential for cytokinetic phragmoplast function.

    Science.gov (United States)

    Müller, Sabine; Smertenko, Andrei; Wagner, Vera; Heinrich, Maria; Hussey, Patrick J; Hauser, Marie-Theres

    2004-03-09

    Directional cell expansion in interphase and nuclear and cell division in M-phase are mediated by four microtubule arrays, three of which are unique to plants: the interphase array, the preprophase band, and the phragmoplast. The plant microtubule-associated protein MAP65 has been identified as a key structural component in these arrays. The Arabidopsis genome has nine MAP65 genes, and here we show that one, AtMAP65-3/PLE, locates only to the mitotic arrays and is essential for cytokinesis. The Arabidopsis pleiade (ple) alleles are single recessive mutations, and we show that these mutations are in the AtMAP65-3 gene. Moreover, these mutations cause C-terminal truncations that abolish microtubule binding. In the ple mutants the anaphase spindle is normal, and the cytokinetic phragmoplast can form but is distorted; not only is it wider, but the midline, the region where oppositely oriented microtubules overlap, is unusually expanded. Here we present data that demonstrate an essential role for AtMAP65-3/PLE in cytokinesis in plant cells.

  11. Pre-concentration of uranium from water samples by dispersive liquid-liquid micro-extraction

    Energy Technology Data Exchange (ETDEWEB)

    Khajeh, Mostafa; Nemch, Tabandeh Karimi [Zabol Univ. (Iran, Islamic Republic of). Dept. of Chemistry

    2014-07-01

    In this study, a simple and rapid dispersive liquid-liquid microextraction (DLLME) was developed for the determination of uranium in water samples prior to high performance liquid chromatography with diode array detection. 1-(2-pyridylazo)-2-naphthol (PAN) was used as complexing agent. The effect of various parameters on the extraction step including type and volume of extraction and dispersive solvents, pH of solution, concentration of PAN, extraction time, sample volume and ionic strength were studied and optimized. Under the optimum conditions, the limit of detection (LOD) and preconcentration factor were 0.3 μg L{sup -1} and 194, respectively. Furthermore, the relative standard deviation of the ten replicate was <2.6%. The developed procedure was then applied to the extraction and determination of uranium in the water samples.

  12. Pre-concentration of uranium from water samples by dispersive liquid-liquid micro-extraction

    International Nuclear Information System (INIS)

    Khajeh, Mostafa; Nemch, Tabandeh Karimi

    2014-01-01

    In this study, a simple and rapid dispersive liquid-liquid microextraction (DLLME) was developed for the determination of uranium in water samples prior to high performance liquid chromatography with diode array detection. 1-(2-pyridylazo)-2-naphthol (PAN) was used as complexing agent. The effect of various parameters on the extraction step including type and volume of extraction and dispersive solvents, pH of solution, concentration of PAN, extraction time, sample volume and ionic strength were studied and optimized. Under the optimum conditions, the limit of detection (LOD) and preconcentration factor were 0.3 μg L -1 and 194, respectively. Furthermore, the relative standard deviation of the ten replicate was <2.6%. The developed procedure was then applied to the extraction and determination of uranium in the water samples.

  13. CONTRIBUTION TO THE DEVELOPMENT OF A SIMULATION SOFTWARE PERFORMANCE AND SHARING RATIO IN LIQUID-LIQUID EXTRACTION

    Directory of Open Access Journals (Sweden)

    A. Hadj Seyd

    2015-07-01

    Full Text Available The present work is to develop software to predict the value yield and the distribution coefficient in the process of liquid-liquid extraction of components of a mixture, from mathematical models expressing these entities, based on equations equilibrium between liquid-liquid phases, and predict the conditions under which the extraction operation is favorable, unfavorable or impossible to realize, by studying the variation of the entities cited, based on the parameters influencing the extraction, which are: initial concentrations, rate of solvent and pH, in the case of a simple extraction (extraction of neutral products or when it is reactive (extraction of complex acids or bases for one or more components.The programming language used is "Delphi" which is a very powerful oriented object programming under Windows.

  14. FIV diversity: FIV Ple subtype composition may influence disease outcome in African lions.

    Science.gov (United States)

    Troyer, Jennifer L; Roelke, Melody E; Jespersen, Jillian M; Baggett, Natalie; Buckley-Beason, Valerie; MacNulty, Dan; Craft, Meggan; Packer, Craig; Pecon-Slattery, Jill; O'Brien, Stephen J

    2011-10-15

    Feline immunodeficiency virus (FIV) infects domestic cats and at least 20 additional species of non-domestic felids throughout the world. Strains specific to domestic cat (FIV(Fca)) produce AIDS-like disease progression, sequelae and pathology providing an informative model for HIV infection in humans. Less is known about the immunological and pathological influence of FIV in other felid species although multiple distinct strains of FIV circulate in natural populations. As in HIV-1 and HIV-2, multiple diverse cross-species infections may have occurred. In the Serengeti National Park, Tanzania, three divergent subtypes of lion FIV (FIV(Ple)) are endemic, whereby 100% of adult lions are infected with one or more of these strains. Herein, the relative distribution of these subtypes in the population are surveyed and, combined with observed differences in lion mortality due to secondary infections based on FIV(Ple) subtypes, the data suggest that FIV(Ple) subtypes may have different patterns of pathogenicity and transmissibility among wild lion populations. Copyright © 2011 Elsevier B.V. All rights reserved.

  15. Pyridinium ionic liquid-based liquid-solid extraction of inorganic and organic iodine from Laminaria.

    Science.gov (United States)

    Peng, Li-Qing; Yu, Wen-Yan; Xu, Jing-Jing; Cao, Jun

    2018-01-15

    A simple, green and effective extraction method, namely, pyridinium ionic liquid- (IL) based liquid-solid extraction (LSE), was first designed to extract the main inorganic and organic iodine compounds (I - , monoiodo-tyrosine (MIT) and diiodo-tyrosine (DIT)). The optimal extraction conditions were as follows: ultrasonic intensity 100W, IL ([EPy]Br) concentration 200mM, extraction time 30min, liquid/solid ratio 10mL/g, and pH value 6.5. The morphologies of Laminaria were studied by scanning electron microscopy and transmission electron microscopy. The recovery values of I - , MIT and DIT from Laminaria were in the range of 88% to 94%, and limits of detection were in the range of 59.40 to 283.6ng/g. The proposed method was applied to the extraction and determination of iodine compounds in three Laminaria. The results showed that IL-based LSE could be a promising method for rapid extraction of bioactive iodine from complex food matrices. Copyright © 2017 Elsevier Ltd. All rights reserved.

  16. Trace hydrogen extraction from liquid lithium tin alloy

    International Nuclear Information System (INIS)

    Xie Bo; Hu Rui; Xie Shuxian; Weng Kuiping

    2010-01-01

    In order to finish the design of tritium extraction system (TES) of fusion fission hybrid reactor (FFHR) tritium blanket, involving the dynamic mathematical model of liquid metal in contact with a gaseous atmosphere, approximate mathematical equation of tritium in lithium tin alloy was deduced. Moreover, carrying process used for trace hydrogen extraction from liquid lithium tin alloy was investigated with hydrogen being used to simulate tritium in the study. The study results indicate that carrying process is effective way for hydrogen extraction from liquid lithium tin alloy, and the best flow velocity of carrier gas is about 4 L/min under 1 kg alloy temperatures and carrying numbers are the main influencing factors of hydrogen number. Hydrogen extraction efficiency can reach 85% while the alloy sample is treated 6 times at 823 K. (authors)

  17. Determination of Organic Pollutants in Small Samples of Groundwaters by Liquid-Liquid Extraction and Capillary Gas Chromatography

    DEFF Research Database (Denmark)

    Harrison, I.; Leader, R.U.; Higgo, J.J.W.

    1994-01-01

    A method is presented for the determination of 22 organic compounds in polluted groundwaters. The method includes liquid-liquid extraction of the base/neutral organics from small, alkaline groundwater samples, followed by derivatisation and liquid-liquid extraction of phenolic compounds after neu...... neutralisation. The extracts were analysed by capillary gas chromatography. Dual detection by flame Ionisation and electron capture was used to reduce analysis time....

  18. Development of Chromatographic Fingerprints of Eurycoma longifolia (Tongkat Ali Roots Using Online Solid Phase Extraction-Liquid Chromatography (SPE-LC

    Directory of Open Access Journals (Sweden)

    Nor Nasriah Zaini

    2016-04-01

    Full Text Available E. longifolia is attracting interest due to its pharmacological properties and pro-vitality effects. In this study, an online SPE-LC approach using polystyrene divinyl benzene (PSDVB and C18 columns was developed in obtaining chromatographic fingerprints of E. longifolia. E. longifolia root samples were extracted using pressurized liquid extraction (PLE technique prior to online SPE-LC. The effects of mobile phase compositions and column switching time on the chromatographic fingerprint were optimized. Validation of the developed method was studied based on eurycomanone. Linearity was in the range of 5 to 50 µg∙mL−1 (r2 = 0.997 with 3.2% relative standard deviation of peak area. The developed method was used to analyze 14 E. longifolia root samples and 10 products (capsules. Selected chemometric techniques: cluster analysis (CA, discriminant analysis (DA, and principal component analysis (PCA were applied to the fingerprint datasets of 37 selected peaks to evaluate the ability of the chromatographic fingerprint in classifying quality of E. longifolia. Three groups were obtained using CA. DA yielded 100% correlation coefficient with 19 discriminant compounds. Using PCA, E. longifolia root samples were clearly discriminated from the products. This study showed that the developed online SPE-LC method was able to provide comprehensive evaluation of E. longifolia samples for quality control purposes.

  19. Association of solvent extraction and liquid-liquid flotation processes for metal recovery

    International Nuclear Information System (INIS)

    Puget, Flavia P.; Mendonca, Luciano A. de; Massarani, Giulio

    2000-01-01

    From the batch solvent extraction process, in this work it has been carried out a preliminary study aiming the determination of the optimal operating conditions for zirconium recovery (10 ppm) using alamine 336 (tricaprylylamine) as extractor. The results have shown that the extraction takes place instantaneously (5s of manual agitation) and that at pH around 2.0 the extraction efficiency is up to 98-99% for an aqueous/organic phase volumetric ratio of 10. Based on these results, it is proposed to evaluate the possibility of using of a pioneering technology for metal recovery at low concentrations, using a experimental set-up that associates standard solvent extraction process with liquid-liquid flotation process. (author)

  20. Evaluation of a contact device type ejector system for liquid-liquid extraction

    International Nuclear Information System (INIS)

    Schwamback, Niomedes

    2002-04-01

    The objective of the present work was to evaluate an ejector system, operated simultaneously with two immiscible liquid phases and a gas phase, as a contact device for liquid-liquid extraction processes. The ejector, made of perspex, has a variable geometry, although this feature was not explored in the thesis. Motivated by recent uses of liquid-liquid extraction processes for the removal of traces of heavy metal from waste waters, it was decided to carry out tests with synthetic effluents. This strategy, typical of experimental work under evaluation of technical feasibility, greatly simplifies experiments, since the nature of the chemical species involved and their feed concentrations are known exactly and do not fluctuate. The extractant used was DEHPA (diethyl hexyl phosphoric acid). The metal chosen for tests was iron with oxidation number +3, because of its high extraction coefficient towards DEHPA and also for its chemical behavior similar to americium and other heavy metals. In addition to that, iron forms soluble coloured complexes adequate to spectrophotometric determination analysis, a simple, quick and very reliable analytical technique. The effects of electrolytes of interest, namely NaCl, FeSO 4 and Al(NO 3 ) 3 , upon the extraction process were investigated. The effects resulting from the introduction of a gas phase, actually air (bubbles), in the ejector upon the extraction efficiency were studied. By coupling advanced digital photographic technique and image analysis with microcomputer, the bubble mean size was measured. It was then correlated with equipment's geometrical (characteristic diameters) and operational variables (phases' flow rates and gas hold-ups). To enable scale-up procedures, data were preferably correlated by means of dimensionless groups. For the systems and conditions investigated in this thesis and under the same operational conditions, the introduction of air bubbles by means of an ejector has greatly improved the process

  1. Recycling of Metal Containing Waste by Liquid-Liquid Extraction

    International Nuclear Information System (INIS)

    Reinhardt, H.

    1999-01-01

    Through the years, a large number of liquid-liquid extraction have been proposed for metal waste recovery and recycling(1,2). However, few of them have achieved commercial application. In fact, relatively little information is available on practical operation and economic feasibility. This presentation will give complementary information by describing and comparing three processes, based on the Am MAR hydrometallurgical concept and representing three different modes of operation

  2. Enhanced flavour extraction in continuous liquid-liquid extractors

    CSIR Research Space (South Africa)

    Apps, P

    2005-08-12

    Full Text Available stirrer that prevents channelling improves extraction efficiency by between 2.8 and 17.6 times. Use of the stir bar extends the application of CLLE to samples that are not free-running liquids, thereby reducing sample manipulations with their associated...

  3. Extractive behavior of U(VI) in the paraffin soluble ionic liquid

    International Nuclear Information System (INIS)

    Rama, R.; Kumaresan, R.; Venkatesan, K.A.; Antony, M.P.; Vasudeva Rao, P.R.

    2013-01-01

    An Aliquat-336 based ionic liquid namely, tri-n-octylmethylammonium bis(2-ethylhexyl)phosphate ((A3636) + (DEHP) - ) was prepared and studied for the extraction of U(VI) from nitric acid medium. Since the ionic liquid, (A336) + (DEHP) - , was miscible in n-dodecane (n-DD), the extraction of U(VI) in the solution of tri-n-butylphosphate (TBP) in n-DD, was investigated in the presence of small concentrations of ionic liquid. The distribution ratio of U(VI) in 0.3 M (A336) + (DEHP) - /n-DD decreased with increase in the concentration of nitric acid. The effect of concentration of TBP, ionic liquid nitric acid and nitrate ion on the extraction of U(VI) in ionic liquid medium was studied. The mechanistic aspect of extraction was investigated by the slope analysis of the extraction data. The studies indicated the feasibility of modifying the extractive properties of U(VI) in TBP/n-DD using ionic liquid. (author)

  4. Pressurized liquid extraction and chemical characterization of safflower oil: A comparison between methods.

    Science.gov (United States)

    Conte, Rogério; Gullich, Letícia M D; Bilibio, Denise; Zanella, Odivan; Bender, João P; Carniel, Naira; Priamo, Wagner L

    2016-12-15

    This work investigates the extraction process of safflower oil using pressurized ethanol, and compares the chemical composition obtained (in terms of fatty acids) with other extraction techniques. Soxhlet and Ultrasound showed maximum global yield of 36.53% and 30.41%, respectively (70°C and 240min). PLE presented maximum global yields of 25.62% (3mLmin(-1)), 19.94% (2mLmin(-1)) and 12.37% (1mLmin(-1)) at 40°C, 100bar and 60min. Palmitic acid showed the lower concentration in all experimental conditions (from 5.70% to 7.17%); Stearic and Linoleic acid presented intermediate concentrations (from 2.93% to 25.09% and 14.09% to 19.06%, respectively); Oleic acid showed higher composition (from 55.12% to 83.26%). Differences between percentages of fatty acids, depending on method were observed. Results may be applied to maximize global yields and select fatty acids, reducing the energetic costs and process time. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Development of a new extraction method based on counter current salting-out homogenous liquid-liquid extraction followed by dispersive liquid-liquid microextraction: Application for the extraction and preconcentration of widely used pesticides from fruit juices.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Feriduni, Behruz; Mogaddam, Mohammad Reza Afshar

    2016-01-01

    In this paper, a new extraction method based on counter current salting-out homogenous liquid-liquid extraction (CCSHLLE) followed by dispersive liquid-liquid microextraction (DLLME) has been developed for the extraction and preconcentration of widely used pesticides in fruit juice samples prior to their analysis by gas chromatography-flame ionization detection (GC-FID). In this method, initially, sodium chloride as a separation reagent is filled into a small column and a mixture of water (or fruit juice) and acetonitrile is passed through the column. By passing the mixture sodium chloride is dissolved and the fine droplets of acetonitrile are formed due to salting-out effect. The produced droplets go up through the remained mixture and collect as a separated layer. Then, the collected organic phase (acetonitrile) is removed with a syringe and mixed with 1,1,2,2-tetrachloroethane (extraction solvent at µL level). In the second step, for further enrichment of the analytes the above mixture is injected into 5 mL de-ionized water placed in a test tube with conical bottom in order to dissolve acetonitrile into water and to achieve a sedimented phase at µL-level volume containing the enriched analytes. Under the optimal extraction conditions (extraction solvent, 1.5 mL acetonitrile; pH, 7; flow rate, 0.5 mL min(-1); preconcentration solvent, 20 µL 1,1,2,2-tetrachloroethane; NaCl concentration; 5%, w/w; and centrifugation rate and time, 5000 rpm and 5 min, respectively), the extraction recoveries and enrichment factors ranged from 87% to 96% and 544 to 600, respectively. Repeatability of the proposed method, expressed as relative standard deviations, ranged from 2% to 6% for intra-day (n=6, C=250 or 500 µg L(-1)) and inter-days (n=4, C=250 or 500 µg L(-1)) precisions. Limits of detection are obtained between 2 and 12 µg L(-1). Finally, the proposed method is applied for the determination of the target pesticide residues in the juice samples. Copyright © 2015

  6. Extraction efficiency of hydrophilic and lipophilic antioxidants from lyophilized foods using pressurized liquid extraction and manual extraction.

    Science.gov (United States)

    Watanabe, Jun; Oki, Tomoyuki; Takebayashi, Jun; Takano-Ishikawa, Yuko

    2014-09-01

    The efficient extraction of antioxidants from food samples is necessary in order to accurately measure their antioxidant capacities. α-Tocopherol and gallic acid were spiked into samples of 5 lyophilized and pulverized vegetables and fruits (onion, cabbage, Satsuma mandarin orange, pumpkin, and spinach). The lipophilic and hydrophilic antioxidants in the samples were sequentially extracted with a mixed solvent of n-hexane and dichloromethane, and then with acetic acid-acidified aqueous methanol. Duplicate samples were extracted: one set was extracted using an automated pressurized liquid extraction apparatus, and the other set was extracted manually. Spiked α-tocopherol and gallic acid were recovered almost quantitatively in the extracted lipophilic and hydrophilic fractions, respectively, especially when pressurized liquid extraction was used. The expected increase in lipophilic oxygen radical absorbance capacity (L-ORAC) due to spiking with α-tocopherol, and the expected increase in 2,2-diphenyl-1-picrylhydrazyl radical scavenging activities and total polyphenol content due to spiking with gallic acid, were all recovered in high yield. Relatively low recoveries, as reflected in the hydrophilic ORAC (H-ORAC) value, were obtained following spiking with gallic acid, suggesting an interaction between gallic acid and endogenous antioxidants. The H-ORAC values of gallic acid-spiked samples were almost the same as those of postadded (spiked) samples. These results clearly indicate that lipophilic and hydrophilic antioxidants are effectively extracted from lyophilized food, especially when pressurized liquid extraction is used. © 2014 Institute of Food Technologists®

  7. Niobium, tantalum and titanium extraction from natural and technogenic raw materials of the Kola Peninsula by liquid-liquid extraction methods

    International Nuclear Information System (INIS)

    Kassikova, N.I.; Kassikov, A.G.; Balabanov, Yu.I.; Petrov, V.B.; Kalinnikov, V.T.

    2003-01-01

    Such rare metals as niobium and tantalum are important strategic materials underlying many of the modern advanced technologies. Since the extraction and processing of rare metal concentrates from own deposits has diminished abruptly in recent years, it is essential to look into the possibility of extracting these elements from various production wastes. This work discusses liquid-liquid extraction and purification of niobium, tantalum and titanium from process solutions of loparite, perovskite and sphene concentrate decomposition with sulphuric and hydrochloric acids; niobium from lithium niobate production wastes decomposed by hydrochloric acid; and tantalum from tantalum capacitor and heat-resistant alloy wastes. (Original)

  8. Pressurized liquid extraction using water/isopropanol coupled with solid-phase extraction cleanup for semivolatile organic compounds, polycyclic aromatic hydrocarbons (PAH), and alkylated PAH homolog groups in sediment

    Science.gov (United States)

    Burkhardt, M.R.; Zaugg, S.D.; Burbank, T.L.; Olson, M.C.; Iverson, J.L.

    2005-01-01

    Polycyclic aromatic hydrocarbons (PAH) are recognized as environmentally relevant for their potential adverse effects on human and ecosystem health. This paper describes a method to determine the distribution of PAH and alkylated homolog groups in sediment samples. Pressurized liquid extraction (PLE), coupled with solid-phase extraction (SPE) cleanup, was developed to decrease sample preparation time, to reduce solvent consumption, and to minimize background interferences for full-scan GC-MS analysis. Recoveries from spiked Ottawa sand, environmental stream sediment, and commercially available topsoil, fortified at 1.5-15 ??g per compound, averaged 94.6 ?? 7.8%, 90.7 ?? 5.8% and 92.8 ?? 12.8%, respectively. Initial method detection limits for single-component compounds ranged from 20 to 302 ??g/kg, based on 25 g samples. Results from 28 environmental sediment samples, excluding homologs, show 35 of 41 compounds (85.4%) were detected in at least one sample with concentrations ranging from 20 to 100,000 ??g/kg. The most frequently detected compound, 2,6-dimethylnaphthalene, was detected in 23 of the 28 (82%) environmental samples with a concentration ranging from 15 to 907 ??g/kg. The results from the 28 environmental sediment samples for the homolog series showed that 27 of 28 (96%) samples had at least one homolog series present at concentrations ranging from 20 to 89,000 ??g/kg. The most frequently detected homolog series, C2-alkylated naphthalene, was detected in 26 of the 28 (93%) environmental samples with a concentration ranging from 25 to 3900 ??g/kg. Results for a standard reference material using dichloromethane Soxhlet-based extraction also are compared. ?? 2005 Elsevier B.V. All rights reserved.

  9. Liquid-liquid extraction of actinides, lanthanides, and fission products by use of ionic liquids: from discovery to understanding.

    Science.gov (United States)

    Billard, Isabelle; Ouadi, Ali; Gaillard, Clotilde

    2011-06-01

    Liquid-liquid extraction of actinides and lanthanides by use of ionic liquids is reviewed, considering, first, phenomenological aspects, then looking more deeply at the various mechanisms. Future trends in this developing field are presented.

  10. Liquid-liquid extraction of actinides, lanthanides, and fission products by use of ionic liquids: from discovery to understanding

    International Nuclear Information System (INIS)

    Billard, Isabelle; Ouadi, Ali; Gaillard, Clotilde

    2011-01-01

    Liquid-liquid extraction of actinides and lanthanides by use of ionic liquids is reviewed, considering, first, phenomenological aspects, then looking more deeply at the various mechanisms. Future trends in this developing field are presented. (orig.)

  11. Liquid-liquid extraction from molten alkaline nitrates by using nitrogenous and organophosphorus derivatives

    International Nuclear Information System (INIS)

    Vittori, Olivier

    1971-01-01

    This research thesis reports the use of a system made of the LiNO 3 -KNO 3 eutectic at 160 deg. C and poly-phenyls in order to study the behaviour of phosphine and arsine oxides as extracting agents in a liquid-liquid process. In a first part, the author presents the studied system, its physical characteristics and its preparation, and the various analytical methods which have used. He discusses existing computation methods adapted to the separation of molten salts and organic phase, and proposes a specific method. Then, he reports the study of the behaviour of a phosphine oxide with Cobalt II and Nickel II, and discusses its application to the separation of this pair, Co II and Ni II. He highlights the different possibilities of three agents which are derivatives of phosphine and arsine in their ability to extract rare earths. A study of separation of rare earths is then addressed. The author reports the application of extraction equilibriums to the study of equilibriums in environments of molten salts with the Co II - chloride ions system. The author finally addresses the synergic phenomenon that pairs of neutral complexing agents of neighbouring structure or different donor central atom may display in liquid-liquid extraction

  12. Separation of tungsten from molybdenum by liquid-liquid extraction and extraction chromatography using thiocyanate and a quarternary ammonium salt

    International Nuclear Information System (INIS)

    Yonezawa, C.; Onishi, H.

    1977-01-01

    Methods were developed for the separation of tungsten from molybdenum by liquid-liquid extraction and extraction chromatography using thiocyanate and a quaternary ammonium salt, Zephiramine. Tungsten was extracted into chloroform as an ion associate of tungsten(V)-thiocyanate complex and Zephiramine cation was retained on a column of Teflon powder coated with Zephiramine, but molybdenum(III) was neither extracted nor retained. The extraction chromatographic method was succesfully applied to the determination of trace amounts of tungsten in molybdenum by neutron activation analysis. The γ-ray spectrum, observed with the Ge(Li) detector, of tungsten fraction separated from irradiated molybdenum are shown. The peaks of 99 Mo, sup(99m)Tc, and sup(99m)Nb (produced by 92 Mo(n,p)sup(99m)Nb) were seen, but these nuclides did nit interfere with the determination of tungsten using a NaI(Tl) detector. The results of the neutron activation analysis of a sample of ammonium molybdate agreed quite well with that of the spectrophotometric determination after extraction chromatographic separation. (T.G.)

  13. Extraction of plutonium(IV) by diglycolamide extractants in room temperature ionic liquids

    Energy Technology Data Exchange (ETDEWEB)

    Prabhu, Dattaprasad R.; Raut, Dhaval R.; Murali, Mallekav S.; Mohapatra, Prasanta K. [Bhabha Atomic Research Centre, Mumbai (India). Radiochemistry Div.

    2017-06-01

    Extraction of Pu(IV) was investigated using solutions of two diglycolamide extractants viz., N,N,N{sup '},N{sup '}-tetra-n-octyldiglycolamide (TODGA) and its branched homolog, N,N,N{sup '},N{sup '}-tetra(2-ethylhexyl) diglycolamide (T2EHDGA), dissolved in two imidazolium based room temperature ionic liquids viz., 1-butyl-3-methylimidazolium bis(trifluoromethanesulphonyl) imide ([C{sub 4}mim][NTf{sub 2}]) and 1-octyl-3-methylimidazolium bis(trifluoromethanesulphonyl) imide ([C{sub 8}mim][NTf{sub 2}]) from aqueous nitric acid medium. The extraction kinetics was found to be extremely slow which is reported for the first time for analogous extraction systems and took as long as 30 h to attain equilibrium D{sub Pu} values. In general, TODGA based solvents showed better extraction of Pu(IV) than the T2EHDGA based solvents, one order of magnitude higher, and though both the ionic liquids ultimately yielded comparable D{sub Pu} values, attainment of equilibrium was slower with [C{sub 4}mim][NTf{sub 2}]. The extracted species conformed to 1:1 for TODGA in both the ionic liquids while a mixture of 1:1 and 1:2 species was observed for T2EHDGA at 1 M HNO{sub 3} which changed to 1:1 species at 4 M HNO{sub 3}. The extracted species is proposed to be (Pu(L){sub x}{sup 4+}){sub IL} (where, L is the extractant and x=1 or 2) at lower acidities suggesting a cation exchange mechanism which changes over to (Pu(NO{sub 3}){sub 4} .L){sub IL} at 4 M HNO{sub 3} conforming to a solvation mechanism for all the systems except for T2EHDGA-[C{sub 8}mim][NTf{sub 2}]. UV-VIS spectroscopic studies were carried out to throw light on the nature of the extracted species.

  14. Parallel artificial liquid membrane extraction of acidic drugs from human plasma

    DEFF Research Database (Denmark)

    Roldan-Pijuan, Mercedes; Pedersen-Bjergaard, Stig; Gjelstad, Astrid

    2015-01-01

    The new sample preparation concept “Parallel artificial liquid membrane extraction (PALME)” was evaluated for extraction of the acidic drugs ketoprofen, fenoprofen, diclofenac, flurbiprofen, ibuprofen, and gemfibrozil from human plasma samples. Plasma samples (250 μL) were loaded into individual......-performance liquid chromatography-ultraviolet detection of the individual acceptor solutions. Important PALME parameters including the chemical composition of the liquid membrane, extraction time, and sample pH were optimized, and the extraction performance was evaluated. Except for flurbiprofen, exhaustive...

  15. Hypoglycemic effects of aqueous persimmon leaf extract in a murine model of diabetes.

    Science.gov (United States)

    Bae, Ui-Jin; Park, Soo-Hyun; Jung, Su-Young; Park, Byung-Hyun; Chae, Soo-Wan

    2015-08-01

    Previously, powdered persimmon leaves have been reported to have glucose- and lipid-lowering effects in diabetic (db/db) mice. As persimmon leaf is commonly consumed as tea, an aqueous extract of persimmon leaves (PLE) was prepared and its anti-diabetic efficacy was investigated. In the present study, PLE was tested for its inhibitory activity on α-glucosidase in vitro. An oral maltose tolerance test was performed in diabetic mice. Next, the acute effect of PLE was examined in streptozotocin-induced diabetic mice. Last, the long-term effect of PLE supplementation was assessed in db/db after eight weeks. An oral glucose tolerance test, biochemical parameters, as well as histological analyses of liver and pancreas were evaluated at the end of the study. PLE inhibited α-glucosidase activity and increased antioxidant capacity. Streptozotocin-induced diabetic mice pre-treated with PLE displayed hypoglycemic activity. Daily oral supplementation with PLE for eight weeks reduced body weight gain without affecting food intake, enhanced the glucose tolerance during the oral glucose tolerance test (OGTT), improved blood lipid parameters, suppressed fat accumulation in the liver and maintained islet structure in db/db mice. Further mechanistic study showed that PLE protected pancreatic islets from glucotoxicity. In conclusion, the results of the present study indicated that PLE exhibits considerable anti-diabetic effects through α-glucosidase inhibition and through the maintenance of functional β-cells. These results provided a rationale for the use of persimmon leaf tea for the maintenance of normal blood glucose levels in diabetic patients.

  16. Liquid-liquid extraction of plutonium and americium by cekanoic acid from alkaline medium

    International Nuclear Information System (INIS)

    Venugopal Chetty, K.; Sagar, V.; Swarup, R.

    2001-01-01

    Liquid-liquid extraction studies of plutonium and americium from aqueous carbonate medium using a high molecular weight carboxylic acid namely cekanoic acid in different diluents has been carried out. The distribution ratio (D) values for Pu(IV) and Am(III) under various parameters such as concentration of extractant, Na 2 CO 3 and initial pH were obtained. Results indicated that Pu(IV) and Am(III) could be satisfactorily extracted together or individually from aqueous carbonate medium using cekanoic acid in different diluents like carbon tetrachloride, cyclohexane, toluene, n-dodecane or solvesso-100. The D values for Pu(IV) and Am(III) also indicated the possibility of their mutual separation. The back extraction of Pu and Am with different reagents was also studied. (orig.)

  17. 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.

  18. Removal of nitrogen compounds from Brazilian petroleum samples by oxidation followed by liquid-liquid extraction

    Energy Technology Data Exchange (ETDEWEB)

    Conceicao, L.; Pergher, S.B.C. [Universidade Regional Integrada do Alto Uruguai e das Misses (URI), Erechim, RS (Brazil). Dept. de Quimica], E-mail: pergher@uricer.edu.br; Oliveira, J.V. [Universidade Regional Integrada do Alto Uruguai e das Misses (URI), Erechim, RS (Brazil). Dept. de Engenharia dos Alimentos; Souza, W.F. [Petroleo Brasileiro S.A. (CENPES/PETROBRAS), Rio de Janeiro, RJ (Brazil). Centro de Pesquisas

    2009-10-15

    This work reports liquid-liquid extraction of nitrogen compounds from oxidized and non-oxidized Brazilian petroleum samples. The experiments were accomplished in a laboratory-scale liquid-liquid apparatus in the temperature range of 303 K-323 K, using methanol, n-methyl-2-pyrrolidone (NMP) and N,Ndimethylformamide (DMF), and their mixtures as extraction solvents, employing solvent to sample volume ratios of 1:2, 1:1 and 2:1, exploring up to three separation stages. Results show that an increase in temperature, solvent to oil ratio, and number of equilibrium stages greatly improves the nitrogen removal from the oxidized sample (from 2600 to 200 ppm). The employed oxidation scheme is thus demonstrated to be an essential and efficient step of sample preparation for the selective liquid-liquid removal of nitrogen compounds. It is shown that the use of mixtures of DMF and NMP as well their use as co-solvents with methanol did not prove to be useful for selective nitrogen extraction since great oil losses were observed in the final process. (author)

  19. Quaternary (liquid + liquid) equilibrium data for the extraction of toluene from alkanes using the ionic liquid [EMim][MSO4

    International Nuclear Information System (INIS)

    Corderí, Sandra; Calvar, Noelia; Gómez, Elena; Domínguez, Ángeles

    2014-01-01

    Highlights: • EMim[MSO 4 ] was proposed as solvent for the extraction of toluene from alkanes. • The quaternary system {heptane + cyclohexane + toluene + [EMim][MSO 4 ]} was evaluated. • The extraction of toluene would be facilitated in the presence of one alkane. • Experimental LLE data were successfully correlated with the NRTL model. - Abstract: (Liquid + liquid) equilibrium (LLE) studies for the extraction of aromatics from alkanes present in the petroleum fractions are important to develop theoretical/semiempirical (liquid + liquid) equilibrium models, which are used in the design of extraction processes. In this work, the ionic liquid 1-ethyl-3-methylimidazolium methylsulfate, [EMim][MSO 4 ], was evaluated as potential solvent for the separation of toluene from heptane and cyclohexane. The LLE data for the quaternary system {heptane (1) + cyclohexane (2) + toluene (3) + [EMim][MSO 4 ] (4)} were experimentally determined at T = 298.15 K and atmospheric pressure. Moreover, the LLE data for the ternary systems {heptane or cyclohexane (1) + toluene (2) + [EMim][MSO 4 ] (3)} were also determined. Solute distribution ratios and selectivities were calculated and analysed in order to evaluate the capability of the ionic liquid to accomplish the separation target. A comparison between the solute distribution ratios and selectivities for the quaternary and the ternary systems was also made. Finally, the experimental tie-line data were correlated with the NRTL model

  20. Evaluation of a novel task specific ionic liquid for actinide ion extraction

    International Nuclear Information System (INIS)

    Paramanik, M.; Ghosh, S.K.; Raut, D.R.; Mohapatra, P.K.

    2016-01-01

    Separation of U and Pu from nuclear waste is of great relevance for a sustainable closed fuel cycle point of view. Spent fuel reprocessing by the well known PUREX process is done world wide for the recovery of U and Pu using TBP as the extractant. Room temperature ionic liquids (RTILs) have shown significantly higher extraction of metal ions, particularly at lower acidity as compared to the molecular diluents. Functionalization of ionic liquids has resulted in highly efficient task specific ionic liquids (TSILs) with superior extraction properties than the analogous extractants dissolved in ionic liquids. The present paper reports the evaluation of a novel task specific ionic liquid (TSIL) containing >P=O functional group for the extraction of actinides like U(VI) and Pu(IV)

  1. Determination of organophosphorus flame retardants in fish by pressurized liquid extraction using aqueous solutions and solid-phase microextraction coupled with gas chromatography-flame photometric detector.

    Science.gov (United States)

    Gao, Zhanqi; Deng, Yuehua; Yuan, Wenting; He, Huan; Yang, Shaogui; Sun, Cheng

    2014-10-31

    A novel method was developed for the determination of organophosphorus flame retardants (PFRs) in fish. The method consists of a combination of pressurized liquid extraction (PLE) using aqueous solutions and solid-phase microextraction (SPME), followed by gas chromatography-flame photometric detector (GC-FPD). The experimental parameters that influenced extraction efficiency were systematically evaluated. The optimal responses were observed by extracting 1g of fish meat with the solution of water:acetonitrile (90:10, v/v) at 150°C for 5min and acid-washed silica gel used as lipid sorbent. The obtained extract was then analyzed by SPME coupled with GC-FPD without any additional clean-up steps. Under the optimal conditions, the proposed procedure showed a wide linear range (0.90-5000ngg(-1)) obtained by analyzing the spiked fish samples with increasing concentrations of PFRs and correlation coefficient (R) ranged from 0.9900 to 0.9992. The detection limits (S/N=3) were in the range of 0.010-0.208ngg(-1) with standard deviations (RSDs) ranging from 2.0% to 9.0%. The intra-day and inter-day variations were less than 9.0% and 7.8%, respectively. The proposed method was successfully applied to the determination of PFRs in real fish samples with recoveries varying from 79.8% to 107.3%. The results demonstrate that the proposed method is highly effective for analyzing PFRs in fish samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. Purification process for aqueous solutions of rare earths by liquid-liquid extraction

    International Nuclear Information System (INIS)

    Rollat, A.; Sabot, J.L.; Burgard, M.; Delloye, T.

    1986-01-01

    Alkaline earth metals are removed by liquid-liquid extraction between on aqueous nitric phase of impure rare earth compounds and an organic phase of polyether (crown ether). This process is particularly suited to removal of Ca, Ba and Ra contained in nitric solutions of rare earths [fr

  3. Task-specific thioglycolate ionic liquids for heavy metal extraction: Synthesis, extraction efficacies and recycling properties

    Energy Technology Data Exchange (ETDEWEB)

    Platzer, Sonja [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, 1090 Vienna (Austria); Kar, Mega [School of Chemistry, Monash University, Clayton, Victoria 3800 (Australia); Leyma, Raphlin; Chib, Sonia; Roller, Alexander [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, 1090 Vienna (Austria); Jirsa, Franz [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, 1090 Vienna (Austria); Department of Zoology, University of Johannesburg, PO Box 524, Auckland Park, 2006 Johannesburg (South Africa); Krachler, Regina [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, 1090 Vienna (Austria); MacFarlane, Douglas R. [School of Chemistry, Monash University, Clayton, Victoria 3800 (Australia); Kandioller, Wolfgang, E-mail: wolfgang.kandioller@univie.ac.at [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, 1090 Vienna (Austria); Keppler, Bernhard K. [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, 1090 Vienna (Austria)

    2017-02-15

    Highlights: • Thioglycolate-based ionic liquids have been synthesized and their physicochemical properties have been examined. • The developed ionic liquids can efficiently remove Cu(II) and Cd(II). • Loaded ionic liquids can be recycled by application of different stripping protocols. - Abstract: Eight novel task-specific ionic liquids (TSILs) based on the thioglycolate anion designed for heavy metal extraction have been prepared and characterized by {sup 1}H and {sup 13}C NMR, UV-Vis, infrared, ESI-MS, conductivity, viscosity, density and thermal properties. Evaluation of their time-resolved extraction abilities towards cadmium(II) and copper(II) in aqueous solutions have been investigated where distribution ratios up to 1200 were observed. For elucidation of the IL extraction mode, crystals were grown where Cd(II) was converted with an excess of S-butyl thioglycolate. It was found by X-ray diffraction analysis that cadmium is coordinated by five oxygen and one sulfur donor atoms provided by two thioglycolate molecules and one water molecule. Leaching behavior of the hydrophobic ionic liquids into aqueous systems was studied by TOC (total dissolved organic carbon) measurements. Additionally, the immobilization on polypropylene was elucidated and revealed slower metal extraction rates and similar leaching behavior. Finally, recovery processes for cadmium and copper after extraction were performed and recyclability was successfully proven for both metals.

  4. Feasibility of bio-based lactate esters as extractant for biobutanol recovery: (Liquid + liquid) equilibria

    International Nuclear Information System (INIS)

    Zheng, Shaohua; Cheng, Hongye; Chen, Lifang; Qi, Zhiwen

    2016-01-01

    Highlights: • Lactate esters were studied as solvent to remove butanol from aqueous media. • (Liquid + liquid) equilibrium data were measured at T = 298.15 K and 1 atm. • Selectivity and 1-butanol partition coefficient were calculated. • COSMO-based study of separation efficiency on solvent structure was conducted. - Abstract: As bio-based solvents, lactate esters can be used as extractant for removing 1-butanol from the aqueous fermentation broths. In order to evaluate the separation efficiency of butyl lactate and 2-ethylhexyl lactate for the extraction of 1-butanol from its mixture with water, the (liquid + liquid) equilibrium for the ternary systems {water (1) + 1-butanol (2) + lactate ester (3)} were measured at T = 298.15 K. The 1-butanol partition coefficient varied in the range of 4.46 to 10.29, and the solvent selectivity within 32.12 to 108.18. For the separation of low-concentration butanol from fermentation broths, butyl lactate exhibits higher partition coefficient and lower selectivity than 2-ethylhexyl lactate. The NRTL model was employed to correlate the experimental data, and the COSMO-RS theory was utilized to predict the (liquid + liquid) equilibria and to analyze the influence of lactate esters on extraction efficiency.

  5. Liquid-liquid extraction assisted by a carbon nanoparticles interface. Electrophoretic determination of atrazine in environmental samples.

    Science.gov (United States)

    Caballero-Díaz, Encarnación; Simonet, Bartolomé; Valcárcel, Miguel

    2013-10-21

    A novel method for the determination of atrazine, using liquid-liquid extraction assisted by a nanoparticles film formed in situ and composed of organic solvent stabilized-carbon nanoparticles, is described. The presence of nanoparticles located at the liquid-liquid interface reinforced the extraction of analyte from matrix prior to capillary electrophoresis (CE) analysis. Some influential experimental variables were optimized in order to enhance the extraction efficiency. The developed procedure confirmed that carbon nanoparticles, especially multi-walled carbon nanotubes, are suitable to be used in sample treatment processes introducing new mechanisms of interaction with the analyte. The application of the proposed preconcentration method followed by CE detection enabled the determination of atrazine in spiked river water providing acceptable RSD values (11.6%) and good recoveries (about 87.0-92.0%). Additionally, a similar extraction scheme was tested in soil matrices with a view to further applications in real soil samples.

  6. Determination of ten steroid hormones in animal waste manure and agricultural soil using inverse and integrated clean-up pressurized liquid extraction and gas chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, Martin; Krogh, Kristine Andersen; Halling-Sørensen, Bent

    2011-01-01

    ... Martin Hansen , Kristine A. Krogh , Bent Halling ... in a 22 mL PLE cell : firstly by flushing the sample with heptane to remove unwanted matrix components (inverse- PLE , i- PLE ) and secondly, performing internal clean-up (ic- PLE ) and eluting the steroid hormones by attaching an ...

  7. Selective solvent extraction of actinides associated to liquid scintillation measurements

    International Nuclear Information System (INIS)

    Ardois, C.; Musikas, C.

    1997-01-01

    The problems associated to radioactive waste disposal have acquired a special attention due, particularly, to the element instability and, consequently, to their lixiviation and to their peculiarities which are essential in the radioactivity penetration in the food chains; the other important parameters are the produced amounts and the noxiousnesses. New commercial liquid scintillation counters allow rapid α/β measurements. Associated with liquid-liquid extraction techniques, rapid and selective actinide analyses are possible. Among various actinide extractants, such as amines or organophosphorus compounds, we were particularly interested in tri-n-octyl-phosphine oxide (TOPO). Uranium, thorium and americium extractions with (TOPO) in toluene have been investigated. A systematic study of the counting parameters of a PACKARD 2550 TR/AB TM liquid scintillation analyzer is under completion

  8. Simultaneous Distillation Extraction of Some Volatile Flavor Components from Pu-erh Tea Samples—Comparison with Steam Distillation-Liquid/Liquid Extraction and Soxhlet Extraction

    Directory of Open Access Journals (Sweden)

    Xungang Gu

    2009-01-01

    Full Text Available A simutaneous distillation extraction (SDE combined GC method was constructed for determination of volatile flavor components in Pu-erh tea samples. Dichloromethane and ethyl decylate was employed as organic phase in SDE and internal standard in determination, respectively. Weakly polar DB-5 column was used to separate the volatile flavor components in GC, 10 of the components were quantitatively analyzed, and further confirmed by GC-MS. The recovery covered from 66.4%–109%, and repeatability expressed as RSD was in range of 1.44%–12.6%. SDE was most suitable for the extraction of the anlytes by comparing with steam distillation-liquid/liquid extraction and Soxhlet extraction. Commercially available Pu-erh tea samples, including Pu-erh raw tea and ripe tea, were analyzed by the constructed method. the high-volatile components, such as benzyl alcohol, linalool oxide, and linalool, were greatly rich in Pu-erh raw teas, while the contents of 1,2,3-Trimethoxylbenzene and 1,2,4-Trimethoxylbenzene were much high in Pu-erh ripe teas.

  9. Punica granatum (pomegranate) leaves extract induces apoptosis through mitochondrial intrinsic pathway and inhibits migration and invasion in non-small cell lung cancer in vitro.

    Science.gov (United States)

    Li, Yali; Yang, Fangfang; Zheng, Weidong; Hu, Mingxing; Wang, Juanxiu; Ma, Sisi; Deng, Yuanle; Luo, Yi; Ye, Tinghong; Yin, Wenya

    2016-05-01

    Most conventional treatments on non-small cell lung carcinoma always accompany with awful side effects, and the incidence and mortality rates of this cancer are increasing rapidly worldwide. The objective of this study was to examine the anticancer effects of extract of Punica granatum (pomegranate) leaves extract (PLE) on the non-small cell lung carcinoma cell line A549, H1299 and mouse Lewis lung carcinoma cell line LL/2 in vitro, and explore its mechanisms of action. Our results have shown that PLE inhibited cell proliferation in non-small cell lung carcinoma cell line in a concentration- and time-dependent manner. Flow cytometry (FCM) assay showed that PLE affected H1299 cell survival by arresting cell cycle progression in G2/M phase in a dose-dependent manner and inducing apoptosis. Moreover, PLE could also decrease the reactive oxygen species (ROS) and the mitochondrial membrane potential (ΔYm), indicating that PLE may induce apoptosis via mitochondria-mediated apoptotic pathway. Furthermore, PLE blocked H1299 cell migration and invasion, and the reduction of matrix metalloproteinase (MMP) MMP-2 and MMP-9 expression were also observed in vitro. These results suggested that PLE could be an effective and safe chemotherapeutic agent in non-small cell lung carcinoma treatment by inhibiting proliferation, inducing apoptosis, cell cycle arrest and impairing cell migration and invasion. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

  10. Separation of phosphorous by liquid-liquid extraction for the measurement of 32P

    International Nuclear Information System (INIS)

    Lee, H.N.; Yang, S.D.

    2010-01-01

    Phosphorous containing radioisotope waste was separated and determined by liquid-liquid extraction method through liquid scintillation counter (LSC). In this process, ammonium phosphate was converted to phosphomolybdate (PMo) by the reaction of ammonium molybdate (Mo) in HCl solution (0.02 M) and maximum UV/VIS absorbance (λ max ) 218 nm was observed. The PMo solution was extracted with TOA (Tri-n-Octylamine)/xylene mixture and λ max 290 nm was found for this organic layer. Absorbance of aqueous and organic layer was linear through concentration. The impurities such as Co, Cr, Gd, etc. remain in aqueous layer by treating with Mo which was determined by ICP-AES and AAS. The quenching correction curve for 32 P was calculated using LSC results. No counting change was observed as the volume of quenchers increased. The recovery was 98% and 81% for the extraction and separation process from the test using H 3 32 PO 4 as standard tracer. (author)

  11. Advancing liquid/liquid extraction through a novel microfluidic device: Theory, instrumentation and applications in gas chromatography

    NARCIS (Netherlands)

    Peroni, D.; van Egmond, W.; Kok, W.T.; Janssen, J.G.M.

    2012-01-01

    A new chip-based liquid-liquid extraction technique for sample preparation of aqueous samples for GC was developed. Extraction is performed in a segmented flow system with additional mixing provided by an etched channel structure. The dimensions of the device are optimized to allow benefiting of the

  12. Functionalized ionic liquids: new agents for the extraction of actinides/lanthanides

    International Nuclear Information System (INIS)

    Ouadi, A.; Hesemann, P.; Billard, I.; Gaillard, C.; Gadenne, B.; Moreau, Joel J.E; Moutiers, G.; Mariet, C.; Labet, A.

    2004-01-01

    The potentialities of hydrophobic ionic liquids BumimPF 6 and BumimTf 2 N for their use in the nuclear fuel cycle were investigated, in particular for the liquid liquid extraction. We demonstrate that the use of RTILs in replacement of the organic diluents for actinides partitioning is promising. In our contribution, we present the synthesis of several task-specific ionic liquids. Our results show that grafting metal complexing groups increases the affinity of metals to the IL phase and gives rise to suitable media for the liquid-liquid extraction of actinides. (authors)

  13. Ionic liquid pre-treatment of microalgae and extraction of biomolecules

    NARCIS (Netherlands)

    Desai, Rupali K.

    2016-01-01

    Liquid-liquid extraction (LLE) techniques are widely used in separation primarily due to ease of scale up. Conventional (LLE) systems based on organic solvents are not suitable for extraction of fragile molecules such as proteins as it would result in denaturation. On the other hand aqueous

  14. Predictive model for ionic liquid extraction solvents for rare earth elements

    International Nuclear Information System (INIS)

    Grabda, Mariusz; Oleszek, Sylwia; Panigrahi, Mrutyunjay; Kozak, Dmytro; Shibata, Etsuro; Nakamura, Takashi; Eckert, Franck

    2015-01-01

    The purpose of our study was to select the most effective ionic liquid extraction solvents for dysprosium (III) fluoride using a theoretical approach. Conductor-like Screening Model for Real Solvents (COSMO-RS), based on quantum chemistry and the statistical thermodynamics of predefined DyF 3 -ionic liquid systems, was applied to reach the target. Chemical potentials of the salt were predicted in 4,400 different ionic liquids. On the base of these predictions set of ionic liquids’ ions, manifesting significant decrease of the chemical potentials, were selected. Considering the calculated physicochemical properties (hydrophobicity, viscosity) of the ionic liquids containing these specific ions, the most effective extraction solvents for liquid-liquid extraction of DyF 3 were proposed. The obtained results indicate that the COSMO-RS approach can be applied to quickly screen the affinity of any rare earth element for a large number of ionic liquid systems, before extensive experimental tests

  15. Liquid-liquid extraction of uranium from nitric acid solution using di-n-butylsulfoxide in petroleum ether as extractant

    Energy Technology Data Exchange (ETDEWEB)

    Khan, M.H.; Shahida, S. [Dept. of Chemistry, Univ. of Azad Jammu and Kashmir, Muzaffarabad (Pakistan); Ali, A. [Nuclear Chemistry Div., Pakistan Inst. of Nuclear Science and Technology, Nilore, Islamabad (Pakistan)

    2008-07-01

    A simple, efficient and economical liquid-liquid extraction method has been developed for quantitative extraction of uranium from 2 M HNO{sub 3} using di-n-butyl sulfoxide in petroleum ether. The dependence of the partition reaction of U(VI) on the concentration of HNO{sub 3}, extractant and temperature was studied. The reaction was found to be inversely dependent upon the temperature and the values for related thermodynamics functions ({delta}H, {delta}S, {delta}G) for extraction equilibrium were determined to be -33.6 kJ/mol, -1.29 kJ/mol/degree and -0.11 kJ/mol/degree, respectively. The effect of Al(NO{sub 3}){sub 3} as salting-out agent and diverse ions on the extraction was examined. The salting-out agent slightly enhanced the extraction. All cations studied have showed negligible effect on the extraction, whereas phosphate and fluoride interfered seriously. Among others, oxalate, citrate and sulphide ions affect the extraction to a lesser extent. Uranium was successfully extracted from a synthetic mixture of Ti{sup +4}, Zr{sup +4}, Hf{sup +4} and Th{sup +4} using EDTA as masking agent. Among strippants, deionized water was found most suitable, and the recovery of uranium was noted to be {>=} 96%. The stoichiometric composition of the extracted species was found to be UO{sub 2}(NO{sub 3}){sub 2} . 2DBSO. The extraction mechanism is discussed on the basis of the results obtained. The extractant has high loading as well as recycling capacity without any degradation. The method was also applied to the Standard Reference Material (NBL-49) and the measured value was found to be in agreement with the reported value within {+-}2% deviation. (orig.)

  16. Task-specific ionic liquids for An and Ln extraction: unusual speciation and extraction mechanisms

    Energy Technology Data Exchange (ETDEWEB)

    Billard, Isabelle; Jobin, Emilie; Ouadi, Ali; Gaillard, Clotilde [IPHC-DRS, Chimie nucleaire, 23 rue du Loess, BP28, 67037 Strasbourg cedex 2 (France)

    2008-07-01

    Extraction mechanisms of uranium by TBP (tributylphosphate) diluted in an ionic liquid BumimTf{sub 2}N (1-butyl-3-methyl-imidazolium bis(tri-fluoro-methyl-sulfonyl)imide) and by Task-Specific Ionic Liquids (TSILs) bearing a phosphoryl group were investigated. Great differences between these mechanisms and the one in the industrial solvent, dodecane, have been put in evidence. While in dodecane, the neutral species, UO{sub 2}(NO{sub 3}){sub 2}(TBP){sub 2}, is the major extracted complex, in BumimTf{sub 2}N and TSILs, at least two species are extracted with more or less similar proportions. Moreover, no uranyl species with two nitrates could be observed in these ionic liquids. Finally, the mechanisms vary from TBP in BumimTf{sub 2}N to TSILs. These results led to a so-to-say new kind of actinide chemistry. (authors)

  17. PERFORMANCE OF A PACKED LIQUID-LIQUID EXTRACTION COLUMN

    Directory of Open Access Journals (Sweden)

    İ. Metin HASDEMİR

    1999-03-01

    Full Text Available The influence of feed ratios ((LE/LR on the performance of a packed liquid-liquid extraction column, with a diameter of 5.86 cm and a column height of 132 cm was investigated. The column is made of borosilicate glass and packed with 10 x 10 mm glass Raschig rings. In this study, a ternary system composed of water + propionic acid + trichloroethylene was used. The data used to triangular diagram were obtained experimentally. The overall mass transfer coefficients, the numbers of overall mass transfer units, the heights of mass transfer units, the numbers of theoretical stages and height equivalent to a theoretical stage (H. E. T. S. values were calculated and compared with each other.

  18. Haze Formation and Behavior in Liquid-Liquid Extraction Processes

    International Nuclear Information System (INIS)

    Arm, Stuart T.; Jenkins, J. A.

    2006-01-01

    Aqueous haze formation and behavior was studied in the liquid-liquid system tri-n-butyl phosphate in odorless kerosene and 3M nitric acid with uranyl nitrate and cesium nitrate representing the major solute and an impurity, respectively. A pulsed column, mixer-settler and centrifugal contactor were chosen to investigate the effect of different turbulence characteristics on the manifestation of haze since these contactors exhibit distinct mixing phenomena. The dispersive processes of drop coalescence and breakage, and water precipitation in the organic phase were observed to lead to the formation of haze drops of ∼1 um in diameter. The interaction between the haze and primary drops of the dispersion was critical to the separation efficiency of the liquid-liquid extraction equipment. Conditions of high power input and spatially homogeneous mixing enabled the haze drops to become rapidly assimilated within the dispersion to maximize the scrub performance and separation efficiency of the equipment

  19. Homogeneous Liquid–Liquid Extraction of Rare Earths with the Betaine—Betainium Bis(trifluoromethylsulfonyl)imide Ionic Liquid System

    Science.gov (United States)

    Hoogerstraete, Tom Vander; Onghena, Bieke; Binnemans, Koen

    2013-01-01

    Several fundamental extraction parameters such as the kinetics and loading were studied for a new type of metal solvent extraction system with ionic liquids. The binary mixture of the ionic liquid betainium bis(trifluoromethylsulfonyl)imide and water shows thermomorphic behavior with an upper critical solution temperature (UCST), which can be used to avoid the slower mass transfer due to the generally higher viscosity of ionic liquids. A less viscous homogeneous phase and mixing on a molecular scale are obtained when the mixture is heated up above 55 °C. The influence of the temperature, the heating and cooling times, were studied for the extraction of neodymium(III) with betaine. A plausible and equal extraction mechanism is proposed in bis(trifluoromethylsulfonyl)imide, nitrate, and chloride media. After stripping of the metals from the ionic liquid phase, a higher recovery of the ionic liquid was obtained by salting-out of the ionic liquid fraction lost by dissolution in the aqueous phase. The change of the upper critical solution temperature by the addition of HCl or betaine was investigated. In addition, the viscosity was measured below and above the UCST as a function of the temperature. PMID:24169434

  20. Polycyclic aromatic hydrocarbons (PAH) in Danish barbecued meat

    DEFF Research Database (Denmark)

    Duedahl-Olesen, Lene; Aaslyng, Margit Dall; Meinert, Lene

    2015-01-01

    Barbecuing is known to result in the formation of polycyclic aromatic hydrocarbons (PAHs). A validated method that employed pressurized liquid extraction (PLE), gel permeation chromatography (GPC) followed by solid phase extraction (SPE) on Silica and analytical determination by GC-MS was applied...

  1. Solvent extraction of Sr2+ and Cs+ based on hydrophobic protic ionic liquids

    International Nuclear Information System (INIS)

    Luo, Huimin; Yu, Miao; Dai, Sheng

    2007-01-01

    A series of new hydrophobic and protic alkylammonium ionic liquids with bis(trifluoromethylsulfonyl) imide or bis(perfluoroethylsulfonyl)imide as conjugated anions was synthesized in a one-pot reaction with a high yield. In essence our synthesis method involves the combination of neutralization and metathesis reactions. Some of these hydrophobic and protic ionic liquids were liquids at room temperature and therefore investigated as new extraction media for separation of Sr 2+ and Cs + from aqueous solutions. An excellent extraction efficiency was found for some of these ionic liquids using dicyclohexano-18-crown-6 and calix[4]arene-bis(tert-octylbenzo-crown-6) as extractants. The observed enhancement in the extraction efficiency can be attributed to the greater hydrophilicity of the cations of the protic ionic liquids. The application of the protic ionic liquids as new solvent systems for solvent extraction opens up a new avenue in searching for simple and efficient ionic liquids for tailored separation processes. (orig.)

  2. Literature Review: Crud Formation at the Liquid/Liquid Interface of TBP-Based Solvent-Extraction Processes

    Energy Technology Data Exchange (ETDEWEB)

    Delegard, Calvin H.; Casella, Amanda J.

    2016-09-30

    This report summarizes the literature reviewed on crud formation at the liquid:liquid interface of solvent extraction processes. The review is focused both on classic PUREX extraction for industrial reprocessing, especially as practiced at the Hanford Site, and for those steps specific to plutonium purification that were used at the Plutonium Reclamation Facility (PRF) within the Plutonium Finishing Plant (PFP) at the Hanford Site.

  3. Gastric pull-up reconstruction combined with free jejunal transfer (FJT) following total pharyngolaryngo-oesophagectomy (PLE).

    Science.gov (United States)

    Ni, Song; Zhu, Yiming; Li, Dezhi; Li, Zhengjiang; Wu, Yuehuang; Xu, Zhengang; Liu, Shaoyan

    2015-06-01

    Reconstruction following total pharyngolaryngo-oesophagectomy (PLE) still challenges surgeons because of the extreme length of removed tissue. Gastric pull-up reconstruction, one of the most common reconstructive methods after PLE, has many complications such as anastomotic fistula and gastric necrosis caused by the high anastomotic tension. However, modifications of gastric pull-up reconstruction aiming to reducing the high anastomotic tension have been less reported compared with other aspects with this technique. Here we report a modified gastric pull-up reconstruction combined with free jejunal transfer (FTJ) to reduce the anastomosis tension, and thus to reduce the risk of complications after PLE. Patients underwent a standard surgical procedure including total pharyngolaryngo-oesophagectomy and bilateral internal jugular lymph nodal clearance. A free jejunal graft about 10 cm was harvested and placed in the appropriate position between mobilized stomach and oropharynx. The anastomosis between the free jejunal graft and the gastric tube was created through a stapler. Vascular anastomosis was made between the jejunal artery and the transverse cervical artery, and between the jejunal vein and the internal jugular vein. Hand suturing technique was used in the anastomosis between jejunum and pharynx. None of the patients suffered from any complications such as anastomotic fistula. Both patients resumed early postoperative oral intake. So far, they remain free of tumor recurrence and are in good health for 46 and 18 months, respectively. Considering the tumor status and the patient condition, the gastric pull-up reconstruction combined with FJT after PLE could be a reliable choice. Copyright © 2015 IJS Publishing Group Limited. Published by Elsevier Ltd. All rights reserved.

  4. Comparison of salting-out and sugaring-out liquid-liquid extraction methods for the partition of 10-hydroxy-2-decenoic acid in royal jelly and their co-extracted protein content.

    Science.gov (United States)

    Tu, Xijuan; Sun, Fanyi; Wu, Siyuan; Liu, Weiyi; Gao, Zhaosheng; Huang, Shaokang; Chen, Wenbin

    2018-01-15

    Homogeneous liquid-liquid extraction (h-LLE) has been receiving considerable attention as a sample preparation method due to its simple and fast partition of compounds with a wide range of polarities. To better understand the differences between the two h-LLE extraction approaches, salting-out assisted liquid-liquid extraction (SALLE) and sugaring-out assisted liquid-liquid extraction (SULLE), have been compared for the partition of 10-hydroxy-2-decenoic acid (10-HDA) from royal jelly, and for the co-extraction of proteins. Effects of the amount of phase partition agents and the concentration of acetonitrile (ACN) on the h-LLE were discussed. Results showed that partition efficiency of 10-HDA depends on the phase ratio in both SALLE and SULLE. Though the partition triggered by NaCl and glucose is less efficient than MgSO 4 in the 50% (v/v) ACN-water mixture, their extraction yields can be improved to be similar with that in MgSO 4 SALLE by increasing the initial concentration of ACN in the ACN-water mixture. The content of co-extracted protein was correlated with water concentration in the obtained upper phase. MgSO 4 showed the largest protein co-extraction at the low concentration of salt. Glucose exhibited a large protein co-extraction in the high phase ratio condition. Furthermore, NaCl with high initial ACN concentration is recommended because it produced high extraction yield for 10-HDA and the lowest amount of co-extracted protein. These observations would be valuable for the sample preparation of royal jelly. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Ionic Liquid-Based Ultrasonic/Microwave-Assisted Extraction of ...

    African Journals Online (AJOL)

    Conclusion: Compared with traditional methods, IL-UMAE method uses Ionic liquid-solvent which greatly shortens the extraction time. IL-UMAE as a simple, effective and environmentally friendly approach shows a broad prospect for active ingredient extraction. Keywords: Dioscorea zingiberensis Steroidal saponins, Ionic ...

  6. Selective extraction of emerging contaminants from water samples by dispersive liquid-liquid microextraction using functionalized ionic liquids.

    Science.gov (United States)

    Yao, Cong; Li, Tianhao; Twu, Pamela; Pitner, William R; Anderson, Jared L

    2011-03-25

    Functionalized ionic liquids containing the tris(pentafluoroethyl)trifluorophosphate (FAP) anion were used as extraction solvents in dispersive liquid-liquid microextraction (DLLME) for the extraction of 14 emerging contaminants from water samples. The extraction efficiencies and selectivities were compared to those of an in situ IL DLLME method which uses an in situ metathesis reaction to exchange 1-butyl-3-methylimidazolium chloride (BMIM-Cl) to 1-butyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide (BMIM-NTf(2)). Compounds containing tertiary amine functionality were extracted with high selectivity and sensitivity by the 1-(6-amino-hexyl)-1-methylpyrrolidinium tris(pentafluoroethyl)trifluorophosphate (HNH(2)MPL-FAP) IL compared to other FAP-based ILs and the BMIM-NTf(2) IL. On the other hand, polar or acidic compounds without amine groups exhibited higher enrichment factors using the BMIM-NTf(2) IL. The detection limits for the studied analytes varied from 0.1 to 55.1 μg/L using the traditional IL DLLME method with the HNH(2)MPL-FAP IL as extraction solvent, and from 0.1 to 55.8 μg/L using in situ IL DLLME method with BMIM-Cl+LiNTf(2) as extraction solvent. A 93-fold decrease in the detection limit of caffeine was observed when using the HNH(2)MPL-FAP IL compared to that obtained using in situ IL DLLME method. Real water samples including tap water and creek water were analyzed with both IL DLLME methods and yielded recoveries ranging from 91% to 110%. Copyright © 2011 Elsevier B.V. All rights reserved.

  7. Rational approach to solvent system selection for liquid-liquid extraction-assisted sample pretreatment in counter-current chromatography.

    Science.gov (United States)

    Wang, Jiajia; Gu, Dongyu; Wang, Miao; Guo, Xinfeng; Li, Haoquan; Dong, Yue; Guo, Hong; Wang, Yi; Fan, Mengqi; Yang, Yi

    2017-05-15

    A rational liquid-liquid extraction approach was established to pre-treat samples for high-speed counter-current chromatography (HSCCC). n-Hexane-ethyl acetate-methanol-water (4:5:4:5, v/v) and (1:5:1:5, v/v) were selected as solvent systems for liquid-liquid extraction by systematically screening K of target compounds to remove low- and high-polarity impurities in the sample, respectively. After liquid-liquid extraction was performed, 1.4g of crude sample II was obtained from 18.5g of crude sample I which was extracted from the flowers of Robinia pseudoacacia L., and then separated with HSCCC by using a solvent system composed of n-hexane-ethyl acetate-methanol-water (1:2:1:2, v/v). As a result, 31mg of robinin and 37mg of kaempferol 7-O-α-l-rhamnopyranoside were isolated from 200mg of crude sample II in a single run of HSCCC. A scale-up separation was also performed, and 160mg of robinin with 95% purity and 188mg of kaempferol 7-O-α-l-rhamnopyranoside with 97% purity were produced from 1.2g of crude sample II. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Extraction of lithium from salt lake brine using room temperature ionic liquid in tributyl phosphate

    International Nuclear Information System (INIS)

    Shi, Chenglong; Jia, Yongzhong; Zhang, Chao; Liu, Hong; Jing, Yan

    2015-01-01

    Highlights: • We proposed a new system for Li recovery from salt lake brine by extraction using an ionic liquid. • Cation exchange was proposed to be the mechanism of extraction followed in ionic liquid. • This ionic liquid system shown considerable extraction ability for lithium and the single extraction efficiency of lithium reached 87.28% under the optimal conditions. - Abstract: Lithium is known as the energy metal and it is a key raw material for preparing lithium isotopes which have important applications in nuclear energy source. In this work, a typical room temperature ionic liquid (RTILs), 1-butyl-3-methyl-imidazolium hexafluorophosphate ([C 4 mim][PF 6 ]), was used as an alternative solvent to study liquid/liquid extraction of lithium from salt lake brine. In this system, the ionic liquid, NaClO 4 and tributyl phosphate (TBP) were used as extraction medium, co-extraction reagent and extractant respectively. The effects of solution pH value, phase ratio, ClO 4 − amount and other factors on lithium extraction efficiency had been investigated. Optimal extraction conditions of this system include the ratio of TBP/IL at 4/1 (v/v), O/A at 2:1, n(ClO 4 − )/n(Li + ) at 2:1, the equilibration time of 10 min and unadjusted pH. Under the optimal conditions, the single extraction efficiency of lithium was 87.28% which was much higher than the conventional extraction system. Total extraction efficiency of 99.12% was obtained by triple-stage countercurrent extraction. Study on the mechanism revealed that the use of ionic liquid increased the extraction yield of lithium through cation exchange in this system. Preliminary results indicated that the use of [C 4 mim][PF 6 ] as an alternate solvent to replace traditional organic solvents (VOCs) in liquid/liquid extraction was very promising

  9. Ionic liquid-based microwave-assisted extraction of rutin from Chinese medicinal plants.

    Science.gov (United States)

    Zeng, Huan; Wang, Yuzhi; Kong, Jinhuan; Nie, Chan; Yuan, Ya

    2010-12-15

    An ionic liquid-based microwave-assisted extraction (ILMAE) method has been developed for the effective extraction of rutin from Chinese medicinal plants including Saururus chinensis (Lour.) Bail. (S. chinensis) and Flos Sophorae. A series of 1-butyl-3-methylimidazolium ionic liquids with different anions were investigated. The results indicated that the characteristics of anions have remarkable effects on the extraction efficiency of rutin and among the investigated ionic liquids, 1-butyl-3-methylimidazolium bromide ([bmim]Br) aqueous solution was the best. In addition, the ILMAE procedures for the two kinds of medicinal herbs were also optimized by means of a series of single factor experiments and an L(9) (3(4)) orthogonal design. Compared with the optimal ionic liquid-based heating extraction (ILHE), marinated extraction (ILME), ultrasonic-assisted extraction (ILUAE), the optimized approach of ILMAE gained higher extraction efficiency which is 4.879 mg/g in S. chinensis with RSD 1.33% and 171.82 mg/g in Flos Sophorae with RSD 1.47% within the shortest extraction time. Reversed phase high performance liquid chromatography (RP-HPLC) with ultraviolet detection was employed for the analysis of rutin in Chinese medicinal plants. Under the optimum conditions, the average recoveries of rutin from S. chinensis and Flos Sophorae were 101.23% and 99.62% with RSD lower than 3%, respectively. The developed approach is linear at concentrations from 42 to 252 mg L(-1) of rutin solution, with the regression coefficient (r) at 0.99917. Moreover, the extraction mechanism of ILMAE and the microstructures and chemical structures of the two researched samples before and after extraction were also investigated. With the help of LC-MS, it was future demonstrated that the two researched herbs do contain active ingredient of rutin and ionic liquids would not influence the structure of rutin. Copyright © 2010 Elsevier B.V. All rights reserved.

  10. Liquid-solid extraction of metallic cations by cationic amphiphiles

    International Nuclear Information System (INIS)

    Mueller, Wolfram; Sievers, Torsten K.; Zemb, Thomas; Diat, Olivier; Sievers, Torsten K.; Dejugnat, Christophe

    2012-01-01

    In the field of selective metal ion separation, liquid-liquid extraction is usually conducted through an emulsion mixing of hydrophobic complexants dispersed in an organic phase and acidic water containing the ionic species. Recently, it has been shown that amphiphilic complexants could influence strongly extraction efficiency by enhancing the interfacial interaction between the metal ion in the aqueous and the complexant in the organic phase. Moreover, these amphiphiles can also substitute the organic phase if an appropriate aliphatic chain is chosen. The dispersion of such amphiphilic complexants in an aqueous solution of salt mixtures is not only attractive for studying specific interactions but also to better the understanding of complex formation in aqueous solution of multivalent metal ions, such as lanthanides and actinides. This understanding is of potential interest for a broad range of industries including purification of rare earth metals and pollute treatment e.g. of fission byproducts. This principle can also be applied to liquid-solid extraction, where the final state of the separation is a solid phase containing the selectively extracted ions. Indeed, a novel solid-liquid extraction method exploits the selective precipitation of metal ions from an aqueous salt mixture using a cationic surfactant, below its Krafft point (temperature below which the long aliphatic chains of surfactant crystallize). This technique has been proven to be highly efficient for the separation of actinides and heavy metal using long chain ammonium or pyridinium amphiphiles. The most important point in this process is the recognition of cationic metal ions by cationic surfactants. By computing the free energy of the polar head group per micelle as a function of the different counter-anions, we have demonstrated for the first time that different interactions exist between the micellar surface and the ions. These interactions depend on the nature of the cation but also on

  11. Extraction Equilibrium of Acrylic Acid by Aqueous Two-Phase Systems Using Hydrophilic Ionic Liquids

    International Nuclear Information System (INIS)

    Lee, Yong Hwa; Lee, Woo Youn; Kim, Ki-Sub; Hong, Yeon Ki

    2014-01-01

    As an effective method for extraction of acrylic acid, aqueous two-phase systems based on morpholinium ionic liquids were used in this study. Effects of the alkyl chain length of cation in morpholinium ionic liquids on phase diagram and extraction efficiencies were investigated. Experimental results show that aqueous two phase systems can be formed by adding appropriate amount of morpholinium ionic liquids to aqueous K 2 HPO 4 solutions. It can be found that the ability of morpholinium ionic liquids for phase separation followed the order [HMMor][Br]>[OMMor][Br]>[BMMor][Br]>[EMMor][Br]. There was little difference between binodal curves of imidazolium ionic liquids and those of morpholinium ionic liquids. 50-90% of the extraction efficiency was observed for acrylic acid by aqueous two phase extraction of acrylic acid with morpholinium ionic liquids. It can be concluded that morpholinium ionic liquids/K 2 HPO 4 were effective for aqueous two phases extraction of acrylic acid comparing to imidazolium ionic liquids/K 2 HPO 4 systems because of their lower cost

  12. 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

  13. Solid-Phase Extraction Combined with High Performance Liquid ...

    African Journals Online (AJOL)

    Methods: Solid-phase extraction method was employed for the extraction of the estrogen from milk and high performance liquid chromatography-diode array detector (HPLC-DAD) was used for the determination of estrogen. Results: Optimal chromatographic conditions were achieved on an Eclipse XDB-C18 column at a ...

  14. Liquid to liquid extraction and liquid chromatography-tandem mass spectrometry determination of hainanmycin in feed.

    Science.gov (United States)

    Wang, Ze Ping; Shen, Jian Zhong; Linhardt, Robert J; Jiang, Hui; Cheng, Lin Li

    2017-03-01

    Hainanmycin is a new veterinary polyether antibiotic and has few sensitive analytical method in present days. In this study, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) relying on multiple reaction monitoring (MRM) detection was developed for analysis of hainanmycin in animal feed. Feed samples were extracted with ethyl acetate and purified by two steps of liquid-liquid extraction (LLE) to get rid of water solvable matrix and lipids one by one. The final simple was analyzed by LC-MS/MS. The LC mobile phase was composed of 0.1% aqueous formic acid and 0.1% formic acidified acetonitrile by gradient elution. Average recoveries ranged from 74.22% to 87.85%, as determined by spiking with 2.0 (LOQ) ∼2500μgkg -1 of hainanmycin. The inter-day and intra-day coefficient of variation was 9.21% to 11.77% and 7.67% to 13.49%, respectively. The limit of detection (LOD) and the limit of quantitation (LOQ) were 0.36μgkg -1 and 2.0μgkg -1 , respectively. Copyright © 2016. Published by Elsevier B.V.

  15. Extraction of lithium from salt lake brine using room temperature ionic liquid in tributyl phosphate

    Energy Technology Data Exchange (ETDEWEB)

    Shi, Chenglong [Key Laboratory of Salt Lake Resources and Chemistry, Qinghai Institute of Salt Lakes, Chinese Academy of Sciences, 810008 Xining (China); University of Chinese Academy of Sciences, 100049 Beijing (China); Jia, Yongzhong [Key Laboratory of Salt Lake Resources and Chemistry, Qinghai Institute of Salt Lakes, Chinese Academy of Sciences, 810008 Xining (China); Zhang, Chao [Key Laboratory of Salt Lake Resources and Chemistry, Qinghai Institute of Salt Lakes, Chinese Academy of Sciences, 810008 Xining (China); University of Chinese Academy of Sciences, 100049 Beijing (China); Liu, Hong [Qinghai Salt Chemical Products Supervision and Inspection Center, 816000 Golmud (China); Jing, Yan, E-mail: 1580707906@qq.com [Key Laboratory of Salt Lake Resources and Chemistry, Qinghai Institute of Salt Lakes, Chinese Academy of Sciences, 810008 Xining (China)

    2015-01-15

    Highlights: • We proposed a new system for Li recovery from salt lake brine by extraction using an ionic liquid. • Cation exchange was proposed to be the mechanism of extraction followed in ionic liquid. • This ionic liquid system shown considerable extraction ability for lithium and the single extraction efficiency of lithium reached 87.28% under the optimal conditions. - Abstract: Lithium is known as the energy metal and it is a key raw material for preparing lithium isotopes which have important applications in nuclear energy source. In this work, a typical room temperature ionic liquid (RTILs), 1-butyl-3-methyl-imidazolium hexafluorophosphate ([C{sub 4}mim][PF{sub 6}]), was used as an alternative solvent to study liquid/liquid extraction of lithium from salt lake brine. In this system, the ionic liquid, NaClO{sub 4} and tributyl phosphate (TBP) were used as extraction medium, co-extraction reagent and extractant respectively. The effects of solution pH value, phase ratio, ClO{sub 4}{sup −} amount and other factors on lithium extraction efficiency had been investigated. Optimal extraction conditions of this system include the ratio of TBP/IL at 4/1 (v/v), O/A at 2:1, n(ClO{sub 4}{sup −})/n(Li{sup +}) at 2:1, the equilibration time of 10 min and unadjusted pH. Under the optimal conditions, the single extraction efficiency of lithium was 87.28% which was much higher than the conventional extraction system. Total extraction efficiency of 99.12% was obtained by triple-stage countercurrent extraction. Study on the mechanism revealed that the use of ionic liquid increased the extraction yield of lithium through cation exchange in this system. Preliminary results indicated that the use of [C{sub 4}mim][PF{sub 6}] as an alternate solvent to replace traditional organic solvents (VOCs) in liquid/liquid extraction was very promising.

  16. Mixing-settling apparatus for liquid-liquid extraction

    International Nuclear Information System (INIS)

    Skolokin, L.I.; Leif, V.E.; Sednev, J.M.

    1989-01-01

    A mixing-settling apparatus for liquid-liquid extraction comprises a casing. A first partition is mounted along its longitudinal axis and above an overflow device. The mixing device is connected to a means of feeding at least one of the phases and is shaped as at least one hollow element mounted essentially perpendicularly to the longitudinal axis of the casing. The walls of the hollow element are provided with openings, the outlet cross-sections of which are directed to the first partition. The first partition is provided with a means for regulating the height of the layer of the mixed phases M in the mixing zone, said means being located in the partition at the point most distant from the means for feeding phases L, S in the longitudinal direction. A second transporting device is mounted in the settling zone. It is fixed on to the casing and is located after the overflow device in the direction of movement of the light phase l. (author) 10 figs

  17. Selective extraction of copper, mercury, silver and palladium ionsfrom water using hydrophobic ionic liquids.

    Energy Technology Data Exchange (ETDEWEB)

    Papaiconomou, Nicolas; Lee, Jong-Min; Salminen, Justin; VonStosch, Moritz; Prausnitz, John M.

    2007-06-25

    Extraction of dilute metal ions from water was performed near room temperature with a variety of ionic liquids. Distribution coefficients are reported for fourteen metal ions extracted with ionic liquids containing cations 1-octyl-4-methylpyridinium [4MOPYR]{sup +}, 1-methyl-1-octylpyrrolidinium [MOPYRRO]{sup +} or 1-methyl-1-octylpiperidinium [MOPIP]{sup +}, and anions tetrafluoroborate [BF{sub 4}]{sup +}, trifluoromethyl sulfonate [TfO]{sup +} or nonafluorobutyl sulfonate [NfO]{sup +}. Ionic liquids containing octylpyridinium cations are very good for extracting mercury ions. However, other metal ions were not significantly extracted by any of these ionic liquids. Extractions were also performed with four new task-specific ionic liquids. Such liquids containing a disulfide functional group are efficient and selective for mercury and copper, whereas those containing a nitrile functional group are efficient and selective for silver and palladium.

  18. Stability of Anthocyanins from Red Grape Skins under Pressurized Liquid Extraction and Ultrasound-Assisted Extraction Conditions

    Directory of Open Access Journals (Sweden)

    Ali Liazid

    2014-12-01

    Full Text Available The stability of anthocyanins from grape skins after applying different extraction techniques has been determined. The following compounds, previously extracted from real samples, were assessed: delphinidin 3-glucoside, cyanidin 3-glucoside, petunidin 3-glucoside, peonidin 3-glucoside, malvidin 3-glucoside, peonidin 3-acetylglucoside, malvidin 3-acetylglucoside, malvidin 3-caffeoylglucoside, petunidin 3-p-coumaroylglucoside and malvidin 3-p-coumaroylglucoside (trans. The techniques used were ultrasound-assisted extraction and pressurized liquid extraction. In ultrasound-assisted extraction, temperatures up to 75 °C can be applied without degradation of the aforementioned compounds. In pressurized liquid extraction the anthocyanins were found to be stable up to 100 °C. The relative stabilities of both the glycosidic and acylated forms were evaluated. Acylated derivatives were more stable than non-acylated forms. The differences between the two groups of compounds became more marked on working at higher temperatures and on using extraction techniques with higher levels of oxygen in the extraction media.

  19. Extraction of tritium from liquid lithium by permeation

    International Nuclear Information System (INIS)

    Alire, R.M.

    1978-01-01

    This paper assesses a method for extracting tritium from liquid lithium for specific application to the conceptual laser fusion reactor that uses a continuous lithium ''waterfall.'' The tritium diffuses through a refractory metal that contains a getter and is then stored in a hydride-forming alloy. There are various uncertainties with this method including helium-4 extraction, unknown impurities that may accumulate in liquid lithium, the effects of these impurities on tritium separation, and the maintenance of tritium-contaminated equipment. Our study indicates that major tritium losses will occur during equipment maintenance rather than as a result of permeation losses through the primary vessel

  20. Determination of Zinc Ions in Environmental Samples by Dispersive Liquid- Liquid Micro Extraction and Atomic Absorption Spectroscopy

    Directory of Open Access Journals (Sweden)

    F. Arabi

    2012-11-01

    Full Text Available In this work preconcentration of the Zn ions was investigated in water sample by Dispersive liquid- liquid micro extraction (DLLME using chloroform as an extraction solvent, methanol as a disperser solvent and 8-Hydroxyquinoline as a chelating agent. The determination of extracted ions was done by graphite furnace atomic absorption spectrometry. The influence of various analytical parameters including pH, extraction and disperser solvent type and volume and concentration of the chelating agent on the extraction efficiency of analyses was investigated. After extraction, the enrichment factor was 26 and the detection limit of the method was 0.0033 µg l-1 and the relative standard deviations (R.S.D for five determinations of 1 ng/ml Zn were 7.41%. 

  1. Evaluation of Analgesic Activity of Papaver libanoticum Extract in Mice: Involvement of Opioids Receptors

    Directory of Open Access Journals (Sweden)

    Mohamad Ali Hijazi

    2017-01-01

    Full Text Available Papaver libanoticum is an endemic plant to Lebanese region (family Papaveraceae that has not been investigated before. The present study aimed to explore the analgesic activity of dried ethanolic extract of Papaver libanoticum (PLE using tail flick, hot plate, and acetic acid induced writhing models in mice. The involvement of opioid receptors in the analgesic mechanism was investigated using naloxone antagonism. Results demonstrated that PLE exhibited a potent dose dependent analgesic activity in all tested models for analgesia. The analgesic effect involved activation of opioid receptors in the central nervous system, where both spinal and supraspinal components might be involved. The time course for analgesia revealed maximum activity after three hours in both tail flick and hot plate methods, which was prolonged to 24 hours. Metabolites of PLE could be responsible for activation of opioid receptors. The EC50 of PLE was 79 and 50 mg/kg in tail flick and hot plate tests, respectively. The total coverage of analgesia by PLE was double that of morphine in both tests. In conclusion, PLE proved to have opioid agonistic activity with a novel feature of slow and prolonged effect. The present study could add a potential tool in the armaments of opioid drugs as a natural potent analgesic and for treatment of opioid withdrawal syndrome.

  2. Determination of Gemfibrozil (Lipitor and Lopid in Water, Biological Fluids and Drug Matrix by Dispersive Liquid-Liquid micro Extraction (DLLME and Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Ghorbani A.

    2014-07-01

    Full Text Available In this study Dispersive liquid-liquid micro extraction (DLLME coupled with High performance liquid chromatography was applied for the determination of Gemfibrozil in water, drug`s matrix and biological liquids (human plasma and urine. In this method, the appropriate mixture of extraction solvent (200 μl chlorophorm and disperser solvent (1 ml methanol are injected rapidly into the aqueous sample (10.0 ml by syringe, cloudy solution is formed that consisted of fine particles of extraction solvent which is dispersed entirely into aqueous phase. The mixture was centrifuged and the extraction solvent is sedimented on the bottom of the conical test tube. 50 μl of the sedimented phase is puted in a vial and it`s solvent is evaporated. Then 1ml methanol injected to vial and 20 μL of it injected into the HPLC for separation and determination of Gemfibrozil. Some important parameters, such as kind of extraction and disperser solvent, volume of them, extraction time, pH and ionic strength of the aqueous feed solution were optimized. Under the optimum conditions, the enrichment factors and extraction recoveries were 10 and 93.64%. The linear range was (0.1-100.0 mgl-1, limit of detection was 12.3 mgl-1. The relative standard deviations (RSD for 2 mgl-1 of Gemfibrozil in water were 1.3%, (n=10.

  3. Application of ionic liquids based enzyme-assisted extraction of chlorogenic acid from Eucommia ulmoides leaves

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Tingting; Sui, Xiaoyu, E-mail: suixiaoyu@outlook.com; Li, Li; Zhang, Jie; Liang, Xin; Li, Wenjing; Zhang, Honglian; Fu, Shuang

    2016-01-15

    A new approach for ionic liquid based enzyme-assisted extraction (ILEAE) of chlorogenic acid (CGA) from Eucommia ulmoides is presented in which enzyme pretreatment was used in ionic liquids aqueous media to enhance extraction yield. For this purpose, the solubility of CGA and the activity of cellulase were investigated in eight 1-alkyl-3-methylimidazolium ionic liquids. Cellulase in 0.5 M [C6mim]Br aqueous solution was found to provide better performance in extraction. The factors of ILEAE procedures including extraction time, extraction phase pH, extraction temperatures and enzyme concentrations were investigated. Moreover, the novel developed approach offered advantages in term of yield and efficiency compared with other conventional extraction techniques. Scanning electronic microscopy of plant samples indicated that cellulase treated cell wall in ionic liquid solution was subjected to extract, which led to more efficient extraction by reducing mass transfer barrier. The proposed ILEAE method would develope a continuous process for enzyme-assisted extraction including enzyme incubation and solvent extraction process. In this research, we propose a novel view for enzyme-assisted extraction of plant active component, besides concentrating on enzyme facilitated cell wall degradation, focusing on improvement of bad permeability of ionic liquids solutions. - Highlights: • An ionic liquid based enzyme-assisted extraction method of natural product was explored. • ILEAE utilizes enzymatic treatment to improve permeability of ionic liquids solution. • Enzyme incubation and solvent extraction process were ongoing simultaneously. • ILEAE process simplified operating process and suitable for more complete extraction.

  4. Application of ionic liquids based enzyme-assisted extraction of chlorogenic acid from Eucommia ulmoides leaves

    International Nuclear Information System (INIS)

    Liu, Tingting; Sui, Xiaoyu; Li, Li; Zhang, Jie; Liang, Xin; Li, Wenjing; Zhang, Honglian; Fu, Shuang

    2016-01-01

    A new approach for ionic liquid based enzyme-assisted extraction (ILEAE) of chlorogenic acid (CGA) from Eucommia ulmoides is presented in which enzyme pretreatment was used in ionic liquids aqueous media to enhance extraction yield. For this purpose, the solubility of CGA and the activity of cellulase were investigated in eight 1-alkyl-3-methylimidazolium ionic liquids. Cellulase in 0.5 M [C6mim]Br aqueous solution was found to provide better performance in extraction. The factors of ILEAE procedures including extraction time, extraction phase pH, extraction temperatures and enzyme concentrations were investigated. Moreover, the novel developed approach offered advantages in term of yield and efficiency compared with other conventional extraction techniques. Scanning electronic microscopy of plant samples indicated that cellulase treated cell wall in ionic liquid solution was subjected to extract, which led to more efficient extraction by reducing mass transfer barrier. The proposed ILEAE method would develope a continuous process for enzyme-assisted extraction including enzyme incubation and solvent extraction process. In this research, we propose a novel view for enzyme-assisted extraction of plant active component, besides concentrating on enzyme facilitated cell wall degradation, focusing on improvement of bad permeability of ionic liquids solutions. - Highlights: • An ionic liquid based enzyme-assisted extraction method of natural product was explored. • ILEAE utilizes enzymatic treatment to improve permeability of ionic liquids solution. • Enzyme incubation and solvent extraction process were ongoing simultaneously. • ILEAE process simplified operating process and suitable for more complete extraction.

  5. El PLE de investigación-docencia: el aprendizaje como enseñanza.

    OpenAIRE

    Peña, Ismael

    2013-01-01

    Para citar: Peña, I. (2013). El PLE de investigación-docencia: el aprendizaje como enseñanza. En L. Castañeda y J. Adell (Eds.), Entornos Personales de Aprendizaje: Claves para el ecosistema educativo en red (pp. 93-110). Alcoy: Marfil.

  6. Novel materials and methods for solid-phase extraction and liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Ambrose, Diana [Iowa State Univ., Ames, IA (United States)

    1997-06-24

    This report contains a general introduction which discusses solid-phase extraction and solid-phase micro-extraction as sample preparation techniques for high-performance liquid chromatography, which is also evaluated in the study. This report also contains the Conclusions section. Four sections have been removed and processed separately: silicalite as a sorbent for solid-phase extraction; a new, high-capacity carboxylic acid functionalized resin for solid-phase extraction; semi-micro solid-phase extraction of organic compounds from aqueous and biological samples; and the high-performance liquid chromatographic determination of drugs and metabolites in human serum and urine using direct injection and a unique molecular sieve.

  7. On-line control of a liquid-liquid extraction column by the modal control method

    International Nuclear Information System (INIS)

    Bonnefoi, P.; Poujol, A.; Zwingelstein, G.; Dargier, C.; Rouyer, H.

    1977-02-01

    The application of modal analysis to the on-line control of a liquid-liquid extraction column is presented. This process is used in reprocessing for U purification. U in the aqueous acid phase is extracted by a solvent flowing at counter-current. The process is described by 4 nonlinear equations and gives the U and acid concentrations in the two phases. An approximative model is established adapted to the control of the column. Some results of a numerical simulation are given when a single mode is controled. They show that a single sensor allows a good control [fr

  8. Counter current 'emulsion flow' extractor for continuous liquid-liquid extraction from suspended solutions

    International Nuclear Information System (INIS)

    Yanase, Nobuyuki; Naganawa, Hirochika; Nagano, Tetsushi; Noro, Junji

    2011-01-01

    A single current 'emulsion flow' liquid-liquid extraction apparatus has a head with a number of holes from which micrometer-sized droplets of an aqueous phase spout into an organic phase to mix the two liquid phases. For practical use, however, a fatal problem can occur when particulate components in the aqueous phase plug the holes. In the present study, we have succeeded in solving the problem by applying a counter current-type emulsion flow extractor where micrometer-sized droplets of the organic phase are generated. (author)

  9. Liquid liquid extraction of Th(IV) and its complexation study by Calix(4)pyrole

    International Nuclear Information System (INIS)

    Rathod, N.V.; Kamble, J.H.; Malkhede, D.D.

    2015-01-01

    Due to increased demand for carbon-free energy, accelerated growth of nuclear power is foreseen in several countries, especially in China and India. This has made the sustainable use of fuel resources such as uranium and thorium very important. Today, uranium is the main-stay of the present generation of nuclear power plants. However, the anticipated growth in nuclear energy may require introducing thorium as a fuel in future. Meso-octamethyl calix(4)pyrole is known for anion receptor however the present study evaluate the effect of cation for complexation of thorium by liquid liquid extraction technique. Calix(4)pyrole was evaluated for extraction of Th(IV), and 97% extraction efficiency was obtained. Th(IV) was determine with arsenazo(III) at 655 nm. The effect of acid molarity of 0.1 M, 1:5 metal to ligand ratio found efficient for maximum extraction. The stoichiometry ratio 1:2 between metal to ligand is established

  10. Contribution to the study of liquid-liquid extraction dynamics in the case of fast transfers. Extractions of uranium, plutonium and neptunium in a laboratory centrifugal extractor

    International Nuclear Information System (INIS)

    Bergeonneau, Philippe

    1978-01-01

    The liquid-liquid extraction (also named solvent-based extraction) is a very important technique for the reprocessing of irradiated nuclear fuels. This research thesis is based on the use of a laboratory centrifugal extractor which allows interesting conditions to be achieved: fast transfer due to an intense solution mixing, very short duration of contact between solutions. Thus, after a report of a bibliographical study on chemical mechanisms of extraction, on the composition of extracted species, on extraction kinetics, and on centrifugal extractors, this thesis reports the design, fabrication and use of a centrifugal extractor: presentation of fundamental principles, description and characteristics (materials, hydrodynamic operation test and problems, prototype). It reports studies of fast transfer kinetics: mathematical processing, result interpretation, results and discussions of extraction kinetics for nitric acid, uranium VI and IV, plutonium IV, neptunium IV, and comparison of the different extraction kinetics

  11. On the problems of Ba, Pb, Zn Ple{e ore deposit (Slovenia

    Directory of Open Access Journals (Sweden)

    Ivan Mlakar

    2003-12-01

    Full Text Available In this paper we present the years ago collected unpublished data on the Ple{e ore deposit which we completed also with some recent ones. They all speak against the offered interpretation of the geologic structure (Dozet, 1999, and especially against the Skythianage of this Ba, Pb and Zn deposit.We showed that the two large concordant barite bodies of syngenegtic origin are associated with an exactly determined horizon within the Carboniferous beds, that they were formed almost certainly in relation with the Asturian orogenic phase, and that theyoccur by chance in the hanging wall contact with the Skythian dolomite along a thrust plane. During Tertiary the epigenetic remobilization brought the ore substance from Paleozoic rocks into the mentioned dolomite. In one of the carefully investigated geochemictraverses the remobilization distance for Pb and Hg is 70 meters, and for Ba greater than 100 meters.For the existence of the PleŠe barite-bearing formation as conceived by Dozet (1999 there are no infallible proofs.

  12. Liquid-liquid reductive extraction in molten fluoride salt/liquid aluminium as a core of process for the An/Ln group separation

    International Nuclear Information System (INIS)

    Conocar, O.

    2007-06-01

    This report concerns a pyrochemical process based on liquid-liquid extraction in a molten fluoride/liquid aluminium system as a core process for actinide (An)/lanthanide (Ln) group separation, studied at CEA. The basic and demonstrative experiments have established the feasibility of the An/Ln group separation in the molten fluoride/liquid aluminium system (U, Pu, Np, Am, Cm traces from Nd, Ce, Eu, Sm, Eu, La - An/Ln separation factors over 1000 - An recovery yield over 98 % in one batch). The main experimental efforts must now be targeted on the recovery of actinides from the Al matrix. A thermodynamic and bibliographical survey has been done. It shows that back-extraction in a molten chloride melt could be a promising technique for this purpose

  13. Liquid-liquid reductive extraction in molten fluoride salt/liquid aluminium as a core of process for the An/Ln group separation

    Energy Technology Data Exchange (ETDEWEB)

    Conocar, O

    2007-06-15

    This report concerns a pyrochemical process based on liquid-liquid extraction in a molten fluoride/liquid aluminium system as a core process for actinide (An)/lanthanide (Ln) group separation, studied at CEA. The basic and demonstrative experiments have established the feasibility of the An/Ln group separation in the molten fluoride/liquid aluminium system (U, Pu, Np, Am, Cm traces from Nd, Ce, Eu, Sm, Eu, La - An/Ln separation factors over 1000 - An recovery yield over 98 % in one batch). The main experimental efforts must now be targeted on the recovery of actinides from the Al matrix. A thermodynamic and bibliographical survey has been done. It shows that back-extraction in a molten chloride melt could be a promising technique for this purpose.

  14. Characterization of rhamnolipids by liquid chromatography/mass spectrometry after solid-phase extraction.

    Science.gov (United States)

    Behrens, Beate; Engelen, Jeannine; Tiso, Till; Blank, Lars Mathias; Hayen, Heiko

    2016-04-01

    Rhamnolipids are surface-active agents with a broad application potential that are produced in complex mixtures by bacteria of the genus Pseudomonas. Analysis from fermentation broth is often characterized by laborious sample preparation and requires hyphenated analytical techniques like liquid chromatography coupled to mass spectrometry (LC-MS) to obtain detailed information about sample composition. In this study, an analytical procedure based on chromatographic method development and characterization of rhamnolipid sample material by LC-MS as well as a comparison of two sample preparation methods, i.e., liquid-liquid extraction and solid-phase extraction, is presented. Efficient separation was achieved under reversed-phase conditions using a mixed propylphenyl and octadecylsilyl-modified silica gel stationary phase. LC-MS/MS analysis of a supernatant from Pseudomonas putida strain KT2440 pVLT33_rhlABC grown on glucose as sole carbon source and purified by solid-phase extraction revealed a total of 20 congeners of di-rhamnolipids, mono-rhamnolipids, and their biosynthetic precursors 3-(3-hydroxyalkanoyloxy)alkanoic acids (HAAs) with different carbon chain lengths from C8 to C14, including three rhamnolipids with uncommon C9 and C11 fatty acid residues. LC-MS and the orcinol assay were used to evaluate the developed solid-phase extraction method in comparison with the established liquid-liquid extraction. Solid-phase extraction exhibited higher yields and reproducibility as well as lower experimental effort.

  15. Can the integration of a PLE in an e-portfolio platform improve generic competences?

    Directory of Open Access Journals (Sweden)

    Cristina Galván-Fernández

    2017-07-01

    Full Text Available The study analyzes the improvement in generic competences through e-portfolio/PLE platform and didactic planning. The new version of the platform, Digital Folder, contains utilities for students and teachers and some PLE components that help the learning process through e-portfolios. Didactic planning is compared for students from the University of Vic and the University of Barcelona, with a total of 61 participants. A questionnaire has been applied for measuring the use of functions and how much these functions aid in the improvement of the generic competences (reflection, planning and selection of information. The results confirm that the most helpful functions for students are: the Schedule, the Academic tasks, the Teacher’s portfolio and Dialogue with the teacher. However, the implication of these functions in the improvement of the competences depends on didactic planning overall for reflection on learning.

  16. Removal of actinide elements from liquid scintillation cocktail wastes using liquid-liquid extraction and demulsification techniques

    International Nuclear Information System (INIS)

    Foltz, K.; Landsberger, S.; Srinivasan, B.; Vandegrift, G.F.

    1994-01-01

    For many years liquid scintillation cocktail (LSC) wastes have been generated and stored at Argonne National Laboratory (ANL). These wastes are stored in thousands of 10--20 m scintillation vials, many of which contain elements with Z > 88. Because storage space is limited, disposal of this waste is pressing. These wastes could be commercially incinerated if the radionuclides with Z>88 are reduced to sufficiently low levels. However, there is currently no deminimus level for these radionuclides, and separation techniques are still being tested. The University of Illinois is conducting experiments to separate radionuclides with Z > 88 from simulated LSC wastes by using liquid-liquid extraction (LLX) and demulsification techniques. The actinide elements are removed from the LSC by extraction into an aqueous phase after the cocktail has been demulsified. The aqueous and organic phases are separated and the organic phase, now free from radionuclides with Z > 88, can be sent to a commercial incineration facility. The aqueous phase may be treated and disposed of using existing techniques. The LLX separation techniques used solutions of sodium oxalate, aluminum nitrate, and tetrasodium EDTA at varying concentrations. These extractants were mixed with the simulated waste in a 1:1 volume ratio. Using 1.0M Na 4 EDTA salt solutions, decontamination ratios as high as 230 were achieved

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

    Science.gov (United States)

    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.

  18. Combination of solvent extractants for dispersive liquid-liquid microextraction of fungicides from water and fruit samples by liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Pastor-Belda, Marta; Garrido, Isabel; Campillo, Natalia; Viñas, Pilar; Hellín, Pilar; Flores, Pilar; Fenoll, José

    2017-10-15

    A multiresidue method was developed to determine twenty-five fungicides belonging to three different chemical families, oxazoles, strobilurins and triazoles, in water and fruit samples, using dispersive liquid-liquid microextraction (DLLME) and liquid chromatography/tandem mass spectrometry (LC-MS 2 ). Solid-liquid extraction with acetonitrile was used for the analysis in fruits, the extract being used as dispersant solvent in DLLME. Since some of the analytes showed high affinity for chloroform and the others were more efficiently extracted with undecanol, a mixture of both solvents was used as extractant in DLLME. After evaporation of CHCl 3 , the enriched phase was analyzed. Enrichment factors in the 23-119 and 12-60 ranges were obtained for waters and fruits, respectively. The approach was most sensitive for metominostrobin with limits of quantification of 1ngL -1 and 5ngkg -1 in waters and fruits, respectively, while a similar sensitivity was attained for tebuconazole in fruits. Recoveries of the fungicides varied between 86 and 116%. Copyright © 2017 Elsevier Ltd. All rights reserved.

  19. Determination of sedative hypnotics in sewage sludge by pressurized liquid extraction with high-performance liquid chromatography and tandem mass spectrometry.

    Science.gov (United States)

    Arbeláez, Paula; Granados, Judith; Borrull, Francesc; Marcé, Rosa Maria; Pocurull, Eva

    2014-12-01

    This paper describes a method for the determination of eight sedative hypnotics (benzodiazepines and barbiturates) in sewage sludge using pressurized liquid extraction and liquid chromatography with tandem mass spectrometry. Pressurized liquid extraction operating conditions were optimized and maximum recoveries were reached using methanol under the following operational conditions: 100ºC, 1500 psi, extraction time of 5 min, one extraction cycle, flush volume of 60% and purge time of 120 s. Pressurized liquid extraction recoveries were higher than 88% for all the compounds except for carbamazepine (55%). The repeatability and reproducibility between days, expressed as relative standard deviation (n = 5), were lower than 6 and 10%, respectively. The detection limits for all compounds were lower than 12.5 μg/kg of dry weight. The method was applied to determine benzodiazepines and barbiturates in sewage sludge from urban sewage treatment plants, and carbamazepine showed the highest concentration (7.9-18.9 μg/kg dry weight). © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Separation of uranium from aqueous solutions using calix[6]arenes in liquid-liquid extraction as well as solid phase extraction

    International Nuclear Information System (INIS)

    Schmeide, K.; Geipel, G.; Bernhard, G.

    2004-11-01

    The suitability of different calyx[n] arene types for uranyl extraction from liquid solutions was examined by means of liquid-liquid extraction using aqueous phases and organic solvents of varying compositions. It was found that COOH-derivatised calyx[6] arenes have good extraction properties and can even be used in the acid pH range. The use of calixarene-modified fleeces for the separation of uranyl from aqueous phases was examined in batch experiments with pH and uranyl concentration as variables and in the presence or absence of competing ions. The results showed that calixarene-modified fleeces can be used for uranium separation starting from pH 4. At pH 5, up to a maximum of 7.6 x 10 -7 mol uranium can be bound per 1 g of calixarene-modified fleece. The separation of uranyl from synthetic pit waters was examined as a means of testing the separation capacity of calixarene-modified fleeces in environmentally sensitive waters. Studies on the reversibility of uranium bonding to calixarene-treated polyester fleeces have shown that under environmentally realistic conditions (neutral pH range) the uranium is firmly bound to the calixarene-modified fleeces and cannot be mobilised. By contrast, in acidic environments calixarene-modified fleeces are capable of near-complete regeneration. Such regenerated textile filter materials can then be used for further uranium separation cycles [de

  1. Liquid-liquid extraction of uranium(VI) using Cyanex 272 in toluene from sodium salicylate medium

    International Nuclear Information System (INIS)

    Madane, Namdev S.; Nikam, Gurunath H.; Jadhav, Deepali V.; Mohite, Baburao S.

    2011-01-01

    Liquid-liquid extraction of U(VI) from sodium salicylate media using Cyanex 272 in toluene has been carried out. Uranium(VI) was quantitatively extracted from 1 x 10 -3 M sodium salicylate with 5 x 10 -4 M Cyanex 272 in toluene. It was stripped quantitatively from the organic phase with 1M HCl and determined spectrophotometrically with arsenazo(III) at 660 nm. The effect of concentrations of sodium salicylate, extractant, diluents, metal ion and strippants have been studied. Separation of uranium(VI) from other elements was achieved from binary as well as from multicomponent mixtures. The method was extended to determination of uranium(VI) in geological samples. The method is simple, rapid and selective with good reproducibility (approximately ± 2%). (author)

  2. Studies of extractant molecules in solution and at liquid-liquid interfaces: structural and mechanistic aspects of synergy effects

    International Nuclear Information System (INIS)

    Baaden, Marc

    2000-01-01

    Molecular dynamics simulations reported herein provide new important insights into cation recognition and complexation in solution as well as liquid-liquid extraction, with a particular focus on the microscopic events taking place at the interface between two immiscible liquids. Preliminary studies concerned the representation of the trivalent rare earth cations La 3+ , Eu 3+ and Yb 3+ in force field simulations, probing structural and energetic features on an experimentally characterized model system based on substituted pyridine dicarboxamide ligands. Complexation of such cations by a novel calixarene derivative was investigated showing unexpected features, such as the position of the cation in the complex. Independent experimental studies published subsequently support these findings. Another part of the work is related to industrial liquid-liquid extraction systems using tri-n-butyl phosphate (TBP) as co-solvent, extractant, surfactant and synergist. We investigate 1) concentration effects simulating up to 60 TBP at a water/chloroform interface, 2) acidity using a neutral and ionic model of HNO 3 and 3) synergistic aspects of mixed TBP/calixarene extraction systems. These simulations provide the first microscopic insights into such issues. We finally addressed the topic of solute transfer across the water/chloroform interface. The potential of mean force for such a process has been calculated by both standard methods and novel approaches [fr

  3. A novel method for analysing key corticosteroids in polar bear (Ursus maritimus) hair using liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Weisser, Johan J; Hansen, Martin; Björklund, Erland; Sonne, Christian; Dietz, Rune; Styrishave, Bjarne

    2016-04-01

    This paper presents the development and evaluation of a methodology for extraction, clean-up and analysis of three key corticosteroids (aldosterone, cortisol and corticosterone) in polar bear hair. Such a methodology can be used to monitor stress biomarkers in polar bears and may provide as a useful tool for long-term and retrospective information. We developed a combined pressurized liquid extraction (PLE)-solid phase extraction (SPE) procedure for corticosteroid extraction and clean-up followed by high pressure liquid chromatography tandem mass spectrometry (HPLC-MS/MS) analysis. This procedure allows for the simultaneous determination of multiple steroids, which is in contrast to previous polar bear studies based on ELISA techniques. Absolute method recoveries were 81%, 75% and 60% for cortisol, corticosterone and aldosterone, respectively. We applied the developed method on a hair sample pooled from four East Greenland polar bears. Herein cortisol and corticosterone were successfully determined in levels of 0.32±0.02ng/g hair and 0.13±0.02ng/g hair, respectively. Aldosterone was below limit of detection (LODpolar bears was consistent with cortisol levels previously determined in the Southern Hudson Bay and James Bay in Canada using ELISA kits. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Application of liquid-liquid extraction in separation of rare earths [Paper No. : V-6

    International Nuclear Information System (INIS)

    Deshpande, S.M.; Krishnan, N.P.K.; Murthy, T.K.S.; Swaminathan, T.V.

    1979-01-01

    The rare earths consist of fifteen elements which have very similar chemical properties and are difficult to separate from each other. Since they exist together in all naturally occurring minerals their separation is one of the important and difficult aspects of their technology. Liquid-liquid extraction has proved to be an efficient technique for their separation. The two important extraction systems that find practical and large scale application, the nitric acid + tri-n-butyl phosphate, and mineral acid (particularly hydrochloric acid) + organo phosphoric acid (like di-2-ethyl hexyl phosphoric acid), are briefly reviewed. The factors affecting the extraction and separation of rare earths in the two systems are discussed. On an industrial scale the extraction process is very often employed for an initial concentration of the desired rare earths from complex mixtures. The final purification is generally achieved by the ion exchange method. The utility of the solvent extraction process for the upgrading of selected rare earths-europium, samarium and gadolinium-from a mixed rare earth chloride, derived from monazite, is illustrated by the work carried out in this laboratory and pilot plant operation at the Alwaye plant of M/s. Indian Rare Earths Ltd. (author)

  5. Double-blind, Placebo-controlled Trial to Evaluate the Effectiveness of Polypodium Leucotomos Extract in the Treatment of Melasma in Asian Skin

    Science.gov (United States)

    Chuah, Sai Yee; Tien, Steven; Thng, Guan; Vitale, María Alejandra; Delgado-Rubin, Arancha

    2018-01-01

    Introduction: Melasma is a common pigmentary disorder with a multifactorial etiology that can hinder its management. The aqueous extract of the fern Polypodium leucotomos (PLE), Fernblock® (IFC, Madrid, Spain), has demonstrated antioxidant and photoprotective activities and has been used for the treatment of several pigmentary disorders. The aim of this study was to evaluate the efficacy and safety of oral PLE in the treatment of melasma in Asian patients. Methods: Forty healthy adult patients with clinical diagnoses of melasma who were receiving treatment with topical 4% hydroquinone cream and sunscreen with a sun protection factor (SPF) of 50+ were recruited for inclusion in this study from the National Skin Centre in Singapore. They were randomized to receive either oral PLE supplementation or placebo for 12 weeks. Patients were assessed at baseline, Day 28, Day 56, and Day 84 using the modified Melasma Area and Severity Index (mMASI); melanin and erythema indexes; VISIA® photography (Canfield Scientific, Parsippany, New Jersey, USA); and the Melasma Quality of Life (MelasQoL) questionnaire. Adverse events were recorded. Results: Following four, eight, and 12 weeks of treatment, there were statistically significant differences between the mMASI scores of both groups as compared with the baseline scores (p≤0.01). mMASI scores of the PLE group at eight and 12 weeks were also significantly lower than those of the placebo group (p≤0.05). At the end of the study, a significant improvement was reached in both groups (both p≤0.01), with no significant differences between them. The scores of the melanin and erythema indices displayed a slight improvement in both groups, without significant differences among them. MelasQoL score showed an improvement in the PLE group versus the placebo group. Our results demonstrate that the PLE aqueous extract product significantly improves and accelerates the outcome reached with hydroquinone and sunscreen almost from the first

  6. Thermodynamic equilibrium model to predict the cobalt distribution coefficient in the CoCl2--HCl--H2O--TBP liquid--liquid extraction system

    International Nuclear Information System (INIS)

    Nevarez, M.; Bautista, R.G.

    1976-01-01

    The development of a thermodynamic equilibrium model to predict the cobalt distribution coefficient in the CoCl 2 -HCl-H 2 O-TBP system is described. The model makes use of the various aqueous phase cobaltous chloride complexes stoichiometric stability constants expressed as their degree of formation, their mechanism of extraction into the organic phase, and the equilibrium constant for the extraction reaction. The model was verified by the good agreement between the calculated cobalt distribution coefficients and those obtained experimentally both in the present study and published by other investigators. The optimum extraction of cobalt by the TBP occurred at an HCl equilibrium aqueous place concentration between 8.5 and 9.5M. The development of efficient procedures for the separation and concentration of important industrial metals from their aqueous solutions by liquid-liquid extraction has recently been given impetus by the realization of an impending shortage of energy and mineral resources. Liquid-liquid extraction is one of the few methods by which it is possible to quantitatively separate elements which are similar in properties. The use of liquid-liquid extraction to separate cobalt and nickel, which very frequently occur in nature together, is an important separation problem in nonferrous metallurgy. There is some fundamental information available in the chemical literature regarding the mechanism and equilibrium thermodynamic properties of selected liquid-liquid extraction systems. This research effort shows how this available information can be utilized to improve existing separation and concentration theory and technique. The development and application of a thermodynamic equilibrium model for describing the liquid-liquid extraction of cobaltous chloride from aqueous HCl solutions by tributyl phosphate (TBP) using experimental data obtained in this investigation and from the literature are presented

  7. Application of ionic liquid for extraction and separation of bioactive compounds from plants.

    Science.gov (United States)

    Tang, Baokun; Bi, Wentao; Tian, Minglei; Row, Kyung Ho

    2012-09-01

    In recent years, ionic liquids (ILs), as green and designer solvents, have accelerated research in analytical chemistry. This review highlights some of the unique properties of ILs and provides an overview of the preparation and application of IL or IL-based materials to extract bioactive compounds in plants. IL or IL-based materials in conjunction with liquid-liquid extraction (LLE), ultrasonic-assisted extraction (UAE), microwave-assisted extraction (MAE), high performance liquid chromatography (HPLC) and solid-phase extraction (SPE) analytical technologies etc., have been applied successfully to the extraction or separation of bioactive compounds from plants. This paper reviews the available data and references to examine the advantages of IL and IL-based materials in these applications. In addition, the main target compounds reviewed in this paper are bioactive compounds with multiple therapeutic effects and pharmacological activities. Based on the importance of the targets, this paper reviews the applications of ILs, IL-based materials or co-working with analytical technologies. The exploitation of new applications of ILs on the extraction of bioactive compounds from plant samples is expected to increase. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. Application of liquid metals for the extraction of solid metals

    International Nuclear Information System (INIS)

    Borgstedt, H.U.

    1996-01-01

    Liquid metals dissolve several solid metals in considerable amounts at moderate temperatures. The dissolution processes may be based upon simple physical solubility, formation of intermetallic phases. Even chemical reactions are often observed in which non-metallic elements might be involved. Thus, the capacity to dissolve metals and chemical properties of the liquid metals play a role in these processes. Besides the solubility also chemical properties and thermochemical data are of importance. The dissolution of metals in liquid metals can be applied to separate the solutes from other metals or non-metallic phases. Relatively noble metals can be chemically reduced by the liquid phases. Such solution processes can be applied in the extractive metallurgy, for instance to extract metals from metallic waste. The recycling of metals is of high economical and ecological importance. Examples of possible processes are discussed. (author)

  9. 99TCM-dextran scintigraphy in protein losing enteropathy (PLE)

    International Nuclear Information System (INIS)

    Gibson, M.; Larden, D.W.; Angelides, S.; Roman, M.R.

    2003-01-01

    Full text: Protein losing enteropathy (PLE) is an uncommon complication following right heart bypass operations (Fontan procedure-FP) caused by chronically raised systemic venous pressure with perhaps concomitant immunological or inflammatory factors. Medical, transcatheter, and surgical therapies aimed at reducing systemic venous pressure are often unsuccessful. Conversely, where intestinal protein loss is circumscribed to a relatively small region, surgical resection has been reported as beneficial. However, confirmation of localised disease is difficult. Nuclear scintigraphy can potentially determine extent of disease. A 14-year-old girl with a background history of tricuspid atresia, right ventricular hypoplasia and ventricular- and atrial-septal defects developed PLE post-FP, resulting in cardiac failure, chronic pleural effusions and worsening ascites. Her condition gradually deteriorated and became refractory to therapy. A 99Tcm-Dextran study was performed for further evaluation. 99Tcm-Dextran 77 000 (260 MBq) was produced aseptically from a previously prepared sterile 'cold kit'. Radiochemical purity was found to be > 95%. Anterior and posterior planar scans of the lower chest, abdomen and pelvis were acquired continuously over the initial 2 h post-intravenous injection of radiotracer using a dual-head gamma-camera. There was focal abnormal accumulation of tracer in the left flank demonstrated, consistent with localised disease, which was confirmed on subsequent small bowel biopsies. The patient is awaiting a limited small bowel resection. Thus, 99Tcm-Dextran scintigraphy was useful in determining extent of disease and further management. Copyright (2003) The Australian and New Zealand Society of Nuclear Medicine Inc

  10. Liquid-solid extraction of cationic metals by cationic amphiphiles

    International Nuclear Information System (INIS)

    Muller, W.

    2010-01-01

    In the field of selective separation for recycling of spent nuclear fuel, liquid-liquid extraction processes are widely used (PUREX, DIAMEX..) in industrial scale. In order to guarantee a sustainable nuclear energy for the forthcoming generations, alternative reprocessing techniques are under development. One of them bases on the studies from Heckmann et al in the 80's and consists in selectively precipitating actinides from aqueous waste solutions by cationic surfactants (liquid-solid extraction). This technique has some interesting advantages over liquid-liquid extraction techniques, because several steps are omitted like stripping or solvent washing. Moreover, the amount of waste is decreased considerably, since no contaminated organic solvent is produced. In this thesis, we have carried out a physico-chemical study to understand the specific interactions between the metallic cations with the cationic surfactant. First, we have analysed the specific effect of the different counter-ions (Cl - , NO 3 - , C 2 O 4 2- ) and then the effect of alkaline cations on the structural properties of the surfactant aggregation in varying thermodynamical conditions. Finally, different multivalent cations (Cu 2+ , Zn 2+ , UO 2 2+ , Fe 3+ , Nd 3+ , Eu 3+ , Th 4+ ) were considered; we have concluded that depending on the anionic complex of these metals formed in acidic media, we can observe either an adsorption at the micellar interface or not. This adsorption has a large influence of the surfactant aggregation properties and determines the limits of the application in term of ionic strength, temperature and surfactant concentration. (author) [fr

  11. Development and Application of Immunoaffinity Chromatography for Coplanar PCBs in Soil and Sediment

    Science.gov (United States)

    An immunoaffinity chromatography (IAC) column was developed as a simple cleanup procedure for preparing environmental samples for analysis of polychlorinated biphenyls (PCBs). Soil and sediment samples were prepared using pressurized liquid extraction (PLE), followed by the IAC c...

  12. Extraction of toluene from aliphatic compounds using an ionic liquid as solvent: Influence of the alkane on the (liquid + liquid) equilibrium

    International Nuclear Information System (INIS)

    Gonzalez, Emilio J.; Calvar, Noelia; Dominguez, Irene; Dominguez, Angeles

    2011-01-01

    Research highlights: → An ionic liquid was analyzed as solvent for extraction of toluene from alkanes. → Liquid-liquid equilibrium data were measured at 298.15 K and atmospheric pressure. → Selectivity and solute distribution ratio were obtained and compared with literature. → The Othmer-Tobias equation was used to ascertain the experimental LLE data. → Experimental data were correlated using NRTL and UNIQUAC models. - Abstract: In this paper, the feasibility of using 1-ethyl-3-methylimidazolium ethylsulfate ionic liquid, [EMim][ESO 4 ], as solvent for the extraction of toluene from aliphatic compounds (hexane, heptane, octane, or nonane) was analyzed. (Liquid + liquid) equilibrium (LLE) data for the ternary systems {alkane (1) + toluene (2) + [EMim][ESO 4 ] (3)} were measured at T = 298.15 K and atmospheric pressure. Selectivity and solute distribution ratio were calculated from the experimental LLE data, and the obtained values were compared to those previously reported using other ionic liquids and sulfolane. The degree of consistency of the experimental LLE data was ascertained using the Othmer-Tobias equation. Finally, the experimental LLE data were satisfactorily correlated with NRTL and UNIQUAC models.

  13. Liquid-liquid extraction to lithium isotope separation based on room-temperature ionic liquids containing 2,2'-binaphthyldiyl-17-crown-5

    International Nuclear Information System (INIS)

    Sun Xiaoli; Zhou Wen; Gu Lin; Qiu Dan; Ren Donghong; Gu Zhiguo; Li Zaijun

    2015-01-01

    A novel liquid-liquid extraction system was investigated for the selective separation of lithium isotopes using ionic liquids (ILs = C 8 mim + PF 6 - , C 8 mim + BF 4 - , and C 8 mim + NTf 2 - ) as extraction solvent and 2,2'-binaphthyldiyl-17-crown-5 (BN-17-5) as extractant. The effects of the concentration of lithium salt, counter anion of lithium salt, initial pH of aqueous phase, extraction temperature, and time on the lithium isotopes separation were discussed. Under optimized conditions, the maximum single-stage separation factor α of 6 Li/ 7 Li obtained in the present study was 1.046 ± 0.002, indicating the lighter isotope 6 Li was enriched in IL phase while the heavier isotope 7 Li was concentrated in the solution phase. The formation of 1:1 complex Li(BN-17-5) + in the IL phase was determined on the basis of slope analysis method. The large value of the free energy change (-ΔG° = 92.89 J mol -1 ) indicated the high separation capability of the Li isotopes by BN-17-5/IL system. Lithium in Li(BN-17-5) + complex was stripped by 1 mol L -1 HCl solution. The extraction system offers high efficiency, simplicity, and green application prospect to lithium isotope separation. (author)

  14. Study on the extraction of rare earth elements in liquid bismuth

    International Nuclear Information System (INIS)

    Harada, M.; Adachi, M.; Kai, Y.; Koike, K.

    1987-01-01

    Three factors, which are important for the extraction of rare earth elements in liquid bismuth - molten salt system, were studied, i. e., the equilibrium distribution of neodymium, samarium and bismuth between molten LiCl - liquid Bi-Li alloys, the extraction rate of rare earths, and the characteristics of the extractor with drop dispersion. The rare earth elements were extracted through redox reactions. In high range of Li-mole fraction in the alloy phase, X Li , the distribution of neodymium and bismuth in the salt phase markedly increased as X Li increased. The anomalous increase is attributed to the formation of the compound comprised of Nd, Li, Bi and oxygen in the salt phase. The redox reaction processes were very fast and the extraction rates for rare earths are controlled by the diffusion processes of the solute and the metallic lithium. The process for the formation of liquid metal drops in the continuous phase is predictable from semiempirical correlations reported for aqueous solution - organic solvent systems. The height of droplet bed being accumulated on drop settling portion is predictable from the coalescence time of single drop to a flat metal interface. The coalescence of metal drop to clean interface was very fast. The extractor type of liquid metal dispersion in molten salt is suitable for the extraction process in the fuel reprocessing of MSR or MSBR. (author)

  15. Liquid-liquid extraction of ion-association complexes of cobalt(II-4-(2-pyridylazoresorcinol with ditetrazolium salts

    Directory of Open Access Journals (Sweden)

    Divarova Vidka V.

    2015-01-01

    Full Text Available The formation and liquid-liquid extraction of ion-association complexes between Co(II-4-(2-Pyridylazoresorcinol (PAR anionic chelates and cations of three ditetrazolium chlorides were studied: Blue Tetrazolium chloride (BTC, Neotetrazolium chloride (NTC and Nitro Blue Tetrazolium chloride (NBT. The optimum conditions for the formation and solvent extraction of the ion-association comlpex chelates were determined. It has been found that in the systems of Co(II-PAR-DTS, the reactants are reacted in molar ratios 1:2:1 and the general formula of complexes was suggested. The extraction equilibria were investigated and quantitatively characterized by the equilibrium constants and the recovery factors. The analytical characteristics of the complexes were calculated.

  16. Predictive thermodynamic models for liquid--liquid extraction of single, binary and ternary lanthanides and actinides

    International Nuclear Information System (INIS)

    Hoh, Y.C.

    1977-03-01

    Chemically based thermodynamic models to predict the distribution coefficients and the separation factors for the liquid--liquid extraction of lanthanides-organophosphorus compounds were developed by assuming that the quotient of the activity coefficients of each species varies slightly with its concentrations, by using aqueous lanthanide or actinide complexes stoichiometric stability constants expressed as its degrees of formation, by making use of the extraction mechanism and the equilibrium constant for the extraction reaction. For a single component system, the thermodynamic model equations which predict the distribution coefficients, are dependent on the free organic concentration, the equilibrated ligand and hydrogen ion concentrations, the degree of formation, and on the extraction mechanism. For a binary component system, the thermodynamic model equation which predicts the separation factors is the same for all cases. This model equation is dependent on the degrees of formation of each species in their binary system and can be used in a ternary component system to predict the separation factors for the solutes relative to each other

  17. Fast and comprehensive analysis of secondary metabolites in cocoa products using ultra high-performance liquid chromatography directly after pressurized liquid extraction.

    Science.gov (United States)

    Damm, Irina; Enger, Eileen; Chrubasik-Hausmann, Sigrun; Schieber, Andreas; Zimmermann, Benno F

    2016-08-01

    Fast methods for the extraction and analysis of various secondary metabolites from cocoa products were developed and optimized regarding speed and separation efficiency. Extraction by pressurized liquid extraction is automated and the extracts are analyzed by rapid reversed-phase ultra high-performance liquid chromatography and normal-phase high-performance liquid chromatography methods. After extraction, no further sample treatment is required before chromatographic analysis. The analytes comprise monomeric and oligomeric flavanols, flavonols, methylxanthins, N-phenylpropenoyl amino acids, and phenolic acids. Polyphenols and N-phenylpropenoyl amino acids are separated in a single run of 33 min, procyanidins are analyzed by normal-phase high-performance liquid chromatography within 16 min, and methylxanthins require only 6 min total run time. A fourth method is suitable for phenolic acids, but only protocatechuic acid was found in relevant quantities. The optimized methods were validated and applied to 27 dark chocolates, one milk chocolate, two cocoa powders and two food supplements based on cocoa extract. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Hollow fibre supported liquid membrane extraction of ...

    African Journals Online (AJOL)

    A simple sample pre-treatment method utilizing hollow fibre supported liquid membrane (HFSLM) was carried out on pharmaceuticals samples comprising of cough syrups (CS1 and CS2) and an anti-inflammatory product (AI). The active ingredients targeted in the extraction process were diphenylhydramine (DPH), ...

  19. Extraction of lithium ion from alkaline aqueous media by a liquid surfactant membrane

    International Nuclear Information System (INIS)

    Kinugasa, Takumi; Ono, Yuri; Kawamura, Yuko; Watanabe, Kunio; Takeuchi, Hiroshi.

    1995-01-01

    Extraction of lithium ion from aqueous alkaline media by a liquid surfactant membrane was performed using a mixture of LIX54 and TOPO as the extractant. Stripping of lithium from the kerosene solution to the acid solution was suppressed with increasing content of polyamine (ECA) surfactant. The extraction rate of lithium by the liquid membrane could be interpreted taking account of an interfacial resistance due to ECA. It was confirmed that swelling of the (W/O) emulsion drops by water permeation through the liquid membrane is evaluated in terms of a change in osmotic pressure gradient between the external and internal aqueous phases during the lithium extraction. In the present operation, the extraction ratio of Li + from the external feed and the uptake into the internal phase reached as high as 95%. (author)

  20. Use of water in aiding olefin/paraffin (liquid + liquid) extraction via complexation with a silver bis(trifluoromethylsulfonyl)imide salt

    International Nuclear Information System (INIS)

    Wang, Yu; Thompson, Jillian; Zhou, Jingjing; Goodrich, Peter; Atilhan, Mert; Pensado, Alfonso S.; Kirchner, Barbara; Rooney, David; Jacquemin, Johan; Khraisheh, Majeda

    2014-01-01

    Highlights: • Silver-based ILs used as olefin extracting agents for olefin/paraffin mixtures. • Each extraction process is based on the olefin complexation and solvation. • The presence of water influences positively each extraction process. • Each extraction process was evaluated by DFT calculations, NMR, IR and Raman. • LLE data were then correlated by using the UNIQUAC model. - Abstract: This paper describes the extraction of C 5 –C 8 linear α-olefins from olefin/paraffin mixtures of the same carbon number via a reversible complexation with a silver salt (silver bis(trifluoromethylsulfonyl)imide, Ag[Tf 2 N]) to form room temperature ionic liquids [Ag(olefin) x ][Tf 2 N]. From the experimental (liquid + liquid) equilibrium data for the olefin/paraffin mixtures and Ag[Tf 2 N], 1-pentene showed the best separation performance while C 7 and C 8 olefins could only be separated from the corresponding mixtures on addition of water which also improves the selectivity at lower carbon numbers like the C 5 and C 6 , for example. Using infrared and Raman spectroscopy of the complex and Ag[Tf 2 N] saturated by olefin, the mechanism of the extraction was found to be based on both chemical complexation and the physical solubility of the olefin in the ionic liquid ([Ag(olefin) x ][Tf 2 N]). These experiments further support the use of such extraction techniques for the separation of olefins from paraffins

  1. Complex Formation in a Liquid-Liquid Extraction System Containing Cobalt(II), 4-(2-Pyridylazo)resorcinol, and Nitron

    OpenAIRE

    Racheva, Petya Vassileva; Gavazov, Kiril Blazhev; Lekova, Vanya Dimitrova; Dimitrov, Atanas Nikolov

    2013-01-01

    Complex formation and liquid-liquid extraction were studied in a system containing cobalt(II), 4-(2-pyridylazo)resorcinol (PAR), 1,4-diphenyl-3-(phenylamino)-1H-1,2,4-triazole (Nitron, Nt), water, and chloroform. The effect of some experimental parameters (pH, shaking time, concentration of PAR, and concentration of Nt) was systematically investigated, and the optimum conditions for cobalt extraction as an ion-association complex, (NtH+)[Co3+(PAR)2], were found. The following key equilibrium ...

  2. Emulsion liquid membrane for selective extraction of bismuth from nitrate medium

    International Nuclear Information System (INIS)

    Mokhtari, Bahram; Pourabdollah, Kobra

    2013-01-01

    The novelty of this work is the selective extraction of bismuth ions from nitrate medium by emulsion liquid membrane. Di(2-ethylhexyl)phosphoric acid was used as extractant of bismuth ions from nitrate medium by emulsion liquid membrane, and Triton X-100 was used as the biodegradable surfactant in n-pentanol n-pentanol bulk membrane. The extraction of bismuth ions was evaluated by the yield of extraction. The experimental parameters were evaluated and were optimized. They included the ratio of di(2-ethylhexyl)phosphoric acid concentration to the concentration of /Triton X-100 concentration (1.0 : 0.5% w/w), nature of diluents (n-pentanol), nature and concentration of the stripping solution (sulfuric acid, 0.5M), stirring speed (1,800 rpm) and equilibrium time of extraction (20min), initial feed solution of bismuth (350 ppm) and the volume ratio of the internal stripping phase to the membrane phase (14 times). The experimental parameters of kinetic extraction revealed that the bismuth ions were extracted at 100% 97%

  3. Emulsion liquid membrane for selective extraction of bismuth from nitrate medium

    Energy Technology Data Exchange (ETDEWEB)

    Mokhtari, Bahram; Pourabdollah, Kobra [Islamic Azad University, Shahreza (Iran, Islamic Republic of)

    2013-07-15

    The novelty of this work is the selective extraction of bismuth ions from nitrate medium by emulsion liquid membrane. Di(2-ethylhexyl)phosphoric acid was used as extractant of bismuth ions from nitrate medium by emulsion liquid membrane, and Triton X-100 was used as the biodegradable surfactant in n-pentanol n-pentanol bulk membrane. The extraction of bismuth ions was evaluated by the yield of extraction. The experimental parameters were evaluated and were optimized. They included the ratio of di(2-ethylhexyl)phosphoric acid concentration to the concentration of /Triton X-100 concentration (1.0 : 0.5% w/w), nature of diluents (n-pentanol), nature and concentration of the stripping solution (sulfuric acid, 0.5M), stirring speed (1,800 rpm) and equilibrium time of extraction (20min), initial feed solution of bismuth (350 ppm) and the volume ratio of the internal stripping phase to the membrane phase (14 times). The experimental parameters of kinetic extraction revealed that the bismuth ions were extracted at 100% 97%.

  4. Metabolite Extraction from Saccharomyces cerevisiae for Liquid Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Rosebrock, Adam P; Caudy, Amy A

    2017-09-01

    Prior to mass spectrometric analysis, cellular small molecules must be extracted and separated from interfering components such as salts and culture medium. To ensure minimal perturbation of metabolism, yeast cells grown in liquid culture are rapidly harvested by filtration as described here. Simultaneous quenching of metabolism and extraction is afforded by immediate immersion in low-temperature organic solvent. Samples prepared using this method are suitable for a range of downstream liquid chromatography-mass spectrometry analyses and are stable in solvent for >1 yr at -80°C. © 2017 Cold Spring Harbor Laboratory Press.

  5. 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.

  6. Measuring Black men's police-based discrimination experiences: Development and validation of the Police and Law Enforcement (PLE) Scale.

    Science.gov (United States)

    English, Devin; Bowleg, Lisa; Del Río-González, Ana Maria; Tschann, Jeanne M; Agans, Robert P; Malebranche, David J

    2017-04-01

    Although social science research has examined police and law enforcement-perpetrated discrimination against Black men using policing statistics and implicit bias studies, there is little quantitative evidence detailing this phenomenon from the perspective of Black men. Consequently, there is a dearth of research detailing how Black men's perspectives on police and law enforcement-related stress predict negative physiological and psychological health outcomes. This study addresses these gaps with the qualitative development and quantitative test of the Police and Law Enforcement (PLE) Scale. In Study 1, we used thematic analysis on transcripts of individual qualitative interviews with 90 Black men to assess key themes and concepts and develop quantitative items. In Study 2, we used 2 focus groups comprised of 5 Black men each (n = 10), intensive cognitive interviewing with a separate sample of Black men (n = 15), and piloting with another sample of Black men (n = 13) to assess the ecological validity of the quantitative items. For Study 3, we analyzed data from a sample of 633 Black men between the ages of 18 and 65 to test the factor structure of the PLE, as we all as its concurrent validity and convergent/discriminant validity. Qualitative analyses and confirmatory factor analyses suggested that a 5-item, 1-factor measure appropriately represented respondents' experiences of police/law enforcement discrimination. As hypothesized, the PLE was positively associated with measures of racial discrimination and depressive symptoms. Preliminary evidence suggests that the PLE is a reliable and valid measure of Black men's experiences of discrimination with police/law enforcement. (PsycINFO Database Record (c) 2017 APA, all rights reserved).

  7. Quaternary ammonium based task specific ionic liquid for the efficient and selective extraction of neptunium

    Energy Technology Data Exchange (ETDEWEB)

    Gupta, Nishesh Kumar [National Institute of Technology, Odisha (India). Dept. of Chemistry; Sengupta, Arijit [Bhabha Atomic Research Centre, Mumbai (India). Radiochemistry Div.; Biswas, Sujoy [Bhabha Atomic Research Centre, Mumbai (India). Uranium Extraction Div.

    2017-07-01

    Liquid-liquid extraction of neptunium from aqueous acidic solution using quaternary ammonium based task specific ionic liquid (TSIL) was investigated. The extraction of Np was predominated by the 'cation exchange' mechanism via [NpO{sub 2}.Hpth]{sup +} species for NpO{sub 2}{sup 2+}, while NpO{sub 2}{sup +} was extracted in ionic liquid as [NpO{sub 2}.H.Hpth]{sup +}. The extraction process was thermodynamically spontaneous while kinetically slower. Na{sub 2}CO{sub 3} as strippant showed quantitative back extraction of neptunium ions from TSIL. TSIL showed excellent radiolytic stability upto 500 kGy gamma exposure. Finally, the TSIL was employed for the processing of simulated high level waste solutions revealing high selectivity of TSIL towards neptunium.

  8. Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction of herbicides in peanuts.

    Science.gov (United States)

    Li, Na; Wang, Zhibing; Zhang, Liyuan; Nian, Li; Lei, Lei; Yang, Xiao; Zhang, Hanqi; Yu, Aimin

    2014-10-01

    Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction was developed and applied to the extraction of pesticides in high fatty matrices. The herbicides were ultrasonically extracted from peanut using ethyl acetate as extraction solvent. The separation of the analytes from a large amount of co-extractive fat was achieved by dispersive solid-phase extraction using MIL-101(Cr) as sorbent. In this step, the analytes were adsorbed on MIL-101(Cr) and the fat remained in bulk. The herbicides were separated and determined by high-performance liquid chromatography. The experimental parameters, including type and volume of extraction solvent, ultrasonication time, volume of hexane and eluting solvent, amount of MIL-101(Cr) and dispersive solid phase extraction time, were optimized. The limits of detection for herbicides range from 0.98 to 1.9 μg/kg. The recoveries of the herbicides are in the range of 89.5-102.7% and relative standard deviations are equal or lower than 7.0%. The proposed method is simple, effective and suitable for treatment of the samples containing high content of fat. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Liquid-liquid extraction of uranium (VI) using Cyanex 272 in kerosene from sodium salicylate medium

    International Nuclear Information System (INIS)

    Kamble, Pravin N.; Mohite, Baburao S.; Suryavanshi, Vishal J.; Salunkhe, Suresh T.

    2015-01-01

    Liquid-liquid extraction of uranium (VI) from sodium salicylate media using Cyanex 272 in kerosene has been carried out. Uranium (VI) was quantitatively extracted from 1x10 -4 M sodium salicylate with 5x10 -4 M Cyanex 272 in kerosene. It was stripped quantitatively from the organic phase with 4M HCl and determined spectrophotometrically with arsenazo(III) at 600 nm. The effects of concentrations of sodium salicylate, metal ions and strippants have been studied. Separation of uranium (VI) from other elements was achieved from binary as well as from multicomponent mixtures. The method is simple, rapid and selective with good reproducibility (approximately ±2%). (author)

  10. Personalised Peer-Supported Learning: The Peer-to-Peer Learning Environment (P2PLE)

    Science.gov (United States)

    Corneli, Joseph; Mikroyannidis, Alexander

    2011-01-01

    The Peer-to-Peer Learning Environment (P2PLE) is a proposed approach to helping learners co-construct their learning environment using recommendations about people, content, and tools. The work draws on current research on PLEs, and participant observation at the Peer-to-Peer University (P2PU). We are particularly interested in ways of eliciting…

  11. Interoperability Issues for Formal Authoring Processes, Community Efforts, and the Creation of Mashup PLE

    NARCIS (Netherlands)

    Klemke, Roland; Schmitz, Birgit

    2009-01-01

    Klemke, R., & Schmitz, B. (2009). Interoperability Issues for Formal Authoring Processes, Community Efforts, and the Creation of Mashup PLE. In F. Wild, M. Kalz, M. Palmér & D. Müller (Eds.), Proceedings of 2nd Workshop Mash-Up Personal Learning Environments (MUPPLE'09). Workshop in conjunction with

  12. Measuring Black Men’s Police-Based Discrimination Experiences: Development and Validation of the Police and Law Enforcement (PLE) Scale

    Science.gov (United States)

    English, Devin; Bowleg, Lisa; del Río-González, Ana Maria; Tschann, Jeanne M.; Agans, Robert; Malebranche, David J

    2017-01-01

    Objectives Although social science research has examined police and law enforcement-perpetrated discrimination against Black men using policing statistics and implicit bias studies, there is little quantitative evidence detailing this phenomenon from the perspective of Black men. Consequently, there is a dearth of research detailing how Black men’s perspectives on police and law enforcement-related stress predict negative physiological and psychological health outcomes. This study addresses these gaps with the qualitative development and quantitative test of the Police and Law Enforcement (PLE) scale. Methods In Study 1, we employed thematic analysis on transcripts of individual qualitative interviews with 90 Black men to assess key themes and concepts and develop quantitative items. In Study 2, we used 2 focus groups comprised of 5 Black men each (n=10), intensive cognitive interviewing with a separate sample of Black men (n=15), and piloting with another sample of Black men (n=13) to assess the ecological validity of the quantitative items. For study 3, we analyzed data from a sample of 633 Black men between the ages of 18 and 65 to test the factor structure of the PLE, as we all as its concurrent validity and convergent/discriminant validity. Results Qualitative analyses and confirmatory factor analyses suggested that a 5-item, 1-factor measure appropriately represented respondents’ experiences of police/law enforcement discrimination. As hypothesized, the PLE was positively associated with measures of racial discrimination and depressive symptoms. Conclusions Preliminary evidence suggests that the PLE is a reliable and valid measure of Black men’s experiences of discrimination with police/law enforcement. PMID:28080104

  13. Solvent Extraction: Structure of the Liquid-Liquid Interface Containing a Diamide Ligand

    Energy Technology Data Exchange (ETDEWEB)

    Scoppola, Ernesto [Institut Laue-Langevin, 38000 Grenoble France; Institut de Chimie Séparative de Marcoule, UMR 5257 CEA/CNRS/ENSCM/Université Montpellier, 30207 Bagnols-sur-Cèze France; Watkins, Erik B. [Institut Laue-Langevin, 38000 Grenoble France; Materials Synthesis and Integrated Devices, Los Alamos National Laboratory, Los Alamos NM 87545 USA; Campbell, Richard A. [Institut Laue-Langevin, 38000 Grenoble France; Konovalov, Oleg [European Synchrotron Radiation Facility, 38430 Grenoble France; Girard, Luc [Institut de Chimie Séparative de Marcoule, UMR 5257 CEA/CNRS/ENSCM/Université Montpellier, 30207 Bagnols-sur-Cèze France; Dufrêche, Jean-Francois [Institut de Chimie Séparative de Marcoule, UMR 5257 CEA/CNRS/ENSCM/Université Montpellier, 30207 Bagnols-sur-Cèze France; Ferru, Geoffroy [Argonne National Labororatory, Lemont IL 60439 USA; Fragneto, Giovanna [Institut Laue-Langevin, 38000 Grenoble France; Diat, Olivier [Institut de Chimie Séparative de Marcoule, UMR 5257 CEA/CNRS/ENSCM/Université Montpellier, 30207 Bagnols-sur-Cèze France

    2016-06-20

    Knowledge of the (supra)molecular structure of an interface that contains amphiphilic ligand molecules is necessary for a full understanding of ion transfer during solvent extraction. Even if molecular dynamics already yield some insight in the molecular configurations in solution, hardly any experimental data giving access to distributions of both extractant molecules and ions at the liquid–liquid interface exist. Here, the combined application of X-ray and neutron reflectivity measurements represents a key milestone in the deduction of the interfacial structure and potential with respect to two different lipophilic ligands. Indeed, we show for the first time that hard trivalent cations can be repelled or attracted by the extractant-enriched interface according to the nature of the ligand.

  14. Double-blind, Placebo-controlled Trial to Evaluate the Effectiveness of Polypodium Leucotomos Extract in the Treatment of Melasma in Asian Skin: A Pilot Study.

    Science.gov (United States)

    Goh, Chee-Leok; Chuah, Sai Yee; Tien, Steven; Thng, Guan; Vitale, María Alejandra; Delgado-Rubin, Arancha

    2018-03-01

    Introduction: Melasma is a common pigmentary disorder with a multifactorial etiology that can hinder its management. The aqueous extract of the fern Polypodium leucotomos (PLE), Fernblock ® (IFC, Madrid, Spain), has demonstrated antioxidant and photoprotective activities and has been used for the treatment of several pigmentary disorders. The aim of this study was to evaluate the efficacy and safety of oral PLE in the treatment of melasma in Asian patients. Methods: Forty healthy adult patients with clinical diagnoses of melasma who were receiving treatment with topical 4% hydroquinone cream and sunscreen with a sun protection factor (SPF) of 50+ were recruited for inclusion in this study from the National Skin Centre in Singapore. They were randomized to receive either oral PLE supplementation or placebo for 12 weeks. Patients were assessed at baseline, Day 28, Day 56, and Day 84 using the modified Melasma Area and Severity Index (mMASI); melanin and erythema indexes; VISIA ® photography (Canfield Scientific, Parsippany, New Jersey, USA); and the Melasma Quality of Life (MelasQoL) questionnaire. Adverse events were recorded. Results: Following four, eight, and 12 weeks of treatment, there were statistically significant differences between the mMASI scores of both groups as compared with the baseline scores ( p ≤0.01). mMASI scores of the PLE group at eight and 12 weeks were also significantly lower than those of the placebo group ( p ≤0.05). At the end of the study, a significant improvement was reached in both groups (both p ≤0.01), with no significant differences between them. The scores of the melanin and erythema indices displayed a slight improvement in both groups, without significant differences among them. MelasQoL score showed an improvement in the PLE group versus the placebo group. Our results demonstrate that the PLE aqueous extract product significantly improves and accelerates the outcome reached with hydroquinone and sunscreen almost from

  15. Ionic liquid-based microwave-assisted extraction of flavonoids from Bauhinia championii (Benth.) Benth.

    Science.gov (United States)

    Xu, Wei; Chu, Kedan; Li, Huang; Zhang, Yuqin; Zheng, Haiyin; Chen, Ruilan; Chen, Lidian

    2012-12-03

    An ionic liquids (IL)-based microwave-assisted approach for extraction and determination of flavonoids from Bauhinia championii (Benth.) Benth. was proposed for the first time. Several ILs with different cations and anions and the microwave-assisted extraction (MAE) conditions, including sample particle size, extraction time and liquid-solid ratio, were investigated. Two M 1-butyl-3-methylimidazolium bromide ([bmim] Br) solution with 0.80 M HCl was selected as the optimal solvent. Meanwhile the optimized conditions a ratio of liquid to material of 30:1, and the extraction for 10 min at 70 °C. Compared with conventional heat-reflux extraction (CHRE) and the regular MAE, IL-MAE exhibited a higher extraction yield and shorter extraction time (from 1.5 h to 10 min). The optimized extraction samples were analysed by LC-MS/MS. IL extracts of Bauhinia championii (Benth.)Benth consisted mainly of flavonoids, among which myricetin, quercetin and kaempferol, β-sitosterol, triacontane and hexacontane were identified. The study indicated that IL-MAE was an efficient and rapid method with simple sample preparation. LC-MS/MS was also used to determine the chemical composition of the ethyl acetate/MAE extract of Bauhinia championii (Benth.) Benth, and it maybe become a rapid method to determine the composition of new plant extracts.

  16. Ionic-Liquid-Mediated Extraction and Separation Processes for Bioactive Compounds: Past, Present, and Future Trends.

    Science.gov (United States)

    Ventura, Sónia P M; E Silva, Francisca A; Quental, Maria V; Mondal, Dibyendu; Freire, Mara G; Coutinho, João A P

    2017-05-24

    Ionic liquids (ILs) have been proposed as promising media for the extraction and separation of bioactive compounds from the most diverse origins. This critical review offers a compilation on the main results achieved by the use of ionic-liquid-based processes in the extraction and separation/purification of a large range of bioactive compounds (including small organic extractable compounds from biomass, lipids, and other hydrophobic compounds, proteins, amino acids, nucleic acids, and pharmaceuticals). ILs have been studied as solvents, cosolvents, cosurfactants, electrolytes, and adjuvants, as well as used in the creation of IL-supported materials for separation purposes. The IL-based processes hitherto reported, such as IL-based solid-liquid extractions, IL-based liquid-liquid extractions, IL-modified materials, and IL-based crystallization approaches, are here reviewed and compared in terms of extraction and separation performance. The key accomplishments and future challenges to the field are discussed, with particular emphasis on the major lacunas found within the IL community dedicated to separation processes and by suggesting some steps to overcome the current limitations.

  17. [Preparation and applications of a supported liquid-liquid extraction column with a composite diatomite material].

    Science.gov (United States)

    Bao, Jianmin; Ma, Zhishuang; Sun, Ying; Wang, Yongzun; Li, Youxin

    2012-08-01

    A rapid and special supported liquid-liquid extraction (SLE) column was developed with a composite diatomite material. The SLE column was evaluated by high performance liquid chromatography (HPLC) with acidic, neutral and alkaline compounds dissolved in water. Furthermore, some real complex samples were also analyzed by HPLC with the SLE method. The recoveries of benzoic acid (acidic), p-nitroaniline (alkaline) and 4-hydroxy-benzoic methyl ester (neutral) treated by the SLE column were 90.6%, 98.1% and 97.7%. However, the recoveries of the three compounds treated by traditional liquid-liquid extraction (LLE) method were 71.9%, 81.9% and 83.9%. The results showed that the SLE technique had higher recoveries than the traditional LLE method. The spiked recoveries of the complex samples, such as benzoic acid in Sprite and dexamethasone acetate, chlorphenamine maleate, indomethacin in bovine serum, were between 80% and 110% and the relative standard deviations (RSDs) were less than 15%. For biological specimen, the results could be accepted. Meantime, many disadvantages associated with traditional LLE method, such as emulsion formation, didn't occur using SLE column. The SLE column technique is a good sample preparation method with many advantages, such as rapid, simple, robust, easily automated, high recovery and high-throughput, which would be widely used in the future.

  18. Ionic liquid performance in pilot plant contactors for aromatics extraction

    NARCIS (Netherlands)

    Onink, S.A.F.

    2011-01-01

    The main objectives of this study were an investigation into the applicability, in this case extraction capacity and equipment performance, of room temperature ionic liquids as solvent in the extraction of aromatics from aliphatics and a comparison of three types of contactors (a rotating disc

  19. The status of research on CFD-PBM simulation of liquid-liquid two-phase flow in extraction columns

    International Nuclear Information System (INIS)

    Li Shaowei; Jing Shan; Wu Qiulin; Zhang Qi

    2012-01-01

    Computational fluid dynamics (CFD) simulation has gained more and more interest in the chemical engineering researchers and is becoming a useful tool for the chemical engineering research. The research on liquid-liquid two-phase flow CFD simulation in extraction columns is now in its initial stage. There is much work to do for the developing of this research field. The purpose of this article is to review the CFD simulation methods for two-phase flow in extraction column. The population balance model (PBM) is detailedly described in this article because it is the main method used in the two-phase flow CFD simulation currently. Then some examples for the two-phase flow simulation in extraction columns are briefly introduced. The strategy for the research on CFD simulation of two-phase flow in extraction columns is suggested at last. (authors)

  20. The transfer of rare earth elements through liquid extraction membranes

    International Nuclear Information System (INIS)

    Kapranchik, V.P.; Proyaev, V.V.; Kopyrin, A.A.

    1988-01-01

    The transfer of rare earth elements through liquid extraction membranes, presenting Dacron nuclear filters, impregnated by extractants of different types (tributylphosphine oxide; di-2-ethylhexylphosphoric acid, HDEHP; trioctylamine, TOA) is investigated. It is ascertained that in systems with extractant-carriers TOA and HDEHP inversion of dependences of flow values and distribution coefficients on the element atomic number is observed. Mathematical model of transfer, permitting to establish relation between extractional and transport characteristics of the membrane, is suggested

  1. Liquid-liquid extraction of beryllium (II) using Cyanex 923 in kerosene from sodium acetate medium

    International Nuclear Information System (INIS)

    Kamble, Pravin N.; Madane, Namdev S.; Mohite, Baburao S.

    2013-01-01

    Liquid-liquid extraction of beryllium(II) from sodium acetate media using cyanex 923 in kerosene has been carried out. Beryllium(II) was quantitatively extracted from 1x10 -1 M sodium acetate with 1x10 -2 M cyanex 923 in kerosene. It was stripped quantitatively from the organic phase with 1M H 2 SO 4 and determined spectrophotometrically with eriochrome cyanine R at 525 nm. The effect of concentrations of sodium acetate, metal ions and strippants have been studied. Separation of beryllium(II) from other elements was achieved from binary as well as from multicomponent mixtures. The method is simple, rapid and selective with good reproducibility (approximately±2%). (author)

  2. Anti-snake venom activities of ethanolic extract of fruits of Piper longum L. (Piperaceae) against Russell's viper venom: characterization of piperine as active principle.

    Science.gov (United States)

    Shenoy, P A; Nipate, S S; Sonpetkar, J M; Salvi, N C; Waghmare, A B; Chaudhari, P D

    2013-05-20

    Piper longum L. fruits have been traditionally used against snakebites in north-eastern and southern region of India. To examine the ability of ethanolic extract of fruits of Piper longum L., Piperaceae (PLE) and piperine, one of the main active principles of Piper longum, to inhibit the Russell's viper (Doboia russelii, Viperidae) snake venom activities. Anti-snake venom activities of ethanolic extract of fruits of Piper longum L. (Piperaceae) and piperine against Russell's viper venom was studied in embryonated fertile chicken eggs, mice and rats by using various models as follows: inhibition of venom lethal action, inhibition of venom haemorrhagic action (in vitro), inhibition of venom haemorrhagic action (in vivo), inhibition of venom necrotizing action, inhibition of venom defibrinogenating action, inhibition of venom induced paw edema, inhibition of venom induced mast cell degranulation, creatine kinase assay and assay for catalase activity. PLE was found to inhibit the venom induced haemorrhage in embryonated fertile chicken eggs. Administration of PLE and piperine significantly (p<0.01) inhibited venom induced lethality, haemorrhage, necrosis, defibrinogenation and inflammatory paw edema in mice in a dose dependent manner. PLE and piperine also significantly (p<0.01) reduced venom induced mast cell degranulation in rats. Venom induced decrease in catalase enzyme levels in mice kidney tissue and increase in creatine kinase enzyme levels in mice serum were significantly (p<0.01) reversed by administration of both PLE and piperine. PLE possesses good anti-snake venom properties and piperine is one of the compounds responsible for the effective venom neutralizing ability of the plant. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

  3. Aprendizaje autorregulado y PLE

    Directory of Open Access Journals (Sweden)

    María del Carmen Llorente Cejudo

    2013-01-01

    Full Text Available Mediante los medios sociales de comunicación los estudiantes amplían su horizonte informativo y formativo. Los esfuerzos de los profesores y estudiantes universitarios que incorporan conceptos y metodologías bajo denominaciones como e-learning 2.0, pedagogía 2.0, estudiante 2.0, profesor 2.0 o clase 2.0, bajo el sufijo “2.0”, se caracteriza por ser una Web social que engloba, entre otras, algunos de los siguientes términos: apertura, personalización, colaboración, redes sociales, presencial social, contenido generado por el usuario, etc. Las situaciones cambiantes de la sociedad en la que el alumnado se encuentra deben ayudar a los estudiantes a desarrollar la capacidad para una toma de decisiones inteligente y la habilidad de tomar el control y la responsabilidad de sus estudios. Como docentes, debe perseguirse que los estudiantes adquieran los conocimientos y habilidades precisas para hacer frente a sus proyectos de aprendizaje de manera intencional, de ahí el concepto de autorregulación del aprendizaje. En el presente artículo establecemos el marco pedagógico desde el cual estructurar la relación entre el aprendizaje autorregulado de los estudiantes a través de Entornos Personales de Aprendizaje (PLE, ofreciendo una experiencia propia basada en el Proyecto de Investigación bajo la denominación “Dipro 2.0”.

  4. Kinetic aspects of hollow fiber liquid-phase microextraction and electromembrane extraction

    DEFF Research Database (Denmark)

    Gjelstad, Astrid; Jensen, Henrik; Rasmussen, Knut Einar

    2012-01-01

    In this paper, extraction kinetics was investigated experimentally and theoretically in hollow fiber liquid-phase microextraction (HF-LPME) and electromembrane extraction (EME) with the basic drugs droperidol, haloperidol, nortriptyline, clomipramine, and clemastine as model analytes. In HF...

  5. Liquid-Liquid Extraction and Determination of Trace Elements in Iron Minerals by Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    Taseska, Milena; Stafilov, Trajche; Makreski, Petre; Jacimovic, Radojko; Jovanovski, Gligor

    2006-01-01

    Various trace elements (cadmium, chromium, cobalt, nickel, manganese) in some iron minerals were determined by flame (FAAS) and electrothermal atomic absorption spectrometry (ETAAS). The studied minerals were chalcopyrite (CuFeS 2 ), hematite (Fe 2 O 3 ) and pyrite (FeS 2 ). To avoid the interference of iron, a method for liquid-liquid extraction of iron and determination of investigated elements in the inorganic phase was proposed. Iron was extracted by diisopropyl ether in hydrochloride acid solution and the extraction method was optimized. Some parameters were obtained to be significantly important: Fe mass in the sample should not exceed 0.3 g, the optimal concentration of HCI should be 7.8 mol 1 -1 and ratio of the inorganic and organic phase should be 1: 1. The procedure was verified by the method of standard additions and by its applications to reference standard samples. The investigated minerals originate from various mines in the Republic of Macedonia. (Author)

  6. Synergistic effect of dicarbollide anions in liquid-liquid extraction: a molecular dynamics study at the octanol-water interface.

    Science.gov (United States)

    Chevrot, G; Schurhammer, R; Wipff, G

    2007-04-28

    We report a molecular dynamics study of chlorinated cobalt bis(dicarbollide) anions [(B(9)C(2)H(8)Cl(3))(2)Co](-)"CCD(-)" in octanol and at the octanol-water interface, with the main aim to understand why these hydrophobic species act as strong synergists in assisted liquid-liquid cation extraction. Neat octanol is quite heterogeneous and is found to display dual solvation properties, allowing to well solubilize CCD(-), Cs(+) salts in the form of diluted pairs or oligomers, without displaying aggregation. At the aqueous interface, octanol behaves as an amphiphile, forming either monolayers or bilayers, depending on the initial state and confinement conditions. In biphasic octanol-water systems, CCD(-) anions are found to mainly partition to the organic phase, thus attracting Cs(+) or even more hydrophilic counterions like Eu(3+) into that phase. The remaining CCD(-) anions adsorb at the interface, but are less surface active than at the chloroform interface. Finally, we compare the interfacial behavior of the Eu(BTP)(3)(3+) complex in the absence and in the presence of CCD(-) anions and extractant molecules. It is found that when the CCD(-)'s are concentrated enough, the complex is extracted to the octanol phase. Otherwise, it is trapped at the interface, attracted by water. These results are compared to those obtained with chloroform as organic phase and discussed in the context of synergistic effect of CCD(-) in liquid-liquid extraction, pointing to the importance of dual solvation properties of octanol and of the hydrophobic character of CCD(-) for synergistic extraction of cations.

  7. Determination of methylphenidate in Calliphorid larvae by liquid-liquid extraction and liquid chromatography mass spectrometry - Forensic entomotoxicology using an in vivo rat brain model

    DEFF Research Database (Denmark)

    Bushby, Sarah K.; Thomas, Nicky; Priemel, Petra A.

    2012-01-01

    and Calliphorid larvae) by liquid-liquid extraction with recovery of >80%, and quantified using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The LC-MS/MS assay was validated for entomotoxicological use and initially applied to male Sprague-Dawley rats (n=6) that were dosed with MPH (20mg/kg) ante...

  8. A rapid method to estimate uranium using ionic liquid as extracting agent from basic aqueous media

    International Nuclear Information System (INIS)

    Prabhath Ravi, K.; Sathyapriya, R.S.; Rao, D.D.; Ghosh, S.K.

    2016-01-01

    Room temperature ionic liquids, as their name suggests are salts with a low melting point typically less than 100 °C and exist as liquid at room temperature. The common cationic parts of ionic liquids are imidazolium, pyridinium, pyrrolidinium, quaternary ammonium, or phosphonium ions, and common anionic parts are chloride, bromide, boron tetrafluorate, phosphorous hexafluorate, triflimide etc. The physical properties of ionic liquids can be tuned by choosing appropriate cations with differing alkyl chain lengths and anions. Application of ionic liquids in organic synthesis, liquid-liquid extractions, electrochemistry, catalysis, speciation studies, nuclear reprocessing is being studied extensively in recent times. In this paper a rapid method to estimate the uranium content in aqueous media by extraction with room temperature ionic liquid tricaprylammoniumthiosalicylate ((A- 336)(TS)) followed by liquid scintillation analysis is described. Re-extraction of uranium from ionic liquid phase to aqueous phase was also studied

  9. A generalized theory of chromatography and multistep liquid extraction

    Science.gov (United States)

    Chizhkov, V. P.; Boitsov, V. N.

    2017-03-01

    A generalized theory of chromatography and multistep liquid extraction is developed. The principles of highly efficient processes for fine preparative separation of binary mixture components on a fixed sorbent layer are discussed.

  10. Some studies on extractive liquid scintillation counting for Th-234/P-234m

    International Nuclear Information System (INIS)

    Grudpan, K.; Singjanusong, P.; Punyodom, W.

    1990-01-01

    A study on solvent extraction for Th-234/Pa-234m by liquid scintillation counting has not been reported. This paper will report an application of the technique on such a study. In a hydrochloric acid solution of an uranyl salt, Pa-234m which is one of the daughters of U-238 can be separated by extraction into isobutyl methyl ketone (IBMK). Cerenkov counting was applied for the extraction investigation. Solvent extraction of Th-234/Pa-234m from an aqueous nitric acid solution by TOPO/PPO in toluene by using liquid scintillation counting will be described

  11. T his article is m ainly about using sim ple trigonom etric identities ...

    Indian Academy of Sciences (India)

    T his article is m ainly about using sim ple trigonom etric identities and basic calculus to deduce som e new and interesting series. In particular, I use basic aspects of. G am m a and B eta integrations to deduce these series. T hese lead to interesting series for ¼ or functions of ¼ . O ne form ofbeta integration w hich is often ...

  12. Malonamide, phosphine oxide and calix[4]arene functionalized ionic liquids: synthesis and extraction of actinides and lanthanides

    International Nuclear Information System (INIS)

    Ternova, Dariia

    2014-01-01

    Radioactive waste treatment is a crucial problem nowadays. This work was dedicated to the development of the new extracting systems for radionuclides on the basis of 'green' solvents Ionic Liquids (Ils). For this purpose Ils were functionalized with various extracting patterns: phosphine oxide, carbamoyl phosphine oxide groups and malonamide fragment. Also the calix[4]arene platforms were used for the synthesis of functionalized ionic liquids (Fils) and their precursors. The Fils of both types cationic and anionic have been obtained. The synthesized Fils were tested for the liquid-liquid extraction of radionuclides. lt was found that extraction well occurs due to the extracting patterns, however a charge of a modified ion influences extraction.The various extracting experiments and mathematical modelling have been performed to determine the mechanisms of extraction. These studies showed that each extracting system is characterized by a different set of extracting equilibria, based mostly on cationic exchange. (author)

  13. Uranium extraction process in a sulfuric medium by means of liquid emulsified membranes

    International Nuclear Information System (INIS)

    Monteillet, A.

    1985-02-01

    Uranium ore processing, after leaching by sulfuric acid, by liquid-liquid extraction is a rather heavy process, not suitable for small deposits. Extraction by emulsions was suggested. In this process the leachate is contacted with an oil in water type emulsion, a liquid organic membrane is formed by the continuous phase. Uranium complexes diffuse through the liquid membrane towards the dispersed aqueous phase of the emulsion (stripping solution). Uranium is recovered by breaking the emulsion. Are successively studied: development of stable emulsions, influence of emulsion composition on uranium transfer kinetics, transfer mechanisms through the membrane and modelling of kinetics data obtained in the experimental study [fr

  14. Liquid-liquid extraction/separation of platinum(IV) and rhodium(III) from acidic chloride solutions using tri-iso-octylamine

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Jin-Young, E-mail: jinlee@kigam.re.kr [Metals Recovery Department, Minerals Resources Research Division, Korea Institute of Geoscience and Mineral Resources (KIGAM), 92 Gahangno, Yuesong-gu, Daejeon 305-350 (Korea, Republic of); Rajesh Kumar, J., E-mail: rajeshkumarphd@rediffmail.com [Metals Recovery Department, Minerals Resources Research Division, Korea Institute of Geoscience and Mineral Resources (KIGAM), 92 Gahangno, Yuesong-gu, Daejeon 305-350 (Korea, Republic of); Kim, Joon-Soo; Park, Hyung-Kyu; Yoon, Ho-Sung [Metals Recovery Department, Minerals Resources Research Division, Korea Institute of Geoscience and Mineral Resources (KIGAM), 92 Gahangno, Yuesong-gu, Daejeon 305-350 (Korea, Republic of)

    2009-08-30

    Liquid-liquid extraction/separation of platinum(IV) and rhodium(III) from acidic chloride solutions was carried out using tri-iso-octylamine (Alamine 308) as an extractant diluted in kerosene. The percentage extraction of platinum(IV) and rhodium(III) increased with increase in acid concentration up to 8 mol L{sup -1}. However, at 10 mol L{sup -1} HCl concentration, the extraction behavior was reversed, indicating the solvation type mechanism during extraction. The quantitative extraction of {approx}98% platinum(IV) and 36% rhodium(III) was achieved with 0.01 mol L{sup -1} Alamine 308. The highest separation factor (S.F. = 184.7) of platinum(IV) and rhodium(III) was achieved with 0.01 mol L{sup -1} Alamine 308 at 1.0 mol L{sup -1} of hydrochloric acid concentration. Alkaline metal salts like sodium chloride, sodium nitrate, sodium thiocyanate, lithium chloride, lithium nitrate, potassium chloride and potassium thiocyanate used for the salting-out effect. LiCl proved as best salt for the extraction of platinum(IV). Temperature effect demonstrates that the extraction process is exothermic. Hydrochloric acid and thiourea mixture proved to be better stripping reagents when compared with other mineral acids and bases.

  15. Separation of {sup 195(m,g),197m}Hg from bulk gold target by liquid-liquid extraction using hydrophobic ionic liquids

    Energy Technology Data Exchange (ETDEWEB)

    Ghosh, Kaustab; Lahiri, Susanta [Saha Institute of Nuclear Physics, Kolkata (India). Chemical Sciences Div.; Maiti, Moumita [Indian Institute of Technology Roorkee, Roorkee (India). Dept. of Physics

    2017-07-01

    The {sup 195(m,g),197m}Hg radionuclides were produced in accelerator when natural Au foil was irradiated with 23 MeV protons. The no-carrier-added (NCA) Hg radioisotopes were separated from the bulk Au target by liquid-liquid extraction (LLX) employing hydrophobic RTILs 1-butyl-3-methylimidazolium hexafluorophosphate([C{sub 4}mim][PF{sub 6}]) and 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide([bmim][Tf{sub 2}N]) as extractant with HNO{sub 3} and HCl. In each case, bulk Au was extracted into the RTIL phase leaving NCA Hg-radionuclides in the aqueous phase. The RTILs were recovered by washing with 1 M K{sub 2}S{sub 2}O{sub 5} and freshly prepared 1 M FeSO{sub 4}. The reported separation methods follow green chemistry approach as it does not involve any volatile reagents.

  16. Solid-Liquid Extraction Kinetics of Total Phenolic Compounds (TPC from Red Dates

    Directory of Open Access Journals (Sweden)

    Bee Lin Chua

    2018-01-01

    Full Text Available Red dates are one of the most famous herbal plants in making traditional Chinese medicine. They contain large amount of bioactive compounds. The objectives of this research were to optimise the crude extract yield and total phenolic compounds (TPC yield from red dates using response surface methodology (RSM and model the extraction kinetics of TPC yield from red dates. Date fruits were dried in an oven under temperatures 50°C, 60°C, 70°C and 80°C until a constant weight was obtained. The optimum drying temperature was 60°C as it gave the highest crude extract yield and TPC yield. Besides that, single factor experiments were used to determine the optimum range of four extraction parameters which were: liquid-solid ratio (10-30 ml/g; ultrasonic power (70-90%; extraction temperature (50-70°C; and extraction time (40-60min. The optimum range of the four parameters were further optimised using the Box-Behken Design (BBD of RSM. The extraction conditions that gave the highest crude extract yield and TPC yield were chosen. The optimum value for liquid-solid ratio, ultrasonic power, extraction temperature and extraction time were 30ml/g, 70%, 60°C and 60 min respectively. The two equations generated from RSM were reliable and can be used to predict the crude extract yield and TPC yield. The higher the extraction temperature, liquid-solid ratio, and extraction time and lower ultrasonic power, the higher the crude extract and TPC yield. Finally, the results of TPC yield versus time based on the optimum extraction parameters from RSM optimisation were fitted into three extraction kinetic models (Peleg’s model, Page’s model and Ponomaryov’s model. It was found that the most suitable kinetic model to represent the extraction process of TPC from red dates was Page’s model due to its coefficient of determination (R2 was the closest to unity, 0.9663 while its root mean square error (RMSE was the closest to zero, 0.001534.

  17. Liquid–liquid extraction of Pu(IV), U(VI) and Am(III) using malonamide in room temperature ionic liquid as diluent

    International Nuclear Information System (INIS)

    Rout, Alok; Venkatesan, K.A.; Srinivasan, T.G.; Vasudeva Rao, P.R.

    2012-01-01

    Highlights: ► Extraction of actinides using malonamide in room temperature ionic liquid. ► High distribution ratios of actinides in room temperature ionic liquid. ► Ion exchange mechanism. ► Stoichiometry of extraction. ► High separation factors of U(VI) and Pu(IV) over Am(III) and fission products. - Abstract: The extraction behavior of U(VI), Pu(IV) and Am(III) from nitric acid medium by a solution of N,N-dimethyl-N,N-dioctyl-2-(2-hexyloxyethyl)malonamide (DMDOHEMA) in the room temperature ionic liquid, 1–butyl–3–methylimidazolium bis(trifluoromethanesulfonyl)imide (C 4 mimNTf 2 ), was studied. The distribution ratio of these actinides in DMDOHEMA/C 4 mimNTf 2 was measured as a function of various parameters such as the concentration of nitric acid, DMDOHEMA, NTf 2 − , alkyl chain length of ionic liquid. The extraction of actinides in the absence of DMDOHEMA was insignificant and the distribution ratio achieved in conjunction with C 4 mimNTf 2 , was remarkable. The separation factor of U(VI) and Pu(IV) achieved with the use of DMDOHEMA, ionic liquid was compared with Am(III) and other fission products. The stoichiometry of the metal-solvate was determined to be 1:2 for U(VI) and Pu(IV) and 1:3 for Am(III).

  18. Screening of commercial and pecan shell-extracted liquid smoke agents as natural antimicrobials against foodborne pathogens.

    Science.gov (United States)

    Van Loo, Ellen J; Babu, D; Crandall, Philip G; Ricke, Steven C

    2012-06-01

    Liquid smoke extracts have traditionally been used as flavoring agents, are known to possess antioxidant properties, and serve as natural alternatives to conventional antimicrobials. The antimicrobial efficacies of commercial liquid smoke samples may vary depending on their source and composition and the methods used to extract and concentrate the smoke. We investigated the MICs of eight commercial liquid smoke samples against Salmonella Enteritidis, Staphylococcus aureus, and Escherichia coli . The commercial liquid smoke samples purchased were supplied by the manufacturer as water-based or concentrated extracts of smoke from different wood sources. The MICs of the commercial smokes to inhibit the growth of foodborne pathogens ranged from 0.5 to 6.0% for E. coli, 0.5 to 8.0% for Salmonella, and 0.38 to 6% for S. aureus. The MIC for each liquid smoke sample was similar in its effect on both E. coli and Salmonella. Solvent-extracted antimicrobials prepared using pecan shells displayed significant differences between their inhibitory concentrations depending on the type of solvent used for extraction. The results indicated that the liquid smoke samples tested in this study could serve as effective natural antimicrobials and that their inhibitory effects depended more on the solvents used for extraction than the wood source.

  19. Ionic liquids as alternative solvents for aromatics extraction

    NARCIS (Netherlands)

    Hansmeier, A.R.

    2010-01-01

    The objective of this thesis was the development of an extraction process for the removal of multiple aromatics from several petrochemical streams by means of an ionic liquid. Due to environmental legislation, the demand of ‘clean’ fuels is increasing and most likely will increase even more towards

  20. Aprendizaje en comunidades virtuales que emergen de los entornos personales de aprendizaje (ple)

    OpenAIRE

    Jara Roa, Dunia Inés

    2015-01-01

    El objetivo de la presente investigación es analizar los niveles de aprendizaje de los(as) estudiantes de una institución privada de educación superior, en cinco Comunidades Virtuales de Aprendizaje (CVA) que se integran de las redes sociales utilizadas en los PLE, lo que permitirá identificar qué potencialidades didácticas han sido utilizadas para la construcción del conocimiento.

  1. The DivJ, CbrA and PleC system controls DivK phosphorylation and symbiosis in Sinorhizobium meliloti

    Science.gov (United States)

    Pini, Francesco; Frage, Benjamin; Ferri, Lorenzo; De Nisco, Nicole J.; Mohapatra, Saswat S.; Taddei, Lucilla; Fioravanti, Antonella; Dewitte, Frederique; Galardini, Marco; Brilli, Matteo; Villeret, Vincent; Bazzicalupo, Marco; Mengoni, Alessio; Walker, Graham C.; Becker, Anke; Biondi, Emanuele G.

    2013-01-01

    SUMMARY Sinorhizobium meliloti is a soil bacterium that invades the root nodules it induces on Medicago sativa, whereupon it undergoes an alteration of its cell cycle and differentiates into nitrogen-fixing, elongated and polyploid bacteroid with higher membrane permeability. In Caulobacter crescentus, a related alphaproteobacterium, the principal cell cycle regulator, CtrA, is inhibited by the phosphorylated response regulator DivK. The phosphorylation of DivK depends on the histidine kinase DivJ, while PleC is the principal phosphatase for DivK. Despite the importance of the DivJ in C. crescentus, the mechanistic role of this kinase has never been elucidated in other Alphaproteobacteria. We show here that the histidine kinases DivJ together with CbrA and PleC participate in a complex phosphorylation system of the essential response regulator DivK in S. meliloti. In particular, DivJ and CbrA are involved in DivK phosphorylation and in turn CtrA inactivation, thereby controlling correct cell cycle progression and the integrity of the cell envelope. In contrast, the essential PleC presumably acts as a phosphatase of DivK. Interestingly, we found that a DivJ mutant is able to elicit nodules and enter plant cells, but fails to establish an effective symbiosis suggesting that proper envelope and/or low CtrA levels are required for symbiosis. PMID:23909720

  2. Aluminium sensitized spectrofluorimetric determination of fluoroquinolones in milk samples coupled with salting-out assisted liquid-liquid ultrasonic extraction

    Science.gov (United States)

    Xia, Qinghai; Yang, Yaling; Liu, Mousheng

    2012-10-01

    An aluminium sensitized spectrofluorimetric method coupled with salting-out assisted liquid-liquid ultrasonic extraction for the determination of four widely used fluoroquinolones (FQs) namely norfloxacin (NOR), ofloxacin (OFL), ciprofloxacin (CIP) and gatifloxacin (GAT) in bovine raw milk was described. The analytical procedure involves the fluorescence sensitization of aluminium (Al3+) by complexation with FQs, salting-out assisted liquid-liquid ultrasonic extraction (SALLUE), followed by spectrofluorometry. The influence of several parameters on the extraction (the salt species, the amount of salt, pH, temperature and phase volume ratio) was investigated. Under optimized experimental conditions, the detection limits of the method in milk varied from 0.009 μg/mL for NOR to 0.016 μg/mL for GAT (signal-to-noise ratio (S/N) = 3). The relative standard deviations (RSD) values were found to be relatively low (0.54-2.48% for four compounds). The calibration graph was linear from 0.015 to 2.25 μg/mL with coefficient of determinations not less than 0.9974. The methodology developed was applied to the determination of FQs in bovine raw milk samples. The main advantage of this method is simple, accurate and green. The method showed promising applications for analyzing polar analytes especially polar drugs in various sample matrices.

  3. 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)

  4. Liquid-liquid extraction and separation of VIII group elements, especially ruthenium, by synergic combinations or aromatic polyimines and micellar cationic exchangers

    International Nuclear Information System (INIS)

    Vitart, X.

    1991-01-01

    This thesis aims to characterize and to quantify the chemical equilibria involved in d-elements liquid-liquid extraction systems, especially elements belonging to the VIII group (Fe, Ni, Co, Ru, Rh, Pd, Pt). These systems are composed of synergic combination of aromatic polyimines and micellar cationic exchangers. Substitutions are first performed in aqueous acidic media by aromatic polyimines; then extractions are operated using micellic canionic exchangers. Chemical equilibria, selectivity effects, especially those due to ion-pair formations, kinetics, extractant behaviour are analysed and quantified [fr

  5. Liquid-liquid extraction of U(VI), Np(V) et Th(IV) ions by two calix[4]arene carboxyls, and effect of Na+ and K+ alkaline ions

    International Nuclear Information System (INIS)

    Montavon, Gilles

    1996-01-01

    As the process mainly used for the reprocessing of nuclear wastes was the Purex process, this research thesis first presents this process and outlines that it allows the residual fissile matter to be recovered and reused for the fabrication of new fuel elements, but is neither efficient nor safe enough to separate fission and activation products. Thus, this thesis reports the study of extraction and selectivity properties of two compounds derived from the p-tert-butyl-calix[4]arene with respect to actinide ions such as Th(IV), U(VI) and Np(VI). The liquid-liquid extraction technique has been used with chloroform and 1,2-dichloroethane as solvents. After some generalities on actinides, calixarenes and the liquid-liquid extraction technique, and a presentation of the experimental method, the author reports and discusses the extractive properties of the studied calixarenes with respect to Na + and K + ions. Structural studies by proton NMR have been performed. He reports and discusses the liquid-liquid extraction on actinide ions when they are alone or in presence on Na + and K + alkaline ions [fr

  6. Quantification of active principles and pigments in leaf extracts of Isatis tinctoria by HPLC/UV/MS.

    Science.gov (United States)

    Mohn, Tobias; Potterat, Olivier; Hamburger, Matthias

    2007-02-01

    An HPLC method has been developed and validated for the quantification of the pharmacologically active principles tryptanthrin (1), 1,3-dihydro-3-[(4-hydroxy-3,5-dimethoxyphenyl)methylene]-2 H-indol-2-one (indolinone) (3), indirubin (4), alpha-linolenic acid (2), and indigo (5), an isomer of indirubin, in extracts from the traditional anti-inflammatory plant Isatis tinctoria (woad). The chromatographic separation was performed on a C-18 column with a linear gradient of acetonitrile in water containing 0.1% formic acid. The method combines UV and electrospray MS detection in the positive ion mode for the detection of the alkaloids, with a switch to the negative mode for the analysis of alpha-linolenic acid. The method was applied to the analysis of woad extracts obtained by supercritical fluid (SFE) CO2 extraction, and by pressurized liquid extraction (PLE) with dichloromethane and methanol, respectively. While the highest concentration of alpha-linolenic acid was found in the SFE extract (7.43%), the concentrations of tryptanthrin , indolinone, indirubin and indigo were the highest in the dichloromethane extract (0.30, 0.035, 2.48 and 0.84%, respectively). Compound 3 was not detected in the methanolic extract and only traces of compounds 1, 4 and 5 and low amount of alpha-linolenic acid (0.39%) were present in this extract.

  7. Studies on the liquid-liquid phase distribution equilibria of selenium and its measurement in water using extraction plant with a pulsation column

    International Nuclear Information System (INIS)

    Iskanderani, F.; Sobhi, K.M.; Ejaz, M.

    1989-01-01

    Normal heptane, xylene and a 0.01 molar solution of 4-(5-nonyl)pyridine in toluene were investigated as extractants for selenium(IV) from nitric acid media in potassium iodide. Various parameters affecting the distribution of the element are investigated. Extraction at high aqueous to organic phase volume ratio was studied, using a liquid-liquid extraction plant with a pulsation column. The results were employed to measure selenium in spiked water samples. (author) 24 refs.; 8 figs

  8. Aromatics extraction from pyrolytic sugars using ionic liquid to enhance sugar fermentability

    NARCIS (Netherlands)

    Li, X.; Luque-Moreno, L.C.; Oudenhoven, Stijn; Rehmann, L.; Kersten, Sascha R.A.; Schuur, Boelo

    2016-01-01

    Fermentative bioethanol production from pyrolytic sugars was improved via aromatics removal by liquid–liquid extraction. As solvents, the ionic liquid (IL) trihexyltetradecylphosphonium dicyanamide (P666,14[N(CN)2]) and ethyl acetate (EA) were compared. Two pyrolytic sugar solutions were created

  9. Extraction of three bioactive diterpenoids from Andrographis paniculata: effect of the extraction techniques on extract composition and quantification of three andrographolides using high-performance liquid chromatography.

    Science.gov (United States)

    Kumar, Satyanshu; Dhanani, Tushar; Shah, Sonal

    2014-10-01

    Andrographis paniculata (Burm.f.) wall.ex Nees (Acanthaceae) or Kalmegh is an important medicinal plant finding uses in many Ayurvedic formulations. Diterpenoid compounds andrographolides (APs) are the main bioactive phytochemicals present in leaves and herbage of A. paniculata. The efficiency of supercritical fluid extraction (SFE) using carbon dioxide was compared with the solid-liquid extraction techniques such as solvent extraction, ultrasound-assisted solvent extraction and microwave-assisted solvent extraction with methanol, water and methanol-water as solvents. Also a rapid and validated reverse-phase high-performance liquid chromatography-diode array detection method was developed for the simultaneous determination of the three biologically active compounds, AP, neoandrographolide and andrograpanin, in the extracts of A. paniculata. Under the best SFE conditions tested for diterpenoids, which involved extraction at 60°C and 100 bar, the extractive efficiencies were 132 and 22 µg/g for AP and neoandrographolide, respectively. The modifier percentage significantly affected the extraction efficiency. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  10. Recent progress of task-specific ionic liquids in chiral resolution and extraction of biological samples and metal ions.

    Science.gov (United States)

    Wu, Datong; Cai, Pengfei; Zhao, Xiaoyong; Kong, Yong; Pan, Yuanjiang

    2018-01-01

    Ionic liquids have been functionalized for modern applications. The functional ionic liquids are also called task-specific ionic liquids. Various task-specific ionic liquids with certain groups have been constructed and exploited widely in the field of separation. To take advantage of their properties in separation science, task-specific ionic liquids are generally used in techniques such as liquid-liquid extraction, solid-phase extraction, gas chromatography, high-performance liquid chromatography, and capillary electrophoresis. This review mainly covers original research papers published in the last five years, and we will focus on task-specific ionic liquids as the chiral selectors in chiral resolution and as extractant or sensor for biological samples and metal ion purification. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Development of an analytical methodology for the determination of the antiparasitic drug toltrazuril and its two metabolites in surface water, soil and animal manure

    DEFF Research Database (Denmark)

    Olsen, Jesper; Björklund, Erland; Krogh, Kristine A

    2012-01-01

    ... with an EC 50 of 3.16 mg L ‚àí1 for toltrazuril [9]. Due to toltrazurils frequent usage ... a LC-MS/MS methodology to determine toltrazuril , toltrazuril sulfoxide and toltrazuril sulfone in ... SPE), and in agricultural soil, animal manure and sediment using pressurized liquid extraction ( PLE ). ...

  12. Molecular dynamics simulations of hydrophobous ions at the liquid-liquid interfaces: case of dicarbollide anions as synergy agents and of ionic liquids as extracting medium

    International Nuclear Information System (INIS)

    Chevrot, G.

    2008-01-01

    Based on molecular dynamics simulations, we first describe the distribution of dicarbollide salts (CCD - , Mn + ) in concentrated monophasic solutions (water, chloroform, octanol, nitrobenzene) and in the corresponding biphasic 'oil' - water solutions. We point to the importance of surface activity of the CCD - s and of their self-aggregation in water, with marked counterions effects, and we explain the synergistic effect of CCD - s in the Eu 3+ extraction by BTP ligands. In the second part of the thesis we report exploratory simulations on the extraction of Sr 2+ by 18-crown-6 to an hydrophobic ionic liquid ([BMI][PF6]), focusing on the liquid - liquid interface. Analogies and differences with a classical aqueous interface are outlined. (author)

  13. Screening and quantitative determination of twelve acidic and neutral pharmaceuticals in whole blood by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Simonsen, Kirsten Wiese; Steentoft, Anni; Buck, Maike

    2010-01-01

    . The method was fully validated for salicylic acid, paracetamol, phenobarbital, carisoprodol, meprobamate, topiramate, etodolac, chlorzoxazone, furosemide, ibuprofen, warfarin, and salicylamide. The method also tentatively includes thiopental, theophylline, piroxicam, naproxen, diclophenac, and modafinil......We describe a multi-method for simultaneous identification and quantification of 12 acidic and neutral compounds in whole blood. The method involves a simple liquid-liquid extraction, and the identification and quantification are performed using liquid chromatography-tandem mass spectrometry...

  14. Simple and Rapid Dual-Dispersive Liquid-Liquid Microextraction as an Innovative Extraction Method for Uranium in Real Water Samples Prior to the Determination of Uranium by a Spectrophotometric Technique.

    Science.gov (United States)

    Khan, Naeemullah; Tuzen, Mustafa; Kazi, Tasneem Gul

    2017-11-01

    An innovative, rapid, and simple dual-dispersive liquid-liquid microextraction (DDLL-ME) approach was used to extract uranium from real samples for the first time. The main objective of this study was to disperse extraction solvent by using an air-agitated syringe system to overcome matrix effects and avoid dispersion of hazardous dispersive organic solvents by using heat. The DDLL-ME method consisted of two dispersive liquid-liquid extraction steps with chloroform as the extracting solvent. Uranium formed complexes with 4-(2-thiazolylazo) resorcinol in the aqueous phase and was extracted in extracting solvent (chloroform) after the first dispersive liquid-liquid process. Uranium was then back-extracted in the acidic aqueous phase in a second dispersive liquid-liquid process. Finally, uranium was determined by a spectrophotometric detection technique. The variables that played a key role in the proposed method were studied and optimized. The LOD and sensitivity enhancement factor for uranium were found to be 0.60 µg/L and 45, respectively, under optimized conditions. Calibration graphs were found to be linear in the range of 5.0-600 µg/L. The RSD was 2.5%. Reliability of the proposed method was verified by analyzing certified reference material TM-28.3.

  15. U(VI) extraction by 8-hydroxyquinoline. A comparison study in ionic liquid and in dichloromethane

    Energy Technology Data Exchange (ETDEWEB)

    Yuan, Li-Yong; Shi, Wei-Qun [Chinese Academy of Sciences, Beijing (China). Lab. of Nuclear Energy Chemistry; Liao, Xiang-Hong [Chinese Academy of Sciences, Beijing (China). Lab. of Nuclear Energy Chemistry; East China Institute of Technology, Nanchang (China). School of Nuclear Engineering and Geophysics; Liu, Zhi-Rong [East China Institute of Technology, Nanchang (China). School of Nuclear Engineering and Geophysics; Chai, Zhi-Fang [Chinese Academy of Sciences, Beijing (China). Lab. of Nuclear Energy Chemistry; Soochow Univ., Suzhou (China). School of Radiological and Interdisciplinary Sciences and Collaborative Innovation Center of Radiation Medicine

    2017-08-01

    Room temperature ionic liquids (RTILs) represent a recent new class of solvents with potential application in liquid/liquid extraction based nuclear fuel reprocessing due to their unique physical and chemical properties. The work herein provides a comparison of U(VI) extraction by 8-hydroxyquinoline (HOX) in a commonly used RTIL, i.e. 1-butyl-3-methylimidazolium hexafluorophosphate ([C{sub 4}mim][PF{sub 6}]) and in conventional solvent, i.e. dichloromethane (CH{sub 2}Cl{sub 2}). The effect of HOX concentration, solution acidity and nitrate ions on the extraction were discussed in detail, and the speciation analyses of the extracted U(VI) were performed. One of the main emphasis of this work is the extraction mechanism of U(VI) extracted from aqueous phase into RTILs and conventional solvent. In CH{sub 2}Cl{sub 2}, the extraction occurs through a combination of ion change and neutral complexation, and the extracted complex is proposed as UO{sub 2}(OX){sub 2}HOX. In [C{sub 4}mim][PF{sub 6}], although a cation-change mechanism as previously reported for RTILs-based system was involved, the extracted complex of UO{sub 2}(OX){sub 1.5}(HOX){sub 1.5}(PF6){sub 0.5} gave a clear indication that the usage of HOX as an acidic extractant markedly inhibited the solubility loss of [C{sub 4}mim][PF{sub 6}] during the extraction by leaching H{sup +} to aqueous phase. Moreover, the extracted U(VI) in [C{sub 4}mim][PF{sub 6}] can be easily stripped by using 0.01 M nitric acid, which provides a simple way of the ionic liquid recycling.

  16. Salting-out assisted liquid-liquid extraction coupled to ultra-high performance liquid chromatography-tandem mass spectrometry for the determination of tetracycline residues in infant foods.

    Science.gov (United States)

    Moreno-González, David; García-Campaña, Ana M

    2017-04-15

    The use of salting-out assisted liquid-liquid extraction (SALLE) combined with ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) has been evaluated for the determination of tetracyclines in infant foods based on meat and vegetables or in milk. To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized. Analytical performances of the method were satisfactory, obtaining limits of quantification lower than 0.48μgkg -1 in all cases. The precision, expressed as relative standard deviation (%, RSD) was below 11.3%. The extraction efficiency for fortified samples ranged from 89.2 to 96.8%, with RSDs lower than 7.3%. Matrix effect was evaluated for all samples studied, being lower than |21|% in all cases. In relation to the low solvent consumption, the proposed methodology could be considered rapid, cheap and environmentally friendly. Its applicability has been successfully tested in a wide range of infant foods. Copyright © 2016 Elsevier Ltd. All rights reserved.

  17. Determination of trace amount of lead in industrial and municipal effluent water samples based on dispersive liquid-liquid extraction

    International Nuclear Information System (INIS)

    Shirkhanloo, H.; Sedighi, K.; Mousavi, H. Z.

    2014-01-01

    In this study, a simple, sensitive and accurate method was developed for the determination of lead ion by combining ionic liquid dispersive liquid-liquid extraction (Il-DLL E) with flame atomic absorption spectrometry. Tetraethyl thiuram disulfide (Tetd), acetone and 1-octyl-3m ethylimidazolium hexafluorophosphate [(C 8 MIM) (PF 6 )] were used as the chelating agent, dispersive and extraction solvent, respectively. Under the optimal conditions, the calibration graph was linear in the range of 5-190 μg L -1 of lead and the detection limit was 0.8 μg L -1 with a sample volume of 200 ml. The proposed method was validated by the analysis of one certified reference material and applied successfully to the determination of lead in real water samples. (Author)

  18. Liquid chromatography-tandem mass spectrometric assay for the quantitative determination of the tyrosine kinase inhibitor quizartinib in mouse plasma using salting-out liquid-liquid extraction

    NARCIS (Netherlands)

    Retmana, Irene A; Wang, Jing; Schinkel, Alfred H; Schellens, Jan H M; Beijnen, Jos H; Sparidans, Rolf W

    2017-01-01

    A bioanalytical assay for quizartinib -a potent, and selective FLT3 tyrosine kinase inhibitor- in mouse plasma was developed and validated. Salting-out assisted liquid-liquid extraction (SALLE), using acetonitrile and magnesium sulfate, was selected as sample pretreatment with deuterated quizartinib

  19. Liquid-Liquid Extraction/Low-Temperature Purification (LLE/LTP Followed by Dispersive Solid-Phase Extraction (d-SPE Cleanup for Multiresidue Analysis in Palm Oil by LC-QTOF-MS

    Directory of Open Access Journals (Sweden)

    Elham Sobhanzadeh

    2013-01-01

    Full Text Available An evaluation of the extraction of multiresidue pesticides from palm oil by liquid-liquid extraction/low-temperature purification (LLE/LTP coupled with dispersive solid-phase extraction (d-SPE as the cleanup procedure with the determination by liquid chromatography mass spectrometry using electrospray as the ionization source (LC-ESI-MS was carried out. Optimization approaches were studied in terms of d-SPE to select efficiency of type and mass of adsorbents to obtain the highest recovery yield of pesticides and the lowest coextract fat residues in the final extract. The optimal conditions of d-SPE were obtained using 3 g of palm oil, 4 g anhydrous MgSO4, 150 mg of PSA, and 50 mg of GCB (PSA: GCB (3 : 1 w/w. Recovery study was performed at three concentration levels (25, 50, and 100 ng kg−1, yielding recovery rates between 71.8 and 112.4% except diuron with relative standard deviations of 3.2–15.1%. Detection and quantification limits were lower than 2.7 and 8.2 ng kg−1, respectively. The proposed method was successfully applied to the analysis of market-purchased palm oil samples from two different brands collected in Kuala Lumpur, showing its potential applicability and revealing the presence of some of the target species in the ng g−1 range.

  20. Caesium extraction from acidic high level liquid wastes with functionalized calixarenes

    International Nuclear Information System (INIS)

    Simon, N.; Eymard, S.; Tournois, B.; Dozol, J.F.

    2000-01-01

    In the framework of French law programme, studies are under way to selectively remove caesium from acidic high activity wastes. Calix[4]arene crown derivatives exhibit outstanding efficiency and selectivity for caesium. An optimisation of the formulation of a selective extractant system for Cs based on crown calixarenes and usable in a process which use liquid-liquid extraction is presented. A system involving a monoamide as a modifier is proposed. Besides these improvements, a reference solvent based on a standard 1,3-di-(n-octyl-oxy)2,4-calix(4)arene crown is studied. Flow-sheets related to this system are calculated and easily transferable to the optimised new system. (authors)

  1. Proof of concept for continuous enantioselective liquid-liquid extraction in capillary microreactors using 1-octanol as a sustainable solvent

    NARCIS (Netherlands)

    Susanti, S.; Meinds, Tim G.; Pinxterhuis, Erik B.; Schuur, Boelo; De Vries, Johannes G.; Feringa, Ben L.; Winkelman, Jozef G.M.; Yue, Jun; Heeres, Hero J.

    2017-01-01

    The use of capillary microreactors for enantioselective liquid-liquid extraction (ELLE) was successfully demonstrated using a model system consisting of a buffered aqueous amino acid derivative (3,5-dinitrobenzoyl-(R,S)-leucine) solution (phosphate buffer, pH 6.58) and a chiral cinchona alkaloid

  2. Liquid membrane extraction techniques for trace metal analysis and speciation in environmental and biological matrices

    Energy Technology Data Exchange (ETDEWEB)

    Ndungu, Kuria

    1999-04-01

    In this thesis, liquid-membrane-based methods for the analysis of trace metal species in samples of environmental and biological origin were developed. By incorporating extracting reagents in the membrane liquid, trace metal ions were selectively separated from humic-rich natural waters and urine samples, prior to their determination using various instrumental techniques. The extractions were performed in closed flow systems thus allowing easy automation of both the sample clean-up and enrichment. An acidic organophosphorus reagent (DEHPA) and a basic tetraalkylammonium reagent (Aliquat-336) were used as extractants in the membrane liquid to selectively extract and enrich cationic and anionic metal species respectively. A speciation method for chromium species was developed that allowed the determination of cationic Cr(III) species and anionic CR(VI) species in natural water samples without the need of a chromatographic separation step prior to their detection. SLM was also coupled on-line to potentiometric stripping analysis providing a fast and sensitive method for analysis of Pb in urine samples. A microporous membrane liquid-liquid extraction (MMLLE) method was developed for the determination of organotin compounds in natural waters that reduced the number of manual steps involved in the LLE of organotin compounds prior to their CC separation. Clean extracts obtained after running unfiltered humic-rich river water samples through the MMLLE flow system allowed selective determination of all the organotin compounds in a single run using GC-MS in the selected ion monitoring mode (SIM) 171 refs, 9 figs, 4 tabs

  3. Molecular dynamics simulations of hydrophobous ions at the liquid-liquid interfaces: case of dicarbollide anions as synergy agents and of ionic liquids as extracting medium; Simulations par dynamique moleculaire d'ions hydrophobes aux interfaces liquide - liquide: le cas des anions dicarbollides comme agents de synergie et celui des liquides ioniques comme milieu extractant

    Energy Technology Data Exchange (ETDEWEB)

    Chevrot, G

    2008-01-15

    Based on molecular dynamics simulations, we first describe the distribution of dicarbollide salts (CCD{sup -}, Mn{sup +}) in concentrated monophasic solutions (water, chloroform, octanol, nitrobenzene) and in the corresponding biphasic 'oil' - water solutions. We point to the importance of surface activity of the CCD{sup -}s and of their self-aggregation in water, with marked counterions effects, and we explain the synergistic effect of CCD{sup -}s in the Eu{sup 3+} extraction by BTP ligands. In the second part of the thesis we report exploratory simulations on the extraction of Sr{sup 2+} by 18-crown-6 to an hydrophobic ionic liquid ([BMI][PF6]), focusing on the liquid - liquid interface. Analogies and differences with a classical aqueous interface are outlined. (author)

  4. Fast, simple and efficient salting-out assisted liquid-liquid extraction of naringenin from fruit juice samples prior to their enantioselective determination by liquid chromatography.

    Science.gov (United States)

    Magiera, Sylwia; Kwietniowska, Ewelina

    2016-11-15

    In this study, an easy, simple and efficient method for the determination of naringenin enantiomers in fruit juices after salting-out-assisted liquid-liquid extraction (SALLE) and high-performance liquid chromatography (HPLC) with diode-array detection (DAD) was developed. The sample treatment is based on the use of water-miscible acetonitrile as the extractant and acetonitrile phase separation under high-salt conditions. After extraction, juice samples were incubated with hydrochloric acid in order to achieve hydrolysis of naringin to naringenin. The hydrolysis parameters were optimized by using a half-fraction factorial central composite design (CCD). After sample preparation, chromatographic separation was obtained on a Chiralcel® OJ-RH column using the mobile phase consisting of 10mM aqueous ammonium acetate:methanol:acetonitrile (50:30:20; v/v/v) with detection at 288nm. The average recovery of the analyzed compounds ranged from 85.6 to 97.1%. The proposed method was satisfactorily used for the determination of naringenin enantiomers in various fruit juices samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Comparison of micellar extraction combined with ionic liquid based vortex-assisted liquid-liquid microextraction and modified quick, easy, cheap, effective, rugged, and safe method for the determination of difenoconazole in cowpea.

    Science.gov (United States)

    Chen, Xiaochu; Bian, Yanli; Liu, Fengmao; Teng, Peipei; Sun, Pan

    2017-10-06

    Two simple sample pretreatment for the determination of difenoconazole in cowpea was developed including micellar extraction combined with ionic liquid based vortex-assisted liquid-liquid microextraction (ME-IL-VALLME) prior to high performance liquid chromatography (HPLC), and modified quick, easy, cheap, effective, rugged, and safe method (QuEChERS) coupled with HPLC-MS/MS. In ME-IL-VALLME method, the target analyte was extracted by surfactant Tween 20 micellar solution, then the supernatant was diluted with 3mL water to decrease the solubility of micellar solution. Subsequently, the vortex-assisted liquid-liquid microextraction (VALLME) procedure was performed in the diluted extraction solution by using the ionic liquid of 1-hexyl-3-methylimidazolium hexafluorophosphate ([HMIM]PF 6 ) as the extraction solvent and Tween 20 as an emulsifier to enhance the dispersion of the water-immiscible ionic liquid into the aqueous phase. Parameters that affect the extraction have been investigated in both methods Under the optimum conditions, the limits of quantitation were 0.10 and 0.05mgkg -1 , respectively. And good linearity was achieved with the correlation coefficient higher than 0.9941. The relative recoveries ranged from 78.6 to 94.8% and 92.0 to 118.0% with the relative standard deviations (RSD) of 7.9-9.6% and 1.2-3.2%, respectively. Both methods were quick, simple and inexpensive. However, the ME-IL-VALLME method provides higher enrichment factor compared with conventional QuEChERS method. The ME-IL-VALLME method has a strong potential for the determination of difenoconazole in complex vegetable matrices with HPLC. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Parallel artificial liquid membrane extraction of new psychoactive substances in plasma and whole blood

    DEFF Research Database (Denmark)

    Vårdal, Linda; Askildsen, Hilde-Merete; Gjelstad, Astrid

    2017-01-01

    Parallel artificial liquid membrane extraction (PALME) was combined with ultra-high performance liquid chromatography-mass spectrometry (UHPLC–MS) and the potential for screening of new psychoactive substances (NPS) was investigated for the first time. PALME was performed in 96-well format...... comprising a donor plate, a supported liquid membrane (SLM), and an acceptor plate. Uncharged NPS were extracted from plasma or whole blood, across an organic SLM, and into an aqueous acceptor solution, facilitated by a pH gradient. MDAI (5,6-methylenedioxy-2-aminoindane), methylone, PFA (para...

  7. Pig Liver Esterase (PLE) as Biocatalyst in Organic Synthesis: From Nature to Cloning and to Practical Applications

    NARCIS (Netherlands)

    Dominguez de Maria, Pablo; Garcia-Burgos, Carlos A.; Bargeman, Gerrald; van Gemert, Robert W.

    2007-01-01

    Pig liver esterase (PLE, EC 3.1.1.1) has been employed extensively for research purposes during the last three decades, especially in kinetic resolutions, in desymmetrizations of prochiral substrates, and in the synthesis of nucleosides. Its practical use, however, has been traditionally hampered

  8. Ionic liquid solutions as extractive solvents for value-added compounds from biomass.

    Science.gov (United States)

    Passos, Helena; Freire, Mara G; Coutinho, João A P

    2014-12-01

    In the past few years, the number of studies regarding the application of ionic liquids (ILs) as alternative solvents to extract value-added compounds from biomass has been growing. Based on an extended compilation and analysis of the data hitherto reported, the main objective of this review is to provide an overview on the use of ILs and their mixtures with molecular solvents for the extraction of value-added compounds present in natural sources. The ILs (or IL solutions) investigated as solvents for the extraction of natural compounds, such as alkaloids, flavonoids, terpenoids, lipids, among others, are outlined. The extraction techniques employed, namely solid-liquid extraction, and microwave-assisted and ultrasound-assisted extractions, are emphasized and discussed in terms of extraction yields and purification factors. Furthermore, the evaluation of the IL chemical structure and the optimization of the process conditions (IL concentration, temperature, biomass-solvent ratio, etc.) are critically addressed. Major conclusions on the role of the ILs towards the extraction mechanisms and improved extraction yields are additionally provided. The isolation and recovery procedures of the value-added compounds are ascertained as well as some scattered strategies already reported for the IL solvent recovery and reusability. Finally, a critical analysis on the economic impact versus the extraction performance of IL-based methodologies was also carried out and is here presented and discussed.

  9. Dispersive liquid-liquid microextraction coupled with magnetic nanoparticles for extraction of zearalenone in wheat samples

    Directory of Open Access Journals (Sweden)

    Mitra Amoli-Diva

    2017-01-01

    Full Text Available A new, sensitive and fast dispersive liquid-liquid microextraction (DLLME coupled with micro-solid phase extraction (μ-SPE was developed for determination of zearalenone (ZEN in wheat samples. The DLLME was performed using acetonitrile/water (80:20 v/v as the disperser solvent and 1-octanol as the extracting solvent.  The acetonitrile/water (80:20 v/v solvent was also used to extract ZEN from solid wheat matrix, and was directly applied as the disperser solvent for DLLME process. Additionally, hydrophobic oleic-acid-modified magnetic nanoparticles were used in μ-SPE approach to retrieve the analyte from the DLLME step. So, the method uses high surface area and strong magnetism properties of these nanoparticles to avoid time-consuming column-passing processes in traditional SPE. Main parameters affecting the extraction efficiency and signal enhancement were investigated and optimized. Under the optimum conditions, the calibration curve showed a good linearity in the range of 0.1-500 μg kg−1 (R2=0.9996 with low detection limit of 83 ng g−1. The intra-day and inter-day precisions (as RSD % in the range of 2.6-4.3 % and high recoveries ranging from 91.6 to 99.1 % were obtained. The pre-concentration factor was 3. The method is simple, inexpensive, accurate and remarkably free from interference effects.

  10. Factors influencing the thermodynamic isotope effect of lithium in polyetherlithium liquid-liquid extraction systems

    International Nuclear Information System (INIS)

    Fu Lian; Fang Shengqiang; Yao Zhongqi; Gao Zhichang; Tan Ganzhu

    1989-01-01

    The published data up to now concerning polyether-lithium liquid-liquid extraction systems, can be summarized by the equation, ε p = (α-1)/[1 + 0.46(1-P)], where α denotes the isotope separation factor; P - the ratio of the lithium concentration in the organic phase to the initial concentration of crown ethers; ε p -the enrichment coefficient as P = 100%. Based on the changes in ε p , P, α and D(distribution ratio), the functions of factors such as polyether's structure, polyether's side group, polyether's concentration, organic solvent, negative ion of lithium salt and lithium salt's concentration, are discussed and reported

  11. Modified Dispersive Liquid-Liquid Micro Extraction Using Green Solvent for Determination of Polycyclic Aromatic Hydrocarbons (PAHs) in Vegetable Samples

    International Nuclear Information System (INIS)

    Kin, C.M.; Shing, W.L.

    2016-01-01

    According to International Agency for Research on Cancer (IARC), most of Polycyclic Aromatic Hydrocarbons (PAHs) known as genotoxic human carcinogen and mutagenic. PAHs represent as poorly degradable pollutants that exist in soils, sediments, surface water and atmosphere. A simple, rapid and sensitive extraction method termed modified Dispersive Liquid-Liquid Micro extraction (DLLME) using green solvent was developed to determine PAHs in vegetable samples namely radish, cabbage and cucumber prior to Gas Chromatography Flame Ionization Detection (GC-FID). The extraction method is based on replacing chlorinated organic extraction solvent in the conventional DLLME with low toxic solvent, 1-bromo-3-methylbutane without using dispersive solvent. Several experimental factors such as type and volume of extraction solvents, extraction time, confirmation of 12 PAHs by GC-MS, recovery percentages on vegetable samples and the comparative analysis with conventional DLLME were carried out. Both DLLME were successfully extracted 12 types of PAHs. In modified DLLME, the recoveries of the analytes obtained were in a range of 72.72 - 88.07 % with RSD value below 7.5 % which is comparable to the conventional DLLME. The use of microliter of low toxic extraction solvent without addition of dispersive solvent caused the method is economic and environmental friendly which is fulfill the current requirement, green chemistry based analytical method. (author)

  12. Solvent extraction in the treatment of acidic high-level liquid waste : where do we stand?

    International Nuclear Information System (INIS)

    Horwitz, E. P.; Schulz, W. W.

    1998-01-01

    During the last 15 years, a number of solvent extraction/recovery processes have been developed for the removal of the transuranic elements, 90 Sr and 137 Cs from acidic high-level liquid waste. These processes are based on the use of a variety of both acidic and neutral extractants. This chapter will present an overview and analysis of the various extractants and flowsheets developed to treat acidic high-level liquid waste streams. The advantages and disadvantages of each extractant along with comparisons of the individual systems are discussed

  13. Recovery of Acetic Acid from An Ethanol Fermentation Broth by Liquid-Liquid Extraction (LLE) Using Various Solvents

    International Nuclear Information System (INIS)

    Pham, Thi Thu Huong; Kim, Tae Hyun; Um, Byung Hwan

    2015-01-01

    Liquid-liquid extraction (LLE) using various solvents was studied for recovery of acetic acid from a synthetic ethanol fermentation broth. The microbial fermentation of sugars presented in hydrolyzate gives rise to acetic acid as a byproduct. In order to obtain pure ethanol for use as a biofuel, fermentation broth should be subjected to acetic acid removal step and the recovered acetic acid can be put to industrial use. Herein, batch LLE experiments were carried out at 25°C using a synthetic fermentation broth comprising 20.0 g l -1 acetic acid and 5.0 g l -1 ethanol. Ethyl acetate (EtOAc), tri-n-octylphosphine oxide (TOPO), tri-n-octylamine (TOA), and tri-n-alkylphosphine oxide (TAPO) were utilized as solvents, and the extraction potential of each solvent was evaluated by varying the organic phase-to-aqueous phase ratios as 0.2, 0.5, 1.0, 2.0, and 4.0. The highest acetic acid extraction yield was achieved with TAPO; however, the lowest ethanol-to-acetic acid extraction ratio was obtained using TOPO. In a single-stage batch extraction, 97.0 % and 92.4 % of acetic acid could be extracted using TAPO and TOPO when the ratio of organic-to-aqueous phases is 4:1 respectively. A higher solvent-to-feed ratio resulted in an increase in the ethanol-to-acetic acid ratio, which decreased both acetic acid purity and acetic acid extraction yield.

  14. Complex Formation in a Liquid-Liquid Extraction System Containing Cobalt(II, 4-(2-Pyridylazoresorcinol, and Nitron

    Directory of Open Access Journals (Sweden)

    Petya Vassileva Racheva

    2013-01-01

    Full Text Available Complex formation and liquid-liquid extraction were studied in a system containing cobalt(II, 4-(2-pyridylazoresorcinol (PAR, 1,4-diphenyl-3-(phenylamino-1H-1,2,4-triazole (Nitron, Nt, water, and chloroform. The effect of some experimental parameters (pH, shaking time, concentration of PAR, and concentration of Nt was systematically investigated, and the optimum conditions for cobalt extraction as an ion-association complex, (NtH+[Co3+(PAR2], were found. The following key equilibrium constants were calculated: constant of association (Log β=4.77±0.06, constant of distribution (LogKD=1.34±0.01, and constant of extraction (LogKex=6.11±0.07. Beer’s law was obeyed for Co concentrations up to 1.7 μg mL−1 with a molar absorptivity of 6.0×104 L mol−1 cm−1 at λmax=520 nm. Some additional characteristics, such as limit of detection, limit of quantification, and Sandell’s sensitivity, were estimated as well.

  15. Lunar Oxygen Production and Metals Extraction Using Ionic Liquids

    Science.gov (United States)

    Marone, Matthew; Paley, Mark Steven; Donovan, David N.; Karr, Laurel J.

    2009-01-01

    Initial results indicate that ionic liquids are promising media for the extraction of oxygen from lunar regolith. IL acid systems can solubilize regolith and produce water with high efficiency. IL electrolytes are effective for water electrolysis, and the spent IL acid media are capable of regeneration.

  16. Determination of trace amount of lead in industrial and municipal effluent water samples based on dispersive liquid-liquid extraction

    Energy Technology Data Exchange (ETDEWEB)

    Shirkhanloo, H. [Iranian Petroleum Industry Health Research Institute, Occupational and Environmental Health Research Center, Tehran (Iran, Islamic Republic of); Sedighi, K.; Mousavi, H. Z., E-mail: hzmousavi@semnan.ac.ir [Semnan University, College of Science, Department of Chemistry, Semnan (Iran, Islamic Republic of)

    2014-10-01

    In this study, a simple, sensitive and accurate method was developed for the determination of lead ion by combining ionic liquid dispersive liquid-liquid extraction (Il-DLL E) with flame atomic absorption spectrometry. Tetraethyl thiuram disulfide (Tetd), acetone and 1-octyl-3m ethylimidazolium hexafluorophosphate [(C{sub 8}MIM) (PF{sub 6})] were used as the chelating agent, dispersive and extraction solvent, respectively. Under the optimal conditions, the calibration graph was linear in the range of 5-190 μg L{sup -1} of lead and the detection limit was 0.8 μg L{sup -1} with a sample volume of 200 ml. The proposed method was validated by the analysis of one certified reference material and applied successfully to the determination of lead in real water samples. (Author)

  17. Complex investigation of extraction techniques applied for cyclitols and sugars isolation from different species of Solidago genus.

    Science.gov (United States)

    Ratiu, Ileana-Andreea; Al-Suod, Hossam; Ligor, Magdalena; Ligor, Tomasz; Railean-Plugaru, Viorica; Buszewski, Bogusław

    2018-03-15

    Cyclitols are phytochemicals naturally occurring in plant material, which attracted an increasing interest due to multiple medicinal attributes, among which the most important are the antidiabetic, antioxidant, and anticancer properties. Due to their valuable properties, sugars are used in the food industry as sweeteners, preservatives, texture modifiers, fermentation substrates, and flavoring and coloring agents. In this study, we report for the first time the quantitative analysis of sugars and cyclitols isolated from Solidago virgaurea L., which was used for the selection of the optimal solvent and extraction technique that can provide the best possible yield. Moreover, the quantities of sugars and cyclitols extracted from two other species, Solidago canadensis and Solidago gigantea, were investigated using the best extraction method and the most appropriate solvent. Comparative analysis of natural plant extracts obtained using five different techniques-maceration, Soxhlet extraction, pressurized liquid extraction, ultrasound-assisted extraction, and supercritical fluid extraction-was performed in order to decide the most suitable, efficient, and economically convenient extraction method. Three different solvents were used. Analysis of samples has been performed by solid-phase extraction for purification and pre-concentration, followed by derivation and GC-MS analysis. Highest efficiency for the total amount of obtained compounds has been reached by PLE, when water was used as a solvent. d-pinitol amount was almost similar for every solvent and for all the extraction techniques involved. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Extraction behaviour and mechanism of Pt(iv) and Pd(ii) by liquid-liquid extraction with an ionic liquid [HBBIm]Br.

    Science.gov (United States)

    Liu, Wenhui; Wang, Qi; Zheng, Yan; Wang, Shubin; Yan, Yan; Yang, Yanzhao

    2017-06-06

    In this study, a method of one-step separation and recycling of high purity Pd(ii) and Pt(iv) using an ionic liquid, 1-butyl-3-benzimidazolium bromate ([HBBIm]Br), was investigated. The effects of [HBBIm]Br concentration, initial metal concentration, and loading capacity of [HBBIm]Br were examined in detail. It was observed that [HBBIm]Br was a very effective extractant for selectively extracting Pd(ii) and precipitating Pt(iv). Through selectively extracting Pd(ii) and precipitating Pt(iv), each metal with high purity was separately obtained from mixed Pd(ii) and Pt(iv) multi-metal solution. The method of one-step separation of Pd(ii) and Pt(iv) is simple and convenient. The anion exchange mechanism between [HBBIm]Br and Pt(iv) was proven through Job's method and FTIR and 1 H NMR spectroscopies. The coordination mechanism between [HBBIm]Br and Pd(ii) was demonstrated via single X-ray diffraction and was found to be robust and distinct, as supported by the ab initio quantum-chemical studies. The crystals of the [PdBr 2 ·2BBIm] complex were formed first. Moreover, the influence of the concentrations of hydrochloric acid, sodium chloride, and sodium nitrate on the precipitation of Pt(iv) and extraction of Pd(ii) was studied herein. It was found that only the concentration of H + could inhibit the separation of Pt(iv) because H + could attract the anion PtCl 6 2- ; thus, the exchange (anion exchange mechanism) between the anions PtCl 6 2- and Br - was prevented. However, both the concentration of H + and Cl - can obviously inhibit the extraction of Pd(ii) because H + and Cl - are the reaction products and increasing their concentration can inhibit the progress of the reaction (coordination mechanism).

  19. Synthesis, characterization and application of 1-butyl-3-methylimidazolium tetrafluoroborate for extractive desulfurization of liquid fuel

    Directory of Open Access Journals (Sweden)

    Swapnil A. Dharaskar

    2016-07-01

    Full Text Available In the present paper the experimental data of extractive desulfurization of liquid fuel using 1-butyl-3-methylimidazolium tetrafluoroborate [BMIM]BF4 have been presented. The data of FTIR, 1H NMR and 13C NMR have been discussed for the molecular confirmation of synthesized [BMIM]BF4. Further, the thermal properties, conductivity, solubility, and viscosity analysis of the [BMIM]BF4 were carried out. The effects of reaction time, reaction temperature, sulfur compounds, and recycling of ionic liquid without regeneration on dibenzothiophene removal of liquid fuel were presented. In extractive desulfurization process, the removal of dibenzothiophene in n-dodecane was 73.02% for mass ratio of 1:1 in 30 min at 30 °C under the mild reaction conditions. The ionic liquids could be reused four times without a significant decrease in activity. Also, the desulfurizations of real fuels, multistage extraction were presented. The data and results provided in the present paper explore the significant insights of imidazoled ILs for extractive desulfurization of liquid fuels.

  20. Comparison between different liquid-liquid and solid phase methods of extraction prior to the identification of the phenolic fraction present in olive oil washing wastewater from the two-phase olive oil extraction system

    Directory of Open Access Journals (Sweden)

    S. Jiménez-Herrera

    2017-09-01

    Full Text Available Phenolic compounds from olive mill wastewater (OMW, are characterized by a strong antioxidant activity. At the same time, they represent an environmental problem because they are difficult to degrade. The purpose of this work was to identify these biologically active compounds in the OMW from two-phase olive oil production in order to convert a polluting residue into a source of natural antioxidants. After optimizing the extraction process of phenolic compounds using liquid-liquid extraction (LLE and solid phase extraction (SPE methods, it was determined that the most appropriate sequence comprised a previous centrifugation to remove the lipid fraction, followed by liquid extraction with ethyl acetate or SPE. The most important compounds identified in olive oil washing wastewater (OOWW were tyrosol, hydroxytyrosol and succinic acid; whereas the ones in the wastewater derived from the washing of the olives (OWW were cresol, catechol, 4-methylcatechol, hydrocinnamic acid and p-hydroxy-hydrocinnamic acid.

  1. Comparison between different liquid-liquid and solid phase methods of extraction prior to the identification of the phenolic fraction present in olive oil washing wastewater from the two-phase olive oil extraction system

    International Nuclear Information System (INIS)

    Jiménez-Herrera, S.; Ochando-Pulido, J.M.; Martínez-Ferez, A.

    2017-01-01

    Phenolic compounds from olive mill wastewater (OMW), are characterized by a strong antioxidant activity. At the same time, they represent an environmental problem because they are difficult to degrade. The purpose of this work was to identify these biologically active compounds in the OMW from two-phase olive oil production in order to convert a polluting residue into a source of natural antioxidants. After optimizing the extraction process of phenolic compounds using liquid-liquid extraction (LLE) and solid phase extraction (SPE) methods, it was determined that the most appropriate sequence comprised a previous centrifugation to remove the lipid fraction, followed by liquid extraction with ethyl acetate or SPE. The most important compounds identified in olive oil washing wastewater (OOWW) were tyrosol, hydroxytyrosol and succinic acid; whereas the ones in the wastewater derived from the washing of the olives (OWW) were cresol, catechol, 4-methylcatechol, hydrocinnamic acid and p-hydroxy-hydrocinnamic acid. [es

  2. Study on novel ionic liquids as extracting agent for priority metals from waste waters

    International Nuclear Information System (INIS)

    Fischer, L.; Falta, T.; Stingeder, G.; Koellensperger, G.; Hann, S.; Kogelnig, D.; Stojanovic, A.; Krachler, R.; Keppler, B.K.

    2009-01-01

    Full text: As the new EU Water Framework Directive (2000/60/EC) sets high environmental quality standards for priority substances in surface water, effective procedures for wastewater treatment are required. The characteristics of ionic liquids (IL) can be adjusted by modifying their ionic composition for liquid-liquid extraction of metals and metal containing compounds (Cd, Hg, Ni, Pb, tributyltin, cancerostatic platinum compounds) from the water phase. The potential of novel IL for selective removal of the above mentioned substances regarding extraction time, pH and matrix were determined by ICPSFMS, HPLC-ICPMS and GC-ICPMS measurements. (author)

  3. Possible applications of crown-ethers to metal extraction using liquid membrane technology - a literature survey

    International Nuclear Information System (INIS)

    Dozol, M.

    1990-01-01

    Ether-crowns, discovered in 1967 by J.C. PEDERSEN, exhibit attractive complexive and extractive properties, enhanced in various fields, such as analytical chemistry, chemical synthesis, field of biology, or extractive chemistry. The investigations carried out on these macrocyclic compounds are continually increasing, as show in international literature. Among the focus of interest, the applications to metal extraction are extensively studied with crown compounds present in liquid phase or impregnated on supports (membranes or resins). The goal of this paper is to describe the application of crown-ethers to metal extraction, using liquid membrane processes. 69 refs

  4. Micro-electromembrane extraction across free liquid membranes. Extractions of basic drugs from undiluted biological samples

    Czech Academy of Sciences Publication Activity Database

    Kubáň, Pavel; Boček, Petr

    2014-01-01

    Roč. 1337, Apr (2014), s. 32-39 ISSN 0021-9673 R&D Projects: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : micro-electromembrane extraction * free liquid membranes * biological samples Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.169, year: 2014

  5. Extraction of metal ions through ligand assisted ionic liquids

    International Nuclear Information System (INIS)

    Kumar, P.; Vincent, T.; Khanna, A.

    2014-01-01

    Extraction of Strontium by crown ether (DCH18C6) has been investigated in [BMIM][TF2N] Ionic Liquid (IL) giving higher extraction ~98% and distribution ratio as compared to other organic solvents (Dodecane, Hexane, & Isodecyl alcohol + Dodecane). Distribution ratio of Sr in IL at 0.15M DCH18C6 indicates an enhancement of 20000, 2000, 500 times over Dodecane, Hexane and 5% Isodecyl Alcohol + 95 % Dodecane at 0.01M aqueous acidity respectively. In presence of IL Sr extraction decreases with increase in HNO 3 concentration in aqueous phase whereas opposite trend was observed with organic solvents. Extraction of Sr initially increases with increase in DCH18C6 concentration in IL, finally reaching an asymptotic constant. Sr can be stripped from the organic phase by precipitating with K 2 SO 4 . (author)

  6. Ionic liquids based simultaneous ultrasonic and microwave assisted extraction of phenolic compounds from burdock leaves

    International Nuclear Information System (INIS)

    Lou Zaixiang; Wang Hongxin; Zhu Song; Chen Shangwei; Zhang Ming; Wang Zhouping

    2012-01-01

    The ionic liquids based simultaneous ultrasonic and microwave assisted extraction (IL-UMAE) technique was first proposed and applied to isolate compounds. The ionic liquids comprising a range of four anions, five 1-alkyl-3-methylimidazolium derivatives were designed and prepared. The results suggested that varying the anion and cation both had apparent effects on the extraction of phenolics. The results also showed that irradiation power, time and solid–liquid ratio significantly affected the yields. The yields of caffeic acid and quercetin obtained by IL-UMAE were higher than those by regular UMAE. Compared with conventional heat-reflux extraction (HRE), the proposed approach exhibited higher efficiency (8–17% enhanced) and shorter extraction time (from 5 h to 30 s). The results indicated ILUMAE to be a fast and efficient extraction technique. Moreover, the proposed method was validated by the reproducibility and recovery experiments. The ILUMAE method provided good recoveries (from 96.1% to 105.3%) with RSD lower than 5.2%, which indicated that the proposed method was credible. Based on the designable nature of ionic liquids, and the rapid and highly efficient performance of the proposed approach, ILUMAE provided a new alternative for preparation of various useful substances from solid samples.

  7. Optimisation of pressurized liquid extraction using a multivariate chemometric approach for the determination of anticancer drugs in sludge by ultra high performance liquid chromatography-tandem mass spectrometry

    OpenAIRE

    Seira , Jordan; Claparols , Catherine; Joannis-Cassan , Claire; Albasi , Claire; Montréjaud-Vignoles , Mireille; Sablayrolles , Caroline

    2013-01-01

    International audience; The present paper describes an analytical method for the determination of 2 widely administered anticancer drugs, ifosfamide and cyclophosphamide, contained in sewage sludge. The method relies on the extraction from the solid matrix by pressurized liquid extraction, sample purification by solid-phase extraction and analysis by ultra high performance liquid chromatography coupled with tandem mass spectrometry. The different parameters affecting the extraction efficiency...

  8. [Protein losing enteropathy (PLE) detected by Tc99m-labelled human serum albumin abdominal scintigraphy--case report].

    Science.gov (United States)

    Hubalewska-Hoła, Alicja; Sowa-Staszczak, Anna; Szczerbiński, Tomasz; Lis, Grzegorz; Huszno, Bohdan; Szybiński, Zbigniew

    2003-01-01

    Protein losing enteropathy (PLE) is a gastrointestinal disorder that is associated with excessive loss of plasma protein into the gut resulting from abnormal mucosal permeability. The disease is usually caused by inflammation. The loss of protein in PLE is a nonselective process affecting albumin, globulin and transferrin. Abdominal scintigraphy with human serum albumin marked by Tc99m seems to be an easy and sensitive method for diagnosing PLE. An 4-year-old girl was presented to an outside Pediatric Department due to hypoproteinemia and recurrent pneumonia which had caused several prior hospitalizations. The laboratory tests revealed hypoproteinemia, hypoalbuminemia, low level of IgG, sideropenia, and a decreased level of T lymphocytes. The loss of protein into the gut was confirmed by fecal clearance of alfa-1 antitrypsin. Only nonspecific inflammation was detected by biopsy of the small intestine. These clinical and laboratory findings, quickly decreasing IgG and albumin levels in spite of i.v. supplementation and the lack of proteinuria permitted PLE diagnosis. The abdominal scintigraphy was planned to assess and localise protein losing through GIT and for strategy of possible surgical treatment. Abdominal dynamic scintigraphy was performed immediately after the injection of 300 MBq Tc99m human albumin. 90 images were taken within 180 minutes. Delayed abdominal images were obtained 6 and 24 hours after the tracer injection. Anterior abdominal scintigraphy showed pathological activity of Tc99m-albumin in small bowel in the upper left segment of the abdomen in the 40th minute after injection. Extensive accumulation of albumin was seen in the 160th minute. Delayed images, after 3 and 6 hours, revealed translocation of the tracer into the lower right abdominal segment. The further passage and tracer concentration was detected in ascendant and transverse colon. Based on the laboratory tests and scintigraphic images the girl was suspected to have segmental

  9. Liquid-liquid and solid-phase extractions of phenols from virgin olive oil and their separation by chromatographic and electrophoretic methods.

    Science.gov (United States)

    Bendini, Alessandra; Bonoli, Matteo; Cerretani, Lorenzo; Biguzzi, Barbara; Lercker, Giovanni; Toschi, Tullia Gallina

    2003-01-24

    The high oxidative stability of virgin olive oil is related to its high monounsaturated/polyunsaturated ratio and to the presence of antioxidant compounds, such as tocopherols and phenols. In this paper, the isolation of phenolic compounds from virgin olive oil, by different methods, was tested and discussed. Particularly liquid-liquid and solid-phase extraction methods were compared, assaying, for the latter, three stationary phases (C8, C18 and Diol) and several elution mixtures. Quantification of phenolic and o-diphenolic substances in the extracts was performed by the traditional Folin-Ciocalteau method and the sodium molybdate reaction, respectively. Furthermore, the quantification of phenolic compounds in the extracts and in a standard mixture was carried out both with diode array and mass spectrometric detection and capillary zone electrophoresis.

  10. Dispersive liquid-liquid microextraction with solidification of floating organic droplets for simultaneous extraction of pesticides, pharmaceuticals and personal care products

    International Nuclear Information System (INIS)

    Marube, Liziane Cardoso; Caldas, Sergiane Souza; Soares, Karina Lotz; Primel, Ednei Gilberto

    2015-01-01

    Dispersive liquid-liquid microextraction based on solidification of floating organic droplets (DLLME-SFO) has been applied to the extraction of pharmaceutical and personal care products (PPCPs) and pesticides from water samples. The PPCPs included bisphenol A, sodium diclofenac, gemfibrozil, furosemide, glibenclamide, nifedipine, nimesulide, propylparaben and triclocarban. The pesticides included 2,4-D, atrazine, azoxystrobin, cyproconazole, clomazone, dichloran, difenoconazole, diuron, epoxiconazole, fenoxaprop-p-ethyl, fipronil, iprodione, irgarol, propanil, propiconazole, tebuconazole, and trifloxystrobin. The type and volume of extraction solvent, type and volume of disperser solvent, ionic strength and pH were optimized. All species were then quantified by liquid chromatography tandem mass spectrometry (LC-MS/MS). The limits of quantification (LOQs) ranged from 50 to 500 ng L −1 , and the linearity ranged from the LOQ of each compound up to 10,000 ng L −1 . Recoveries ranged from 63 to 120 %, with relative standard deviations lower than 14 %. It is making use of a low-toxicity and affordable extraction solvent (1-dodecanol) and was successfully applied to the analysis of surface water samples. (author)

  11. A green deep eutectic solvent dispersive liquid-liquid micro-extraction (DES-DLLME) for the UHPLC-PDA determination of oxyprenylated phenylpropanoids in olive, soy, peanuts, corn, and sunflower oil.

    Science.gov (United States)

    Ferrone, Vincenzo; Genovese, Salvatore; Carlucci, Maura; Tiecco, Matteo; Germani, Raimondo; Preziuso, Francesca; Epifano, Francesco; Carlucci, Giuseppe; Taddeo, Vito Alessandro

    2018-04-15

    A green dispersive liquid-liquid microextraction (DLLME) using deep eutectic solvent (DES) as the extracting solvent has been developed and applied for the simultaneous quantification of ferulic acid, umbelliferone, boropinic acid, 7-isopentenyloxycoumarin, 4'-geranyloxyferulic acid (GOFA), and auraptene in some vegetable oils using ultra high performance liquid chromatography (UHPLC) with photodiode array detection (PDA). All parameters in the extraction step, including selection and loading of both extracting and dispersing solvents, amount of both extractant and disperser solvent were investigated and optimized. PhAA/TMG DES achieved higher recovery and enrichment factor compared to other DESs. The validated method showed good linearity with correlation coefficients, r 2 >0.9990 for all the analytes. Furthermore, this is the first time that eco-friendly solvents are used for the extraction of oxyprenylated phenylpropanoids and the corresponding extract analyzed with ultra high performance liquid chromatography with photodiode array detection. Copyright © 2017 Elsevier Ltd. All rights reserved.

  12. Chiral separation of substituted phenylalanine analogues using chiral palladium phosphine complexes with enantioselective liquid-liquid extraction

    NARCIS (Netherlands)

    Verkuijl, B.J.V.; Schuur, B.; Minnaard, A.J.; Vries, de J.G.; Feringa, B.L.

    2010-01-01

    Chiral palladium phosphine complexes have been employed in the chiral separation of amino acids and phenylalanine analogues in particular. The use of (S)-xylyl-BINAP as a ligand for the palladium complex in enantioselective liquid–liquid extraction allowed the separation of the phenylalanine

  13. Feasibility of corona discharge ion mobility spectrometry for direct analysis of samples extracted by dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Jafari, Mohammad T; Riahi, Farhad

    2014-05-23

    The capability of corona discharge ionization ion mobility spectrometry (CD-IMS) for direct analysis of the samples extracted by dispersive liquid-liquid microextraction (DLLME) was investigated and evaluated, for the first time. To that end, an appropriate new injection port was designed and constructed, resulting in possibility of direct injection of the known sample volume, without tedious sample preparation steps (e.g. derivatization, solvent evaporation, and re-solving in another solvent…). Malathion as a test compound was extracted from different matrices by a rapid and convenient DLLME method. The positive ion mobility spectra of the extracted malathion were obtained after direct injection of carbon tetrachloride or methanol solutions. The analyte responses were compared and the statistical results revealed the feasibility of direct analysis of the extracted samples in carbon tetrachloride, resulting in a convenient methodology. The coupled method of DLLME-CD-IMS was exhaustively validated in terms of sensitivity, dynamic range, recovery, and enrichment factor. Finally, various real samples of apple, river and underground water were analyzed, all verifying the feasibility and success of the proposed method for the easy extraction of the analyte using DLLME separation before the direct analysis by CD-IMS. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. A new dispersive liquid-liquid microextraction using ionic liquid based microemulsion coupled with cloud point extraction for determination of copper in serum and water samples.

    Science.gov (United States)

    Arain, Salma Aslam; Kazi, Tasneem Gul; Afridi, Hassan Imran; Arain, Mariam Shahzadi; Panhwar, Abdul Haleem; Khan, Naeemullah; Baig, Jameel Ahmed; Shah, Faheem

    2016-04-01

    A simple and rapid dispersive liquid-liquid microextraction procedure based on ionic liquid assisted microemulsion (IL-µE-DLLME) combined with cloud point extraction has been developed for preconcentration copper (Cu(2+)) in drinking water and serum samples of adolescent female hepatitits C (HCV) patients. In this method a ternary system was developed to form microemulsion (µE) by phase inversion method (PIM), using ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ([C4mim][PF6]) and nonionic surfactant, TX-100 (as a stabilizer in aqueous media). The Ionic liquid microemulsion (IL-µE) was evaluated through visual assessment, optical light microscope and spectrophotometrically. The Cu(2+) in real water and aqueous acid digested serum samples were complexed with 8-hydroxyquinoline (oxine) and extracted into IL-µE medium. The phase separation of stable IL-µE was carried out by the micellar cloud point extraction approach. The influence of of different parameters such as pH, oxine concentration, centrifugation time and rate were investigated. At optimized experimental conditions, the limit of detection and enhancement factor were found to be 0.132 µg/L and 70 respectively, with relative standard deviation <5%. In order to validate the developed method, certified reference materials (SLRS-4 Riverine water) and human serum (Sero-M10181) were analyzed. The resulting data indicated a non-significant difference in obtained and certified values of Cu(2+). The developed procedure was successfully applied for the preconcentration and determination of trace levels of Cu(2+) in environmental and biological samples. Copyright © 2015 Elsevier Inc. All rights reserved.

  15. CHEMOMETRICS IN BIOANALYTICAL SAMPLE PREPARATION - A FRACTIONATED COMBINED MIXTURE AND FACTORIAL DESIGN FOR THE MODELING OF THE RECOVERY OF 5 TRICYCLIC AMINES FROM PLASMA AFTER LIQUID-LIQUID-EXTRACTION PRIOR TO HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY

    NARCIS (Netherlands)

    WIELING, J; MENSINK, CK; JONKMAN, JHG; COENEGRACHT, PMJ; DUINEVELD, CAA; DOORNBOS, DA

    1993-01-01

    A general systematic approach is described for the chemometric modelling of liquid-liquid extraction data of drugs from biological fluids. Extraction solvents were selected from Snyder's solvent selectivity triangle: methyl tert.-butyl ether, methylene chloride and chloroform. The composition of a

  16. Ionic-liquid-based ultrasound-assisted extraction of isoflavones from Belamcanda chinensis and subsequent screening and isolation of potential α-glucosidase inhibitors by ultrafiltration and semipreparative high-performance liquid chromatography.

    Science.gov (United States)

    Li, Senlin; Li, Sainan; Huang, Yu; Liu, Chunming; Chen, Lina; Zhang, Yuchi

    2017-06-01

    The separation of a compound of interest from its structurally similar homologues to produce high-purity natural products is a challenging problem. This work proposes a novel method for the separation of iristectorigenin A from its structurally similar homologues by ionic-liquid-based ultrasound-assisted extraction and the subsequent screening and isolation of potential α-glucosidase inhibitors via ultrafiltration and semipreparative high-performance liquid chromatography. Ionic-liquid-based ultrasound-assisted extraction was successfully applied to the extraction of tectorigenin, iristectorigenin A, irigenin, and irisflorentin from Belamcanda chinensis. The optimum conditions for the efficient extraction of isoflavones were determined as 1.0 M 1-ethyl-3-methylimidazolium tetrafluoroborate with extraction time of 30 min and a solvent to solid ratio of 30 mL/g. Ultrafiltration with liquid chromatography and mass spectrometry was applied to screen and identify α-glucosidase inhibitors from B. chinensis, followed by the application of semipreparative high-performance liquid chromatography to separate and isolate the active constituents. Four major compounds including tectorigenin, iristectorigenin A, irigenin, and irisflorentin were screened and identified as α-glucosidase inhibitors, and then the four active compounds abovementioned were subsequently isolated by semipreparative high-performance liquid chromatography (99.89, 88.97, 99.79, and 99.97% purity, respectively). The results demonstrate that ionic liquid extraction can be successfully applied to the extraction of isoflavones from B. chinensis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Poisoning of liquid membrane carriers in extraction of metal ions

    International Nuclear Information System (INIS)

    Wang, Yuchun; Wang, Dexian

    1992-01-01

    As means of effective separation and preconcentration, emulsion liquid membranes (ELMs) have found application in many fields including biochemical separation, wastewater treatment, hydrometallurgy, and preconcentration in analytical chemistry. In the extraction of desired metal (scandium, mixed rare earths) ions using chelating extractants (TTA, HDEHP) as liquid membrane carriers, the carriers will become poisoned owing to the presence of even minute quantity of certain high ionic potential ions in the feed solution. The reason for the poisoning of carriers is that those ions have so much greater affinity than the desired ions for the membrane carrier that the ion-carrier coordination compound cannot be stripped at the interior interface of the membrane and gradually no more free carrier transports any metal ions across the membrane. The calculated results are in agreement with the experiments, and methods to avoid the poisoning are given in the paper

  18. Multi-staging for extraction of cesium from nitric acid by a single liquid-liquid countercurrent centrifugal extractor with Taylor vortices

    International Nuclear Information System (INIS)

    Nakase, Masahiko; Kinuhata, Hiroshi; Takeshita, Kenji

    2013-01-01

    Fission products that emit considerable decay heat and radioactivity, such as 137 Cs, have a large impact on waste management. Small and high-performance extractor is desirable for separating such nuclei. In this study, we implemented the continuous extraction of Cs from nitric acid in a single liquid-liquid countercurrent centrifugal extractor with Taylor Vortices by calix arene-bis(t-octylbenzo-crown-6)(BOBCalixC6) as an extractant with trioctylamine(TOA) as a suppressant and with 1-(2,2,3,3-tetrafluoropropoxy)-3-(4-sec-butylphenoxy)-2-propanol (Cs-7SB) as a phase modifier. Because of slow extraction kinetics of this process, extraction with multiple theoretical stages by just replacing conventional extractors into the single centrifugal extractor is difficult. Hence, we improved the dispersion of organic phase by an inner rotor made of lipophilic epoxy resin and elevating the solution temperature to lower the viscosity. Higher temperature was not appropriate from the aspect of chemical equilibrium in this process, but extraction with multiple theoretical stages was found to be possible. (author)

  19. Selective extraction and recovery of rare earth metals from phosphor powders in waste fluorescent lamps using an ionic liquid system

    International Nuclear Information System (INIS)

    Yang, Fan; Kubota, Fukiko; Baba, Yuzo; Kamiya, Noriho; Goto, Masahiro

    2013-01-01

    Highlights: • Recycling of rare earth metals from fluorescent lamps was conducted by ionic liquid-mediated extraction. • Acid leaching from a waste phosphor powder was carried out using sulfuric and nitric acids. • An ionic liquid was used as extracting solvent for the rare earth metals. • Selective extraction of rare earth metals from leach solutions was attained. •The extracting ionic liquid phase was recyclable in the recovery process. -- Abstract: The recycling of rare earth metals from phosphor powders in waste fluorescent lamps by solvent extraction using ionic liquids was studied. Acid leaching of rare earth metals from the waste phosphor powder was examined first. Yttrium (Y) and europium (Eu) dissolved readily in the acid solution; however, the leaching of other rare earth metals required substantial energy input. Ionization of target rare earth metals from the waste phosphor powders into the leach solution was critical for their successful recovery. As a high temperature was required for the complete leaching of all rare earth metals, ionic liquids, for which vapor pressure is negligible, were used as an alternative extracting phase to the conventional organic diluent. An extractant, N, N-dioctyldiglycol amic acid (DODGAA), which was recently developed, showed a high affinity for rare earth metal ions in liquid–liquid extraction although a conventional commercial phosphonic extractant did not. An effective recovery of the rare earth metals, Y, Eu, La and Ce, from the metal impurities, Fe, Al and Zn, was achieved from the acidic leach solution of phosphor powders using an ionic liquid containing DODGAA as novel extractant system

  20. Selective extraction and recovery of rare earth metals from phosphor powders in waste fluorescent lamps using an ionic liquid system

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Fan; Kubota, Fukiko; Baba, Yuzo [Department of Applied Chemistry, Graduate School of Engineering, Kyushu University, 744 Motooka, Fukuoka 819-0395 (Japan); Kamiya, Noriho [Department of Applied Chemistry, Graduate School of Engineering, Kyushu University, 744 Motooka, Fukuoka 819-0395 (Japan); Center for Future Chemistry, Kyushu University, 744 Motooka, Fukuoka 819-0395 (Japan); Goto, Masahiro, E-mail: m-goto@mail.cstm.kyushu-u.ac.jp [Department of Applied Chemistry, Graduate School of Engineering, Kyushu University, 744 Motooka, Fukuoka 819-0395 (Japan); Center for Future Chemistry, Kyushu University, 744 Motooka, Fukuoka 819-0395 (Japan)

    2013-06-15

    Highlights: • Recycling of rare earth metals from fluorescent lamps was conducted by ionic liquid-mediated extraction. • Acid leaching from a waste phosphor powder was carried out using sulfuric and nitric acids. • An ionic liquid was used as extracting solvent for the rare earth metals. • Selective extraction of rare earth metals from leach solutions was attained. •The extracting ionic liquid phase was recyclable in the recovery process. -- Abstract: The recycling of rare earth metals from phosphor powders in waste fluorescent lamps by solvent extraction using ionic liquids was studied. Acid leaching of rare earth metals from the waste phosphor powder was examined first. Yttrium (Y) and europium (Eu) dissolved readily in the acid solution; however, the leaching of other rare earth metals required substantial energy input. Ionization of target rare earth metals from the waste phosphor powders into the leach solution was critical for their successful recovery. As a high temperature was required for the complete leaching of all rare earth metals, ionic liquids, for which vapor pressure is negligible, were used as an alternative extracting phase to the conventional organic diluent. An extractant, N, N-dioctyldiglycol amic acid (DODGAA), which was recently developed, showed a high affinity for rare earth metal ions in liquid–liquid extraction although a conventional commercial phosphonic extractant did not. An effective recovery of the rare earth metals, Y, Eu, La and Ce, from the metal impurities, Fe, Al and Zn, was achieved from the acidic leach solution of phosphor powders using an ionic liquid containing DODGAA as novel extractant system.

  1. Analysis of 99Tc in the radioactive liquid waste after extraction into suitable solvent

    International Nuclear Information System (INIS)

    Sonar, N.L.; Vaishali De; Pardeshi, V.; Raghvendra, Y.; Valsala, T.P.; Sonavane, M.S.; Kulkarni, Y.; Raj Kanwar

    2012-01-01

    99 Tc is one of the long lived fission product with high fission yield. >From radioactive waste management point of view it is very much essential to evaluate the concentration of technetium in the radioactive liquid waste in order to finalise the treatment process to extract/isolate it from the stream which is discharged to the environment. For the estimation of 99 Tc in the radioactive liquid waste stream, extraction of the stable complex of technetium-tetraphenyl arsonium chloride (TPAC) into chloroform followed by beta counting was studied. Various parameters like pH, time of equilibration, concentration of TPAC in chloroform, use of other solvent for extraction as well as interference of various other radionuclides present in the waste were also studied. The radioactive liquid waste being handled in plant contains high concentrations of salts in the form of sodium nitrate. Hence effect of salt concentration on the percentage extraction was also evaluated. The extraction behavior does not dependent on change in the pH of the solution. Almost 99.5% extraction was observed in the pH range of 1-13.0. High concentration of salt is affecting the extraction. However, this can be taken care by diluting the radioactive waste. It takes almost 90 min time for maximum extraction. Presence of radionuclides like 137 Cs, 90 Sr are not interfering the extraction of 99 Tc. However, 106 Ru is getting slightly extracted along with 99 Tc. The error due to 106 Ru can be eliminated by taking gamma spectrum and deducting the activity from the total beta activity to get 99 Tc activity. Nitrobenzene can be used for extraction of Tc-TPAC complex in place of chloroform. (author)

  2. Determination of organophosphorus pesticides by dispersive liquid-liquid micro extraction coupled with gas chromatography-electron capture detection

    International Nuclear Information System (INIS)

    Mohd Marsin Sanagi; Siti Umairah Mokhtar; Mazidatul Akmam Miskam; Wan Aini Wan Ibrahim

    2011-01-01

    A simple, rapid and sensitive method termed as dispersive liquid-liquid micro extraction (DLLME) combined with gas chromatography-electron capture detector (GC-ECD) was developed for the determination of selected organophosphorus pesticides (OPPs) namely chloropyrifos, dimethoate and diazinon in water sample. In this method, a mixture of carbon disulfide, CS 2 (extraction solvent) and methanol (disperser solvent) was rapidly injected using syringe into the 5.00 mL water sample to form a cloudy solution where the OPPs were extracted into the fine droplets of extraction solvent. Upon centrifugation for 3 min at 3500 rpm, the fine droplets were sedimented at the bottom of the centrifuge tube. Sedimented phase (1 μL) was injected into the GC-ECD for separation and determination of OPPs. Important extraction parameters, such as type of disperser solvent, volume of extraction solvent and volume of disperser solvent were investigated. The optimized conditions for DLLME of the selected OPPs were methanol as disperser solvent, 30 μL of extraction solvent (CS 2 ) and 1.0 mL of disperser solvent (methanol). Under the optimum extraction conditions, the method showed good linearity in the range of 0.1 to 1.0 μg/ mL with correlation coefficient (r 2 ), in the range of 0.9976 to 0.9994 and low limits of detection (LOD) between 0.047 and 0.201 μg/ mL. The proposed method provided acceptable recoveries (72.67- 144 %) with good RSDs ranging from 2.74 % to 7.48 %. This method was successfully applied to the determination of OPPs in water samples obtained from a golf course and chloropyrifos and diazinon were detected at concentration 0.18 μg/ mL and 0.07 μg/ mL, respectively. (author)

  3. Application of dispersive liquid-liquid microextraction and dispersive micro-solid-phase extraction for the determination of quinolones in swine muscle by high-performance liquid chromatography with diode-array detection

    International Nuclear Information System (INIS)

    Tsai, Wen-Hsien; Chuang, Hung-Yi; Chen, Ho-Hsien; Huang, Joh-Jong; Chen, Hwi-Chang; Cheng, Shou-Hsun; Huang, Tzou-Chi

    2009-01-01

    Dispersive liquid-liquid microextraction (DLLME) and dispersive micro-solid-phase extraction (DMSPE) are two simple and low-cost sample preparation methods for liquid samples. In this work, these two methods were applied to solid tissue sample for the determination of seven quinolones by high-performance liquid chromatography with diode-array detection (HPLC-DAD). After the homogenization of the swine muscle with acetonitrile and salt-promoted partitioning, small amounts of the extract were used for the DLLME and DMSPE methods. In the DLLME approach, the target analytes in the extraction solvent were rapidly extracted into a small volume of dichloromethane for drying and the residue was reconstituted for HPLC-DAD analysis. In the DMSPE approach, the target analytes in the extraction solvent were trapped by dispersive silica-based PSA (primary and secondary amine) sorbents and desorbed into a small amount of desorption solution for HPLC-DAD analysis. Under the optimal conditions, relative recoveries were determined for swine muscle spiked 50-200 μg kg -1 and quantification was achieved by matrix-matched calibration. The calibration curves of seven quinolones showed linearity with a correlation coefficient value above 0.998 for both approaches. Relative recoveries ranged from 93.0 to 104.7% and from 95.5 to 111.0% for DLLME and DMSPE, respectively. Limits of detection (LODs) ranged from 5.6 to 23.8 μg kg -1 and from 7.5 to 26.3 μg kg -1 for DLLME and DMSPE, respectively.

  4. Drop of egg production in chickens by experimental infection with an avian metapneumovirus strain PLE8T1 derived from swollen head syndrome and the application to evaluate vaccine.

    Science.gov (United States)

    Sugiyama, Miki; Koimaru, Hiroyuki; Shiba, Masahiro; Ono, Eriko; Nagata, Tadashi; Ito, Toshihiro

    2006-08-01

    Decreases in egg production and increased incidence of abnormal eggs due to malformation of egg shells were observed in specific pathogen free (SPF) 173-day-old laying hens inoculated intravenously with an avian metapneumovirus (aMPV) strain PLE8T1. This strain was derived from an isolate from broiler birds exhibiting swollen head syndrome (SHS). Some SPF birds inoculated with the virus showed, slight diarrhea without any respiratory symptoms. Thus, the PLE8T1 strain was used as a challenge virus to evaluate efficacy of aMPV vaccines. SPF chickens which received a live attenuated aMPV vaccine (NEMOVAC; Merial) at 7 or 77 days old and an inactivated aMPV vaccine (OVO-4; Merial) at 105 days old were protected against poor egg production caused by the challenge with the PLE8T1 strain. Thus, aMPV, the PLE8T1 strain passaged 22 times after isolation, from birds exhibiting SHS, could induce a drop in egg production in laying hens accompanied by malformation of egg shells. It was suggested that this challenge system could be applied to evaluate the efficacy of aMPV vaccine.

  5. Continuous process for selective metal extraction with an ionic liquid

    NARCIS (Netherlands)

    Parmentier, D.; Paradis, S.; Metz, S.J.; Wiedmer, S.K.; Kroon, M.C.

    2016-01-01

    This work describes for the first time a continuous process for selective metal extraction with an ionic liquid (IL) at room temperature. The hydrophobic fatty acid based IL tetraoctylphosphonium oleate ([P8888][oleate]) was specifically chosen for its low viscosity and high selectivity towards

  6. Material analyses of foam-based SiC FCI after dynamic testing in PbLi in MaPLE loop at UCLA

    Energy Technology Data Exchange (ETDEWEB)

    Gonzalez, Maria, E-mail: maria.gonzalez@ciemat.es [LNF-CIEMAT, Avda Complutense, 40, 28040 Madrid (Spain); Rapisarda, David; Ibarra, Angel [LNF-CIEMAT, Avda Complutense, 40, 28040 Madrid (Spain); Courtessole, Cyril; Smolentsev, Sergey; Abdou, Mohamed [Fusion Science and Technology Center, UCLA (United States)

    2016-11-01

    Highlights: • Samples from foam-based SiC FCI were analyzed by looking at their SEM microstructure and elemental composition. • After finishing dynamic experiments in the flowing hot PbLi, the liquid metal ingress has been confirmed due to infiltration through local defects in the protective inner CVD layer. • No direct evidences of corrosion/erosion were observed; these defects could be related to the manufacturing process. - Abstract: Foam-based SiC flow channel inserts (FCIs) developed and manufactured by Ultramet, USA are currently under testing in the flowing hot lead-lithium (PbLi) alloy in the MaPLE loop at UCLA to address chemical/physical compatibility and to access the MHD pressure drop reduction. UCLA has finished the first experimental series, where a single uninterrupted long-term (∼6500 h) test was performed on a 30-cm FCI segment in a magnetic field up to 1.8 T at the temperature of 300 °C and maximum flow velocities of ∼ 15 cm/s. After finishing the experiments, the FCI sample was extracted from the host stainless steel duct and cut into slices. Few of them have been analyzed at CIEMAT as a part of the joint collaborative effort on the development of the DCLL blanket concept in the EU and the US. The initial inspection of the slices using optical microscopic analysis at UCLA showed significant PbLi ingress into the bulk FCI material that resulted in degradation of insulating properties of the FCI. Current material analyses at CIEMAT are based on advanced techniques, including characterization of FCI samples by FESEM to study PbLi ingress, imaging of cross sections, composition analysis by EDX and crack inspection. These analyses suggest that the ingress was caused by local defects in the protective inner CVD layer that might be originally present in the FCI or occurred during testing.

  7. Extraction of rare earth elements with organophosphorus extractants as carriers in supported liquid membranes

    International Nuclear Information System (INIS)

    Kopunec, R.; Benitez, J.C.

    1991-01-01

    The membrane extraction of Y, Ce, Eu, Tm and their binary mixtures Ce-Y, Ce-Eu, Ce-Tm with supported liquid membranes containing TBP and HDEHP as carriers in decane-dodecane hydrocarbon solvent, has been studied. Upon extraction with TBP aqueous nitrate solutions of rare earth elements (REE) were used as feed phase. In some cases they also contained EDTA or DCTA. In most cases, the receiving phase was an aqueous solution of EDTA. Extraction with HDEHP was performed from nitrate and chloride solutions and the receiving phase was the corresponding dilute acid. Pertraction of an element through a membrane was studied as a function of time and of initial composition of phases. The results are presented in the following forms: flux of metal through membrane, coefficients of permeability, separation factors and effective diffusion coefficients. (author) 24 refs.; 8 figs.; 3 tabs

  8. Maghemite nanoparticle-decorated hollow fiber electromembrane extraction combined with dispersive liquid-liquid microextraction for the determination of thymol from Carum copticum

    DEFF Research Database (Denmark)

    Khajeh, Mostafa; Pedersen-Bjergaard, Stig; Bohlooli, Mousa

    2017-01-01

    BACKGROUND A novel technique using maghemite nanoparticle-decorated hollow fibers to assist electromembrane extraction is proposed. Electromembrane extraction combined with dispersive liquid–liquid microextraction (EME-DLLME) was applied for the extraction of thymol from Carum copticum, followed...... by gas chromatography with flame ionization detection (GC-FID). RESULTS The use of maghemite nanoparticle-decorated hollow fibers was found to improve the extraction efficiency of thymol significantly. Important operational parameters, including pH of acceptor phase, extraction time, voltage...

  9. Identification of chemical compounds in a liquid-liquid extraction system

    International Nuclear Information System (INIS)

    Ramirez C, F de M de la.

    1980-01-01

    The objective of the present work is to identify the chemical compounds that are distributed in a liquid-liquid extraction system in which the third phase is observed; for this purpose the FeCl 3 (0.12M) - HCl (8.43M) - Diisopropilic ether - system was used, for the quantitative determination of the chemical compounds, FeCl 3 solutions labelled with 59 Fe or witH 38 Cl were used; the Karl Fischer method for the determination of the water concentration at the organic phases was used, the obtained data was used for the calculations of the H + distribution in each phase. The results are that when the distribution equilibrium is reached, the aqueous phase is a 7.5M HCl solution; the light organic phase contains 2 H[FeCl 4 ].6H 2 O and the dense organic phase contains 2 H[FeCl 4 ].6H 2 O.3HCl.12H 2 O. The differences between these compounds are due to a high concentration of water and the HCl in the organic solvent. This causes a heterogeneous physic field, and then the third phase formation. (author)

  10. The liquid membrane for extraction of Yttrium and Dysprosium from Acid Nitric

    International Nuclear Information System (INIS)

    Johny, W.S.; Raldi-Artono-Koestoer; Kris-Tri-Basuki; Sudibyo

    1996-01-01

    The determination of surfactant in liquid membrane has been done. The surfactant is span-80 (sorbitol-monooleate), the liquid membrane phase was the organic phase (O), the internal liquid phase (W) with ratio O/W = 1, and surfactant. The organic phase using D 2 EHPA in the kerosene and the internal liquid phase using aqua des or acid nitric. The determination of surfactant with variation of span-80 (0,25 - 2%) in the liquid membrane volume. The speed of stirrer was 3500 rpm in 20 minute. The ratio of liquid membrane phase form and external phase (aqua des or acid nitric) was 1, the speed of stirrer was 350 rpm in 10 minute (permeation process). The liquid phase and the liquid membrane phase was separated and then determinated the volume of liquid membrane, the result of percentage of span-80 was 0,25 % volume. The extraction of yttrium and dysprosium in 2 M HNO 3 was Kd y = 2.945 and Kd D y = 0.019

  11. RECOVERY OF CARBOXYLIC ACIDS FROM AQUEOUS SOLUTIONS BY LIQUID-LIQUID EXTRACTION WITH A TRIISOOCTYLAMINE DILUENT SYSTEM

    Directory of Open Access Journals (Sweden)

    G. Malmary

    2001-12-01

    Full Text Available Tertiary alkylamines in solution with organic diluents are attractive extractants for the recovery of carboxylic acids from dilute aqueous phases. The aim of this study was to investigate the mechanism for extraction of organic acids from water by a long-chain aliphatic tertiary amine. In order to attain this objective, we studied the liquid-liquid equilibria between the triisooctylamine + 1-octanol + n-heptane system as solvent and an aqueous solution of an individual carboxylic acid such as citric, lactic and malic acids. The experiments showed that the partition coefficient for a particular organic acid depends on the kind of solute, notably when the acid concentration in the aqueous phase is low. A mathematical model, where both chemical association and physical distribution are taken into consideration, is proposed. The model suggests that the various complexes obtained between amine and organic acids contribute to the distribution of the solute between the coexisting phases in equilibrium.

  12. Extraction of Uranium from Aqueous Solutions Using Ionic Liquid and Supercritical Carbon Dioxide in Conjunction

    International Nuclear Information System (INIS)

    Wang, Joanna S.; Sheaff, Chrystal N.; Yoon, Byunghoon; Addleman, Raymond S.; Wai, Chien M.

    2009-01-01

    Uranyl ions (UO2)2+ in aqueous nitric acid solutions can be extracted into supercritical CO2 (sc-CO2) via an imidazolium-based ionic liquid using tri-n-butylphosphate (TBP) as a complexing agent. The transfer of uranium from the ionic liquid to the supercritical fluid phase was monitored by UV/Vis spectroscopy using a high-pressure fiberoptic cell. The form of the uranyl complex extracted into the supercritical CO2 phase was found to be UO2(NO3)2(TBP)2. The extraction results were confirmed by UV/Vis spectroscopy and by neutron activation analysis. This technique could potentially be used to extract other actinides for applications in the field of nuclear waste management.

  13. 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)

  14. Separation of toluene from n-heptane by liquid–liquid extraction using binary mixtures of [bpy][BF4] and [4bmpy][Tf2N] ionic liquids as solvent

    International Nuclear Information System (INIS)

    García, Silvia; Larriba, Marcos; García, Julián; Torrecilla, José S.; Rodríguez, Francisco

    2012-01-01

    Highlights: ► Binary mixtures of ionic liquids as extraction solvents of aromatics. ► [4bmpy][Tf 2 N] shows higher capacity but lower selectivity than sulfolane. ► [bpy][BF 4 ] shows lower capacity but higher selectivity than sulfolane. ► Mixed {[4bmpy][Tf 2 N] + [bpy][BF 4 ]} improves both extractive properties. - Abstract: The use of binary mixture of ionic liquids N-butylpyridinium tetrafluoroborate ([bpy][BF 4 ]), and 1-butyl-4-methylpyridinium bis(trifluoromethylsulfonyl)imide ([4bmpy][Tf 2 N]) in the liquid–liquid extraction of toluene from n-heptane has been investigated at 313.2 K and atmospheric pressure. The experimental capacity of extraction and selectivity for this binary mixture has proved to be intermediate to those corresponding to the pure ionic liquids, and they can be predicted using a logarithmic–linear model of solubility. Furthermore, the results showed that the use of binary mixture of {[bpy][BF 4 ] + [4bmpy][Tf 2 N]} at a mole solvent composition around 0.7 for [bpy][BF 4 ] improves both the capacity of extraction of toluene and the selectivity with respect to those of sulfolane, the organic solvent taken as a benchmark. Thus, this mixed ionic liquid could be likely to be used in the extraction of aromatic from aliphatic in replacement to sulfolane.

  15. Separation of uranium(VI) by liquid-solid extraction with tri-n-octylphosphine oxide diluted with naphthalene

    International Nuclear Information System (INIS)

    Shigetomi, Y.; Kojima, T.; Kamba, H.; Yamamoto, Y.

    1980-01-01

    Liquid-liquid distribution with tri-n-octylphosphine oxide (TOPO) and molten naphthalene has been investigated for the extraction of 20 metals from nitric acid and hydrochloric acid solutions. Uranium is quantitatively extracted from 1 M nitric acid or hydrochloric acid by using 100 mg of TOPO and 200 mg of naphthalene and shaking for 5 min at 80 0 C, and separated from transition metals, alkaline earth metals and rare earth metals (except scandium). Addition of naphthalene increases the extraction efficiency. (Auth.)

  16. Ultrasound-Assisted Extraction of Carnosic Acid and Rosmarinic Acid Using Ionic Liquid Solution from Rosmarinus officinalis

    Directory of Open Access Journals (Sweden)

    Chunjian Zhao

    2012-09-01

    Full Text Available Ionic liquid based, ultrasound-assisted extraction was successfully applied to the extraction of phenolcarboxylic acids, carnosic acid and rosmarinic acid, from Rosmarinus officinalis. Eight ionic liquids, with different cations and anions, were investigated in this work and [C8mim]Br was selected as the optimal solvent. Ultrasound extraction parameters, including soaking time, solid–liquid ratio, ultrasound power and time, and the number of extraction cycles, were discussed by single factor experiments and the main influence factors were optimized by response surface methodology. The proposed approach was demonstrated as having higher efficiency, shorter extraction time and as a new alternative for the extraction of carnosic acid and rosmarinic acid from R. officinalis compared with traditional reference extraction methods. Ionic liquids are considered to be green solvents, in the ultrasound-assisted extraction of key chemicals from medicinal plants, and show great potential.

  17. 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)

  18. Liquid-liquid extraction. Choice, calculation and design of devices

    International Nuclear Information System (INIS)

    Leybros, J.

    2005-01-01

    The aim of this work is to study the problematic due to the choice of an equipment, to its size and to its industrial bringing into operation. Besides its efficiency to carry out a mass transfer, the economical interest of an industrial device will be proportional to its specific rate (volume treated by surface unit of the cross section of the extractor). Nevertheless, as it seems to be logic to maximize the three parameters which have an influence on it (transfer coefficient, interfacial surface and transfer potential), there exists no device which can modify separately any of these parameters. In order to satisfy these aims, a great diversity of devices have been put on the market. Indeed, it exists about twenty different industrial devices. This diversity leads the engineer, during the design of a solvent extraction device, to take difficult and subjective decisions without pilot experiment on the considered system. The main problem of an economical and optimized calculation of the liquid-liquid extractors from theoretical data has still not found totally satisfying solutions. Thus, except in some cases where we have empirical correlations, the recourse to prototype experiments is required and the most recent advances have resulted essentially to define more reliable rules for the extrapolation of these experiments for the size of industrial devices. (O.M.)

  19. Determination of Np, Pu and Am in high level radioactive waste with extraction-liquid scintillation counting

    International Nuclear Information System (INIS)

    Yang Dazhu; Zhu Yongjun; Jiao Rongzhou

    1994-01-01

    A new method for the determination of transuranium elements, Np, Pu and Am with extraction-liquid scintillation counting has been studied systematically. Procedures for the separation of Pu and Am by HDEHP-TRPO extraction and for the separation of Np by TTA-TiOA extraction have been developed, by which the recovery of Np, Pu and Am is 97%, 99% and 99%, respectively, and the decontamination factors for the major fission products ( 90 Sr, 137 Cs etc.) are 10 4 -10 6 . Pulse shape discrimination (PSD) technique has been introduced to liquid scintillation counting, by which the counting efficiency of α-activity is >99% and the rejection of β-counts is >99.95%. This new method, combining extraction and pulse shape discrimination with liquid scintillation technique, has been successfully applied to the assay of Np, Pu and Am in high level radioactive waste. (author) 7 refs.; 7 figs.; 4 tabs

  20. Acid extraction by supported liquid membranes containing basic carriers

    International Nuclear Information System (INIS)

    Danesi, P.R.; Cianetti, C.; Horwitz, E.P.

    1983-01-01

    The extraction of HNO 3 (nitric acid) from aqueous solutions by permeation through a number of supported liquid membranes containing basic carriers dissolved in diethylbenzene has been studied. The results have shown that the best permeations are obtained with long chain aliphatic amines (TLA, Primene JM-T) followed by TOPO (trioctylphosphine oxide) and then by other monofunctional and bifunctional organophosphorous basic carriers. The influence of an aliphatic diluent on the permeability of HNO 3 through a supported liquid membrane containing TLA as carrier was also investigated. In this case the permeability to HNO 3 decreases as a result of the lower diffusion coefficient of the acid-carrier complex in the more vicous aliphatic solvent. 4 figures

  1. Non-porous membrane-assisted liquid-liquid extraction of UV filter compounds from water samples.

    Science.gov (United States)

    Rodil, Rosario; Schrader, Steffi; Moeder, Monika

    2009-06-12

    A method for the determination of nine UV filter compounds [benzophenone-3 (BP-3), isoamyl methoxycinnamate, 4-methylbenzylidene camphor, octocrylene (OC), butyl methoxydibenzoylmethane, ethylhexyl dimethyl p-aminobenzoate (OD-PABA), ethylhexyl methoxycinnamate (EHMC), ethylhexyl salicylate and homosalate] in water samples was developed and evaluated. The procedure includes non-porous membrane-assisted liquid-liquid extraction (MALLE) and LC-atmospheric pressure photoionization (APPI)-MS/MS. Membrane bags made of different polymeric materials were examined to enable a fast and simple extraction of the target analytes. Among the polymeric materials tested, low- and high-density polyethylene membranes proved to be well suited to adsorb the analytes from water samples. Finally, 2 cm length tailor-made membrane bags were prepared from low-density polyethylene in order to accommodate 100 microL of propanol. The fully optimised protocol provides recoveries from 76% to 101% and limits of detection (LOD) between 0.4 ng L(-1) (OD-PABA) and 16 ng L(-1) (EHMC). The interday repeatability of the whole protocol was below 18%. The effective separation of matrix molecules was proved by only marginal matrix influence during the APPI-MS analysis since no ion suppression effects were observed. During the extraction step, the influence of the matrix was only significant when non-treated wastewater was analysed. The analysis of lake water indicated the presence of seven UV filter compounds included in this study at concentrations between 40 ng L(-1) (BP-3) and 4381 ng L(-1) (OC). In non-treated wastewater several UV filters were also detected at concentration levels as high as 5322 ng L(-1) (OC).

  2. Optimization and application of homogeneous liquid-liquid extraction in preconcentration of copper (II) in a ternary solvent system

    Energy Technology Data Exchange (ETDEWEB)

    Farajzadeh, Mir Ali [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)], E-mail: farajzade@yahoo.com; Bahram, Morteza [Department of Chemistry, Faculty of Science, Urmia University, Urmia (Iran, Islamic Republic of); Zorita, Saioa [Department of Analytical Chemistry, University of Lund, P.O. Box 124, 221 00 Lund (Sweden); Mehr, Behzad Ghorbani [Department of Chemistry, Faculty of Science, Urmia University, Urmia (Iran, Islamic Republic of)

    2009-01-30

    In this study a homogeneous liquid-liquid extraction based on the Ph-dependent phase-separation process was investigated using a ternary solvent system (water-acetic acid-chloroform) for the preconcentration of Cu{sup 2+} ions. 8-Hydroxy quinoline was used as the chelating agent prior to its extraction. Flame atomic absorption spectrophotometry using acetylene-air flame was used for the quantitation of analyte after preconcentration. The effect of various experimental parameters in extraction step was investigated using two optimization methods, one variable at a time and central composite design. The experimental design was done at five levels of operating parameters. Nearly the same optimized results were obtained using both methods: sample size, 5 mL; volume of NaOH 10 M, 2 mL; chloroform volume, 300 {mu}L; 8-hydroxy quinoline concentration more than 0.01 M and salt amount did not affect the extraction significantly. Under the optimum conditions the calibration graph was linear over the range 10-2000 {mu}g L{sup -1}. The relative standard deviation was 7.6% for six repeated determinations (C = 500 {mu}g L{sup -1}). Furthermore, the limit of detection (S/N = 3) and limit of quantification (S/N = 10) of the method were obtained as 1.74 and 6 {mu}g L{sup -1}, respectively.

  3. Separation by liquid-liquid extraction of actinides(III) from lanthanides(III) using new molecules: the picolinamides; Separation par extraction liquide-liquide des actinides(III) des lanthanides(III) par de nouvelles molecules: les picolinamides

    Energy Technology Data Exchange (ETDEWEB)

    Cordier, P Y [CEA Marcoule, Departement de Recherche en Retraitement et en Vitrification, 30 - Bagnols-sur-Ceze (France); [Clermont-Ferrand-2 Univ., 63 - Aubiere (France)

    1996-07-01

    In the field of long-lived radionuclides separation from waste generated during spent fuel reprocessing, the picolinamides have been chosen as potential extractants for the selective extraction of actinides (III) from lanthanides (III). The first studies initiated on the most simple molecule of the picolinamide family, namely 2-pyridinecarboxamide, pointed out that in an aqueous media the complexation stability constant between this ligand and Am(III) is roughly 10 times higher than the ones corresponding to Ln(III). The synthesis of lipophilic derivatives of 2-pyridinecarboxamide leaded to extraction experiments. The extraction of metallic cation by lipophilic picolinamides, according to a solvatation mechanism, is strongly dependent on the nature of the amide function: a primary amide function (group I) leads to a good extraction; on the contrary, there is a decrease for secondary (group II) and tertiary (group III) amide functions. From a theoretical point of view, this work leads finally to the following conclusions: confirmation of the importance of the presence of soft donor atoms within the extractants (nitrogen in our case) for An(III)/Ln(III). Also, sensitivity of this soft donor atom regarding the protonation reaction; prevalence in our case of the affinity of the extractant for the metallic cation over the lipophilia of the extractant to ensure good distribution coefficients. The extraction and Am(III)/Ln(III) separation performances of the picolinamides from pertechnetic media leads to the design of a possible flowsheet for the reprocessing of high level liquid waste, with the new idea of an integrated technetium reflux. (author) 105 refs.

  4. 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.

  5. Oxidative desulfurization of dibenzothiophene from model oil using ionic liquids as extracting agent

    Science.gov (United States)

    Taha, Mohd F.; Atikah, N.; Chong, F. K.; Shaharun, Maizatul S.

    2012-09-01

    The oxidative desulfurization of dibenzothiophene (DBT) from model oil (in n-dodecane) was carried out using ionic liquid as the extractant and catalyst, and hydrogen peroxide (H2O2) in combination with acetic acid (CH3COOH) and sulphuric acid (H2SO4) as the oxidant. The ionic liquids used were 1-butyl-3-methylimidazolium octyl sulphate ([Bmim][OcSO4]) and 1-butyl-3-methylimidazolium acetate ([Bmim][Ac]). The effect of the amounts of H2O2 on oxidative desulphurization of model oil was first investigated without the usage of ionic liquids at room temperature. The results indicate that greater amount of H2O2 give higher desulfurization and the maximum desulfurization in this study, i.e. 34 %, was occurred when the molar ratio of H2O2 to sulfur was 5:1. With the usage of ionic liquid and the molar ratio of 5:1 (H2O2:sulfur), the efficiency of DBT removal from model oil was increased significantly in terms of percent removal and removal time. Ionic liquid of [Bmim][OcSO4] performed better than [Bmim][Ac] with 72 % DBT removal. When molar ratio of H2O2 to sulphur was 5:1, volume ratio of ionic liquid to model oil was 1:1 and mixing time was 60 min at room temperature. The results indicate the potential of ionic liquids as the extractant and catalyst for oxidative desulfurization of hydrocarbon fuels.

  6. Effect of anions and cations on liquid extraction of TcO{sub 4} - in ionic liquids; Vplyv anionov a kationov na kvapalinovu extrakciu TcO4 - v ionovych kvapalinach

    Energy Technology Data Exchange (ETDEWEB)

    Suchanek, P.; Galambos, M.; Meciarova, M.; Rajec, P [Univerzita Komenskeho, Prirodovedecka fakulta, Katedra jadrovej chemie, 84215 Bratislava (Slovakia)

    2013-04-16

    An influence of monovalent and divalent cations and anions on an liquid extraction of pertechnetate anion from aqueous media using ionic liquids solubilized in various organic solvents has been studied. Suppression of extraction percentage was obtained with a divalent cations in a compare with monovalent cations showing almost no influence on extraction percentage. In a case of anions, perchlorate anion suppressed the extraction percentage in a highest degree. (authors)

  7. Injection molded lab-on-a-disc platform for screening of genetically modified E. coli using liquid-liquid extraction and surface enhanced Raman scattering

    DEFF Research Database (Denmark)

    Morelli, Lidia; Serioli, Laura; Centorbi, Francesca Alessandra

    2018-01-01

    We present the development of an automated centrifugal microfluidic platform with integrated sample pre-treatment (filtration and liquid-liquid extraction) and detection (SERS-based sensing). The platform consists of eight calibration and four assay modules, fabricated with polypropylene using...... injection molding and bonded with ultrasonic welding. The platform was used for detection of a secondary bacterial metabolite (p-coumaric acid) from bacterial supernatant. The obtained extraction efficiency was comparable to values obtained in batch experiments and the SERS-based sensing showed a good...

  8. O processo de transferência linguística no ambiente multilíngue de aprendizagem de PLE: uma abordagem pragmático-cognitiva

    Directory of Open Access Journals (Sweden)

    Luciana de Fátima do Nascimento

    2017-03-01

    Full Text Available Este artigo analisa pragmático-cognitivamente, sob a perspectiva da Teoria da Relevância (SPERBER; WILSON, 1986/1995, o papel do esforço de processamento cognitivo nas instâncias de transferência linguística identificadas em um contexto multilíngue de aprendizagem de português como língua estrangeira (PLE. As análises foram realizadas a partir de dados de rastreamento ocular e de registro de teclado e mouse, triangulados (ALVES, 2003 com protocolos retrospectivos e com dados do questionário prospectivo. Foi realizado um experimento com participantes estrangeiros, aprendizes de PLE, para investigar as possíveis relações do esforço cognitivo despendido durante o processo de execução de três tarefas em língua portuguesa com transferências linguísticas ocorridas na produção de PLE. Os resultados mostraram que, durante a execução das três tarefas, o processo de transferências linguísticas ocorridas nesse ambiente de interação multilíngue pode estar relacionado ao esforço cognitivo despendido na produção textual em língua portuguesa.

  9. 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.

  10. [Determination of fatty acid esters of chloropropanediols in diet samples by gas chromatography-mass spectrometry coupled with solid-supported liquid-liquid extraction].

    Science.gov (United States)

    Gao, Jie; Liu, Qing; Han, Feng; Miao, Hong; Zhao, Yunfeng; Wu, Yongning

    2014-05-01

    To establish a method for the determination of fatty acid esters of 3-monochloropropane-1, 2-diol (3-MCPD) and 2-monochloropropane-1, 3-diol (2-MCPD) in diet samples by gas chromatography-mass spectrometry (GC-MS) with solid-supported liquid-liquid extraction (SLE). Diet samples were ultrasonically extracted by hexane, followed by ester cleavage reaction with sodium methylate in methanol, and then purified by solid-supported liquid-liquid extraction. (SLE) using diatomaceous earth as the sorbent. After derivatization with heptafluorobutyrylimidazole, the analytes were detected by GC-MS and quantified by the deuterated internal standards. The limits of detection (LODs) of 3-MCPD esters and 2-MCPD esters in different diet samples were 0.002 - 0.005 mg/kg and 0.002 - 0.006 mg/kg. The average recoveries of 3-MCPD esters and 2-MCPD esters at the spiking levels of 0.05 and 0.1 mg/kg in the diet samples were in the range of 65.9% - 104.2% and 75.4% - 118.0%, respectively, with the relative standard deviations in the range of 2.2% - 14.2% and 0.8% - .13.9%. The method is simple, accurate and rugged for the determination of fatty acid esters of 3-MCPD and 2-MCPD in diet samples.

  11. Self-Reported Learning Effects of a Tagging Activity Carried out in a Personal Learning Environment (PLE) by Secondary-School Pupils

    NARCIS (Netherlands)

    Verpoorten, Dominique; Glahn, Christian; Chatti, Amine; Westera, Wim; Specht, Marcus

    2011-01-01

    Verpoorten, D., Glahn, C., Chatti, A., Westera, W., & Specht, M. (2011). Self-Reported Learning Effects of a Tagging Activity Carried out in a Personal Learning Environment (PLE) by Secondary-School Pupils. International Journal for Cross-Disciplinary Subjects in Education, 2(1), 276-284.

  12. Continuous extraction of molten chloride salts with liquid cadmium alloys

    International Nuclear Information System (INIS)

    Chow, L.S.; Basco, J.K.; Ackerman, J.P.; Johnson, T.R.

    1993-01-01

    A pyrochemical method is being developed at Argonne National Laboratory (ANL) to provide contnuous multistage extractions between molten chloride salts and liquid cadmium alloys at 500 degrees C. The extraction method will be used to recover transuranic (TRU) elements from the process salt in the electroretiner used in the pyrochemical reprocessing of spent fuel from the Integral Fast Reactor (IFR). The IFR is one of the Department of Energy's advanced power reactor concepts. The recovered TRU elements are returned to the electrorefiner. The extracted salt undergoes further processing to remove rare earths and other fission products so that most of the purified salt can also be returned to the electrorefiner, thereby extending the useful life of the process salt many times

  13. Conceptual process design and economic analysis of a process based on liquid-liquid extraction for the recovery of glycols from aqueous streams

    NARCIS (Netherlands)

    Garcia Chavez, L.Y.; Schuur, Boelo; de Haan, A.B.

    2013-01-01

    The recovery of monoethylene glycol (MEG) and 1,2-propylene glycol (PG) from aqueous streams via liquid–liquid extraction (LLE) using a tailor-made ionic liquid [TOA MNaph] is evaluated as an alternative technology to conventional triple effect evaporation of water. In this paper, the conceptual

  14. Reactive liquid/liquid extraction of heavy metals from landfill seepage waters. Its characterisation and application

    International Nuclear Information System (INIS)

    Woller, N.

    1994-06-01

    This study demonstrates the applicability of liquid-liquid extraction by means of the commercial complexers LIX26 R and LIX84 R to heavy metal removal from waste waters. The composition of this oil-soluble complex is MeR 2 , where Me denotes Hg 2+ , Cd 2+ , Zn 2+ , Cu 2+ , and Ni 2+ , and R denotes LIX84 R . This composition makes the complex electrically neutral, and all polar groups are located inside the molecule. The extraction efficiency of the complexer LIX84 R for the various metal ions is evident in the succession Cu 2+ , Ni 2+ >> Zn 2+ > Hg 2+ > Cd 2+ . These heavy metal ions are even readily extractable at chloride concentrations of up to 1 mol/l. As the structure of the complexer is that of an oil-soluble surfactant with complexing properties, it accumulates at the phase boundary between oil and water. Measurement of interfacial tension in various solvent systems showed that the polar solvent chloroform permits only a weak accumulation of the complexer (400 nmol/m 2 ), whereas the unpolar solvent kerosine permits greater accumulation specifically on the water side of the phase boundary (1958 nmol/m 2 ). Organic solvents solvate the complexer so well, that it is even removed from the air side of the phase boundary. The differing accumulation of the complexer at the water/oil phase boundary explains the differing increase of phase separation time for polar and unpolar solvents. (orig.) [de

  15. Ionic liquid-modified materials for solid-phase extraction and separation: a review.

    Science.gov (United States)

    Vidal, Lorena; Riekkola, Marja-Liisa; Canals, Antonio

    2012-02-17

    In recent years, materials science has propelled to the research forefront. Ionic liquids with unique and fascinating properties have also left their footprints to the developments of materials science during the last years. In this review we highlight some of their recent advances and provide an overview at the current status of ionic liquid-modified materials applied in solid-phase extraction, liquid and gas chromatography and capillary electrochromatography with reference to recent applications. In addition, the potential of ionic liquids in the modification of capillary inner wall in capillary electrophoresis is demonstrated. The main target material modified with ionic liquids is silica, but polymers and monoliths have recently joined the studies. Although imidazolium is still clearly the most commonly used ionic liquid for the covalently modification of materials, the exploitation of pyridinium and phosphonium will most probably increase in the future. Copyright © 2011 Elsevier B.V. All rights reserved.

  16. Assessment of strobilurin fungicides' content in soya-based drinks by liquid micro-extraction and liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Campillo, Natalia; Iniesta, María Jesús; Viñas, Pilar; Hernández-Córdoba, Manuel

    2015-01-01

    Seven strobilurin fungicides were pre-concentrated from soya-based drinks using dispersive liquid-liquid micro-extraction (DLLME) with a prior protein precipitation step in acid medium. The enriched phase was analysed by liquid chromatography (LC) with dual detection, using diode array detection (DAD) and electrospray-ion trap tandem mass spectrometry (ESI-IT-MS/MS). After selecting 1-undecanol and methanol as the extractant and disperser solvents, respectively, for DLLME, the Taguchi experimental method, an orthogonal array design, was applied to select the optimal solvent volumes and salt concentration in the aqueous phase. The matrix effect was evaluated and quantification was carried out using external aqueous calibration for DAD and matrix-matched calibration method for MS/MS. Detection limits in the 4-130 and 0.8-4.5 ng g(-1) ranges were obtained for DAD and MS/MS, respectively. The DLLME-LC-DAD-MS method was applied to the analysis of 10 different samples, none of which was found to contain residues of the studied fungicides.

  17. The PLE(2)NO self-management and exercise program for knee osteoarthritis: Study Protocol for a Randomized Controlled Trial.

    Science.gov (United States)

    Marconcin, Priscila; Espanha, Margarida; Yázigi, Flávia; Campos, Pedro

    2016-06-07

    International recommendations suggest exercise and self-management programs, including non-pharmacological treatments, for knee osteoarthritis (KOA) because they can benefit pain relief and improve function and exercise adherence. The implementation of a combined self-management and exercise program termed PLE(2)NO may be a good method for controlling KOA symptoms because it encourages the development of self-efficacy to manage the pathology. This study will assess the effects of a self-management and exercise program in comparison to an educational intervention (control program) on symptoms, physical fitness, health-related quality of life, self-management behaviors, self-efficacy, physical activity level and coping strategies. This PLE(2)NO study is a single-blinded, randomized controlled trial of elderly (aged above 60 yrs old) patients with clinical and radiographic KOA. The patients will be allocated into either an educational group (control) or a self-management and exercise group (experimental). All participants will receive a supplement of chondroitin and glucosamine sulfates. This paper describes the protocol that will be used in the PLE(2)NO program. This program has several strengths. First, it involves a combination of self-management and exercise approaches, is available in close proximity to the patients and occurs over a short period of time. The latter two characteristics are crucial for maintaining participant adherence. Exercise components will be implemented using low-cost resources that permit their widespread application. Moreover, the program will provide guidance regarding the effectiveness of using a self-management and exercise program to control KOA symptoms and improve self-efficacy and health-related quality of life. NCT02562833 (09/23/2015).

  18. Hollow fiber liquid-phase microextraction of cadmium(II) using an ionic liquid as the extractant

    International Nuclear Information System (INIS)

    Chen, Hui; Wang, Yun; Hu, Yutao; Ni, Liang; Liu, Yingying; Kang, Wenbing; Liu, Yan; Han, Juan

    2014-01-01

    A method is presented for hollow fiber liquid-phase microextraction (HF-LPME) of cadmium(II), which is chelated with 1-(2-pyridylazo)-2-naphthol (PAN) to obtain a hydrophobic complex which then is extracted into a polypropylene hollow fiber containing an ionic liquid in its pores which acts as the membrane phase. EDTA is then injected into the lumen of the membrane as an acceptor phase to trap the analyte. The extraction time (20 min), agitation (400 rpm at 25 °C), pH value (10.0), and the concentrations of PAN (2.5 ng mL −1 ) and EDTA (250 ng mL −1 ) were optimized. With a sample volume of 50 mL and a stripping volume of 15 μL, the enrichment factor is 162. Cadmium(II) was then quantified by graphite furnace AAS. The limit of detection is 0.12 pg mL −1 , the relative standard deviation is 5.2 %, and the linear working range extends from 4 to 45 pg mL −1 . The method was successfully applied to the determination of Cd(II) in environmental and food samples. (author)

  19. Separation of cesium from intermediate level liquid radioactive waste by solvent extraction with antioxidants

    International Nuclear Information System (INIS)

    Gulis, G.

    1989-01-01

    Antioxidants AO 2246, AO 4, AO 4K, AO 301 (Czechoslovakia) and NOCRAC 2246 (Japan) were tested as extracting agents for the separation of cesiium by solvent extraction with substituted phenols. The following effects on extraction were studied: pH of water phase, influence of diluent and of antioxidant concentration, extraction time, influence of salt content. The extraction of cesium from liquid radioactive waste was tested. The best results were obtained by NOCRAC 2246 in nitrobenzene, the extraction efficiency was 92.3% with pH 13.23. (author) 7 refs.; 5 figs.; 4 tabs

  20. The solid-liquid extraction separation of lithium isotopes by porous composite materials doped with ionic liquids and 2,2'-binaphthyldiyl-17-crown-5

    International Nuclear Information System (INIS)

    Xiao-Li Sun; Ling Gu; Dan Qiu; Dong-Hong Ren; Zaijun Li; Zhi-Guo Gu; Jiangnan University, Wuxi

    2015-01-01

    A green and efficient solid-liquid extraction method of lithium isotopes separation by porous composite materials doped with imidazolium ionic liquids and 2,2'-binaphthyldiyl-17-crown-5 has been reported in this paper. The composite materials of mesoporous silica and impregnated resin were synthesized by sol-gel and direct impregnation process, respectively. Various extraction parameters such as the concentration of lithium salt, anion of lithium salt, initial pH, time and temperature were investigated. Under optimized conditions, the maximum single-stage separation factor of 6 Li/ 7 Li was 1.048 ± 0.002, the maximum extraction efficiency was 15.86 %. The sorbents can be regenerated easily with HCl solution and reused repeatedly. (author)

  1. Determination of a metabolite of nifursol in foodstuffs of animal origin by liquid-liquid extraction and liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Wang, Chuanxian; Qu, Li; Liu, Xia; Zhao, Chaomin; Zhao, Fengjuan; Huang, Fuzhen; Zhu, Zhenou; Han, Chao

    2017-02-01

    An analytical method has been developed for the detection of a metabolite of nifursol, 3,5-dinitrosalicylic acid hydrazide, in foodstuffs of animal origin (chicken liver, pork liver, lobster, shrimp, eel, sausage, and honey). The method combines liquid chromatography and tandem mass spectrometry with liquid-liquid extraction. Samples were hydrolyzed with hydrochloric acid and derivatized with 2-nitrobenzaldehyde at 37°C for 16 h. The solutions of derivatives were adjusted to pH 7.0-7.5, and the metabolite was extracted with ethyl acetate. 3,5-Dinitrosalicylic acid hydrazide determination was performed in the negative electrospray ionization method. Both isotope-labeled internal standard and matrix-matched calibration solutions were used to correct the matrix effects. Limits of quantification were 0.5 μg/kg for all samples. The average recoveries, measured at three concentration levels (0.5, 2.0, and 10 μg/kg) were in the range of 75.8-108.4% with relative standard deviations below 9.8%. The developed method exhibits a high sensitivity and selectivity for the routine determination and confirmation of the presence of a metabolite of nifursol in foodstuffs of animal origin. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Recent developments in the extraction separation method for treatment of high-level liquid waste

    International Nuclear Information System (INIS)

    Jiao Rongzhou; Song Chongli; Zhu Yongjun

    2000-01-01

    A description and review of the recent developments in the extraction separation method for partitioning transuranium elements from high-level liquid waste (HLLW) is presented. The extraction separation processes such as TRUEX process, DIAMEX process, DIDPA process, CTH process, TRPO process are briefly discussed

  3. Deterpenation of eucalyptus essential oil by liquid + liquid extraction: Phase equilibrium and physical properties for model systems at T = 298.2 K

    International Nuclear Information System (INIS)

    Gonçalves, Daniel; Koshima, Cristina Chiyoda; Nakamoto, Karina Thiemi; Umeda, Thayla Karla; Aracava, Keila Kazue; Gonçalves, Cintia Bernardo; Rodrigues, Christianne Elisabete da Costa

    2014-01-01

    Highlights: • Fractionation of essential oil compounds. • Liquid + liquid equilibria of limonene, citronellal, ethanol and water were studied. • Distribution coefficients of limonene and citronellal were evaluated. • Densities and viscosities of the phases were experimentally determined. • Solvent selectivities and physical properties were dependent on citronellal and water mass fractions. -- Abstract: As the principal source in Brazil of eucalyptus essential oil extracts, Eucalyptus citriodora contains citronellal, an oxygenated compound responsible for the flavour characteristics. Deterpenation processes, consisting of the removal of terpenic hydrocarbons with the subsequent concentration of the oxygenated compounds, can be used to improve the aromatic characteristics of this essential oil. The purpose of this work was to perform a study of the technical feasibility of using a liquid + liquid extraction process to deterpenate eucalyptus essential oil. Model systems with various mixtures of limonene and citronellal (representing eucalyptus essential oil) as well as solvent (ethanol with various water mass fractions) were used to obtain liquid + liquid equilibrium data. The raffinate and extract phases were also analyzed to characterize the physical properties (density and viscosity). The equilibrium data were used to adjust the NRTL and UNIQUAC parameters. Two empirical models, the simple mixing rule and the Grunberg–Nissan model, were evaluated for use in the descriptions of the densities and viscosities, respectively, of the samples. Increasing the water content in the solvent resulted in decreases in the limonene and citronellal distribution coefficients, with consequential increases in the solvent selectivity values. Increasing values of the densities and viscosities, especially for the solvent-rich phases, were associated with systems using high amounts of hydrated ethanolic solvents

  4. Selective extraction and recovery of rare earth metals from phosphor powders in waste fluorescent lamps using an ionic liquid system.

    Science.gov (United States)

    Yang, Fan; Kubota, Fukiko; Baba, Yuzo; Kamiya, Noriho; Goto, Masahiro

    2013-06-15

    The recycling of rare earth metals from phosphor powders in waste fluorescent lamps by solvent extraction using ionic liquids was studied. Acid leaching of rare earth metals from the waste phosphor powder was examined first. Yttrium (Y) and europium (Eu) dissolved readily in the acid solution; however, the leaching of other rare earth metals required substantial energy input. Ionization of target rare earth metals from the waste phosphor powders into the leach solution was critical for their successful recovery. As a high temperature was required for the complete leaching of all rare earth metals, ionic liquids, for which vapor pressure is negligible, were used as an alternative extracting phase to the conventional organic diluent. An extractant, N, N-dioctyldiglycol amic acid (DODGAA), which was recently developed, showed a high affinity for rare earth metal ions in liquid-liquid extraction although a conventional commercial phosphonic extractant did not. An effective recovery of the rare earth metals, Y, Eu, La and Ce, from the metal impurities, Fe, Al and Zn, was achieved from the acidic leach solution of phosphor powders using an ionic liquid containing DODGAA as novel extractant system. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. Entropy feature extraction on flow pattern of gas/liquid two-phase flow based on cross-section measurement

    International Nuclear Information System (INIS)

    Han, J; Dong, F; Xu, Y Y

    2009-01-01

    This paper introduces the fundamental of cross-section measurement system based on Electrical Resistance Tomography (ERT). The measured data of four flow regimes of the gas/liquid two-phase flow in horizontal pipe flow are obtained by an ERT system. For the measured data, five entropies are extracted to analyze the experimental data according to the different flow regimes, and the analysis method is examined and compared in three different perspectives. The results indicate that three different perspectives of entropy-based feature extraction are sensitive to the flow pattern transition in gas/liquid two-phase flow. By analyzing the results of three different perspectives with the changes of gas/liquid two-phase flow parameters, the dynamic structures of gas/liquid two-phase flow is obtained, and they also provide an efficient supplementary to reveal the flow pattern transition mechanism of gas/liquid two-phase flow. Comparison of the three different methods of feature extraction shows that the appropriate entropy should be used for the identification and prediction of flow regimes.

  6. Simultaneous determination of four trace estrogens in feces, leachate, tap and groundwater using solid-liquid extraction/auto solid-phase extraction and high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Liu, Na; Shi, Yue-e; Li, Mengyan; Zhang, Ting-di; Gao, Song

    2015-10-01

    A simple and selective high-performance liquid chromatography method coupled with fluorescence detection was developed for the simultaneous measurement of trace levels of four estrogens (estrone, estradiol, estriol and 17α-ethynyl estradiol) in environmental matrices. For feces samples, solid-liquid extraction was applied with a 1:1 v/v mixture of acetonitrile and ethyl acetate as the extraction solvent. For liquid samples (e.g., leachate and groundwater), hydrophobic/lipophilic balanced automated solid-phase extraction disks were selected due to their high recoveries compared to conventional C18 disks. Chromatographic separations were performed on a reversed-phase C18 column gradient-eluted with a 45:55 v/v mixture of acetonitrile and water. The detection limits were down to 1.1 × 10(-2) (estrone), 4.11 × 10(-4) (estradiol), 5.2 × 10(-3) (estriol) and 7.18 × 10(-3) μg/L (17α-ethynyl estradiol) at excitation/emission wavelengths of 288/310 nm, with recoveries in the range of 96.9 ± 3.2-105.4 ± 3.2% (n = 3). The method was successfully applied to determine estrogens in feces and water samples collected at livestock farms and a major river in Northeast China. We observed relatively high abundance and widespread distribution of all four estrogens in our sample collections, implying the urgency for a comprehensive and intricate investigation of estrogenic fate and contamination in our researched area. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. 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.

  8. Studies on Three Liquid Phase Extraction (TLPE) system for separation of rare earths

    International Nuclear Information System (INIS)

    Yadav, Kartikey K.; Singh, D.K.; Anitha, M.; Singh, H.

    2014-01-01

    Three-liquid-phase extraction (TLPE) is relatively a new separation technique, which takes the advantage of the differences in physicochemical properties of three coexisted phases to achieve multi-phase liquid separation of two or more components in one-step extraction. TLPE system consists of three liquid layers namely an organic solvent phase (organophosphorous type) and two aqueous phases one rich in polymer phase (poly alkylene glycol) and other a salt solution. To study the feasibility of using such system for separation of rare earths, it is important to optimize the preparatory conditions by selective suitable polymer and salt solutions at an appropriate pH to obtain a stable three phase layers to effect the separation. D2EHPA (di-2-ethyl hexyl phosphoric acid) is a well- established extractant in the rare earth industry and has been chosen in the present work to form a TLPE with polymer and salt solution. In the present investigation after preparing the stable three phase, the feasibility of using TLPE has been examined to separate rare earths from a multicomponent solutions. This study has demonstrated the ability of TLPE having D2EHPA as organic phase to separate rare earths from a multicomponent system. Effect of pH, concentration and types of polymer, complexing agent and D2EHPA concentration has been studied. Variation in pH study indicated that 4.0 leads to extraction of rare earths in the polymer phase. PEG 600 was found to be best amongst the polymer investigated. Presence of DTPA as complexing agent in the salt solution having pH >4.0 resulted in enhanced extraction of rare earths in PEG phase

  9. Role of an ionic liquid, 1-butyl-3-methylimidazolium 2-(2-methoxyethoxy)ethyl sulfate in extraction studies of gadolinium oxide

    Energy Technology Data Exchange (ETDEWEB)

    Sen, Kamalika [Calcutta Univ., Kolkata (India). Dept. of Chemistry; Wolterbeek, H.T. [Technical Univ. Delft (NL). Section RIH (Radiation and Isotopes in Health)

    2012-07-01

    The room temperature ionic liquid (RTIL), 1-butyl-3-methylimidazolium 2-(2-methoxyethoxy)ethyl sulfate was studied for its extraction behavior for {sup 159}Gd in an environmentally benign liquid-liquid extraction system. The gadolinium oxide when dissolved in nitric acid and extracted in an RTIL/dextran biphasic system, was found to get completely extracted in the IL phase. The otherwise difficult to dissolve gadolinium oxide was found to have some solubility in the IL studied. Biphasic systems consisting of IL/dextran and certain IL/salt were studied for the extraction behavior of Gd{sub 2}O{sub 3} dissolved in the above RTIL. A similar experiment was also done with acid-dissolved gadolinium oxide for comparison. (orig.)

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

    Science.gov (United States)

    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.

  11. 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)

  12. Vacuum sieve tray for tritium extraction from liquid Pb-17Li

    Energy Technology Data Exchange (ETDEWEB)

    Okino, Fumito, E-mail: fumito.okino@iae.kyoto-u.ac.jp [Graduate School of Energy Science, Kyoto University, Uji, Kyoto 611-0011 (Japan); Noborio, Kazuyuki [Institute of Sustainability Science, Kyoto University, Uji, Kyoto 611-0011 (Japan); Yamamoto, Yasushi [Faculty of Engineering Science, Kansai University, 3-3-35 Suita-shi, Osaka 564-8680 (Japan); Konishi, Satoshi [Institute of Advanced Energy, Kyoto University, Uji, Kyoto 611-0011 (Japan)

    2012-08-15

    Formation of droplet of liquid Li-17Pb released from a nozzle into vacuum was studied for the evaluation of the feasibility as a tritium extraction process. Size of droplets formed from the nozzles was estimated by theoretical and experimental methods. For the theoretical estimation, the non-dimensional comparison of the physical bulk property of liquid Pb-17Li with water (H{sub 2}O) at ambient temperature was applied. It was found to be reasonable to apply the Plateau-Rayleigh-Instability theory for the droplet size formula of the fluid Pb-17Li for the nozzle diameter 0.4 mm-1.0 mm, temperature 400 Degree-Sign C-500 Degree-Sign C, at initial velocity of 3 m/s. The experimental results of the droplet size showed good agreement with the theory. This device was used for the parametric study of extraction of deuterium during their free fall in vacuum. The scaling of the device suggests the engineering feasibility of the process.

  13. Determination of trace bisphenol A in environmental water by high-performance liquid chromatography using magnetic reduced graphene oxide based solid-phase extraction coupled with dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Li, Danping; Ma, Xiaoguo; Wang, Rui; Yu, Yumian

    2017-02-01

    Bisphenol A (BPA), an endocrine-disrupting chemical, has received much attention from researchers and the general public. In this paper, a novel method of determining BPA at trace levels was developed, using magnetic reduced graphene oxide (rGO-Fe 3 O 4 )-based solid-phase extraction coupled with dispersive liquid-liquid microextraction (DLLME), followed by high-performance liquid chromatographic determination. The rGO-Fe 3 O 4 was prepared and then characterized by Fourier transform infrared spectroscopy, transmission electron microscopy, and vibrating sample magnetometry. The greatest saturation magnetization of rGO-Fe 3 O 4 was up to 43.8 emu g -1 , which allowed rapid isolation of the rGO-Fe 3 O 4 from solutions upon applying an appropriate magnetic field. The effects of solution pH, adsorbent amount, type and volume of eluent and extraction solvent, extraction time, and salt concentration on the extraction efficiency of BPA were examined and optimized. Under the optimum conditions, an enrichment factor of 5217 and an LOD of 0.01 μg L -1 for BPA were obtained. The reusability of rGO-Fe 3 O 4 for at least 12 repeated cycles without any significant decrease in the extraction recovery of BPA was demonstrated. The proposed method was applied to the determination of BPA in different real water samples, with relative recoveries of 84.8-104.9 % and RSDs of 0.8-8.3 % in the spiked concentration range 1-10 μg L -1 .

  14. Liquid metal extraction of Nd from NdFeB magnet scrap

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Yanchen [Iowa State Univ., Ames, IA (United States)

    1999-12-10

    This research involves using molten magnesium (Mg) to remove neodymium (Nd) from NdFeB magnet scrap by diffusion. The results show that liquid metal extraction of Nd may be a viable and inexpensive method for recovering the expensive rare earth element Nd for use in Mg castings.

  15. In situ derivatization-liquid liquid extraction as a sample preparation strategy for the determination of urinary biomarker prolyl-4-hydroxyproline by liquid chromatography-tandem mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Cimlová, Jana; Kružberská, Pavla; Švagera, Z.; Hušek, Petr; Šimek, Petr

    2012-01-01

    Roč. 47, č. 3 (2012), s. 294-302 ISSN 1076-5174 R&D Projects: GA ČR GA203/09/2014; GA MZd NS9755; GA MŠk 7F09028 Institutional research plan: CEZ:AV0Z50070508 Keywords : alkyl chloroformate derivatization * liquid liquid extraction * urine Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.214, year: 2012 http://onlinelibrary.wiley.com/doi/10.1002/jms.2952/full

  16. 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...

  17. Ionic Liquids as Benign Solvents for the Extraction of Aromatics

    International Nuclear Information System (INIS)

    Hossain, Md. Anwar; Lee, Jeesun; Kim, Dai Hyun; Nguyen, Dinh Quan; Cheong, Minserk; Kim, Hoon Sik

    2012-01-01

    Ionic liquids (ILs) have been extensively investigated as promising alternatives to conventional organic solvents such as sulfolane and N,N-dimethylformamide for the selective extraction of aromatic hydrocarbons from the C 6 -C 10 hydrocarbon mixtures produced from the cracking processes of naphtha and light oils. The most important advantage of ILs over conventional organic solvents is that they are immiscible with aliphatic hydrocarbons, and thus the back extraction of ILs from the raffinate phases and top hydrocarbon-rich layers is not necessary. In this paper, a brief review on the state of the art in the utilization of ILs for aromatics separation is presented

  18. Radiological objectives and severe accident mitigation strategy for the generation II PWRs in France in the framework of PLE

    International Nuclear Information System (INIS)

    Cenerino, G.; Dubreuil, M.; Raimond, E.; Pichereau, F.

    2012-01-01

    In France, EDF is involved in the construction of a first generation III (Gen III) reactor (European Pressurized Reactor - EPR) on Flamanville site next to two PWRs. Plant Life Extension (PLE) of reactors will consequently lead to simultaneous operation of Gen III and Gen II reactors during a long period of time. As a consequence, EDF was requested by the French Nuclear Safety Authority to prepare a PWR life management program including, in addition to an ageing management of Systems, Structures and Components, a consequent reactor safety enhancement program. The objective was stated to EDF by the French Nuclear Safety Authority: 'the safety objectives of the Gen III reactors should be used as a reference for all studies undertaken in the frame of PLE'. One part of the EDF program deals with additional arrangements able to reduce more drastically the consequences of any accident. The relevance, according to IRSN, of the EDF radiological objectives for Design Basis Accidents, of the new EDF objectives for Severe Accidents (SA) and of the EDF potential modifications for SA mitigation are presented. (author)

  19. HPLC/Fluorometric Detection of Carvedilol in Real Human Plasma Samples Using Liquid-Liquid Extraction.

    Science.gov (United States)

    Yilmaz, Bilal; Arslan, Sakir

    2016-03-01

    A simple, rapid and sensitive high-performance liquid chromatography (HPLC) method has been developed to quantify carvedilol in human plasma using an isocratic system with fluorescence detection. The method included a single-step liquid-liquid extraction with diethylether and ethylacetate mixture (3 : 1, v/v). HPLC separation was carried out by reversed-phase chromatography with a mobile phase composed of 20 mM phosphate buffer (pH 7)-acetonitrile (65 : 35, v/v), pumped at a flow rate of 1.0 mL/min. Fluorescence detection was performed at 240 nm (excitation) and 330 nm (emission). The calibration curve for carvedilol was linear from 10 to 250 ng/mL. Intra- and interday precision values for carvedilol in human plasma were plasma averaged out to 91.8%. The limits of detection and quantification of carvedilol were 3.0 and 10 ng/mL, respectively. Also, the method was successfully applied to three patients with hypertension who had been given an oral tablet of 25 mg carvedilol. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  20. Inhibitory activities of Perilla frutescens britton leaf extract against the growth, migration, and adhesion of human cancer cells

    Science.gov (United States)

    Kwak, Youngeun

    2015-01-01

    BACKGROUND/OBJECTIVES Perilla frutescens Britton leaves are a commonly consumed vegetable in different Asian countries including Korea. Cancer is a major cause of human death worldwide. The aim of the current study was to investigate the inhibitory effects of ethanol extract of perilla leaf (PLE) against important characteristics of cancer cells, including unrestricted growth, resisted apoptosis, and activated metastasis, using human cancer cells. MATERIALS/METHODS Two human cancer cell lines were used in this study, HCT116 colorectal carcinoma cells and H1299 non-small cell lung carcinoma cells. Assays using 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide were performed for measurement of cell growth. Soft agar and wound healing assays were performed to determine colony formation and cell migration, respectively. Nuclear staining and cell cycle analysis were performed for assessment of apoptosis. Fibronectin-coated plates were used to determine cell adhesion. RESULTS Treatment of HCT116 and H1299 cells with PLE resulted in dose-dependent inhibition of growth by 52-92% (at the concentrations of 87.5, 175, and 350 µg/ml) and completely abolished the colony formation in soft agar (at the concentration of 350 µg/ml). Treatment with PLE at the 350 µg/ml concentration resulted in change of the nucleus morphology and significantly increased sub-G1 cell population in both cells, indicating its apoptosis-inducing activity. PLE at the concentration range of 87.5 to 350 µg/ml was also effective in inhibiting the migration of H1299 cells (by 52-58%) and adhesion of both HCT116 and H1299 cells (by 25-46%). CONCLUSIONS These results indicate that PLE exerts anti-cancer activities against colon and lung cancers in vitro. Further studies are needed in order to determine whether similar effects are reproduced in vivo. PMID:25671062

  1. Influence of ionic liquids on actinides extraction by diphenyl(dibutyl)carbamoylmethylphosphine oxide in different solvents from nitric acid solution

    International Nuclear Information System (INIS)

    Pribylova, G.A.

    2011-01-01

    Influence of ionic liquids (ILs) addition (1-50 wt%) on extraction efficiency of actinides by diphenyl(dibutyl)carbamoylmethylphosphine oxide (Ph 2 Bu 2 ) from 3 M HNO 3 has been studied. Am(III) distribution ratios in two-phase systems 0.1 M Ph 2 Bu 2 in either DCE or CHCl 3 -3 M HNO 3 depending on the nature of additional ionic liquids: imidazolium-based ILs: [C 4 mim][PF 6 ], [C 4 mim][BF 4 ] and phosphonium-based ILs: PPF 6 , PBF 4 and PCl were determined. The highest value of Am(III) extraction ratio change (1040) was found on addition of PPF 6 to Ph 2 Bu 2 in CHCl 3 . Extraction of Pu(IV) and U(VI) by 0.001 M Ph 2 Bu 2 in the presence of [C 4 mim][PF 6 ] in DCE, CHCl 3 or meta-nitrobenzotrifluoride (NBTF) have been investigated. The greatest enhancement of extraction efficiency was observed using CHCl 3 , the least polar studied solvent. Using a mixture of conventional solvent and ionic liquid as a solvent for extractant enables one to increase distribution ratios and reduce viscosity of organic phase as compared with ionic liquid viscosity. The marked increase of Am(III), Pu(IV) and U(VI) extraction extent by Ph 2 Bu 2 on addition of ionic liquids to the extent of 10 wt% permit one essentially to diminish amounts considerably more expensive carbamoylmethylphosphine oxide(the general name is CMPO) used in TRUEX process. (author)

  2. Development of a surfactant liquid membrane extraction process for the cleansing of industrial aqueous effluents containing metallic cation traces

    International Nuclear Information System (INIS)

    Rapaumbya Akaye, Guy-Roland

    1994-01-01

    The purpose of this work was to develop a process of surfactant liquid membrane extraction to purify industrial waste solution containing Cu(II), Fe(III), and Zn(II) (about 0,1 g/L). The extractant is the ammonium salt of Cyanex 306 and Aliquat 336. The first part of this work deals with the study of the liquid-liquid extraction of the metals. The efficiency of the extractant has been shown for the extraction of each metal alone and for Cu(II) and Zn(II) in the case of a mixture of the three metals. During this study we have observed that Fe(III) is reduced to Fe(II) (which is not extracted by the salt of Cyanex 301) in presence of Cu(II) and the quaternary ammonium salt (Aliquat 336). The optimisation of the experimental conditions for the discontinuous surfactant liquid membrane process led us to choose the following composition of the emulsion: 1,5 % of Cyanex 301 salt, 2,5 % of ECA 4360, dodecan. The internal phase is an aqueous solution containing 3,5 mol/L of NaOH and 0,5 mol/L tri-ethanolamin The residual concentration of Cu(II) and Zn(II) in the external phase is very low. In the case of iron, only 60 % are extracted because of the reduction phenomenon (10 % in liquid-liquid extraction). The realisation of the continuous process in pulsed column, after optimisation of hydrodynamics conditions, leads to similar results. In stationary conditions, we obtain a raffinate containing less than 0,5 mg/L of Cu(II) and Zn(II) and 36 mg/L of iron. The internal phase contains about 2 g/L of Cu(II) an Zn(II). We tried and minimize the reduction of Fe(III) in surfactant liquid membrane process. Less than 16 % of iron cannot be reduced. This leads to a purification of only 84 % In the basis of these results, processes of purification have been proposed for effluents of various composition. They enable to purify the effluent and besides to concentrate the pollutants about twenty times. (author) [fr

  3. Solvent extraction of gold using ionic liquid based process

    Science.gov (United States)

    Makertihartha, I. G. B. N.; Zunita, Megawati; Rizki, Z.; Dharmawijaya, P. T.

    2017-01-01

    In decades, many research and mineral processing industries are using solvent extraction technology for metal ions separation. Solvent extraction technique has been used for the purification of precious metals such as Au and Pd, and base metals such as Cu, Zn and Cd. This process uses organic compounds as solvent. Organic solvents have some undesired properties i.e. toxic, volatile, excessive used, flammable, difficult to recycle, low reusability, low Au recovery, together with the problems related to the disposal of spent extractants and diluents, even the costs associated with these processes are relatively expensive. Therefore, a lot of research have boosted into the development of safe and environmentally friendly process for Au separation. Ionic liquids (ILs) are the potential alternative for gold extraction because they possess several desirable properties, such as a the ability to expanse temperature process up to 300°C, good solvent properties for a wide range of metal ions, high selectivity, low vapor pressures, stability up to 200°C, easy preparation, environmentally friendly (commonly called as "green solvent"), and relatively low cost. This review paper is focused in investigate of some ILs that have the potentials as solvent in extraction of Au from mineral/metal alloy at various conditions (pH, temperature, and pressure). Performances of ILs extraction of Au are studied in depth, i.e. structural relationship of ILs with capability to separate Au from metal ions aggregate. Optimal extraction conditon in order to gain high percent of Au in mineral processing is also investigated.

  4. Ionic liquid-based microwave-assisted extraction of essential oil and biphenyl cyclooctene lignans from Schisandra chinensis Baill fruits.

    Science.gov (United States)

    Ma, Chun-hui; Liu, Ting-ting; Yang, Lei; Zu, Yuan-gang; Chen, Xiaoqiang; Zhang, Lin; Zhang, Ying; Zhao, Chunjian

    2011-12-02

    Ionic liquid-based microwave-assisted extraction (ILMAE) has been successfully applied in extracting essential oil and four kinds of biphenyl cyclooctene lignans from Schisandra chinensis Baill. 0.25 M 1-lauryl-3-methylimidazolium bromide ionic liquid is selected as solvent. The optimum parameters of dealing with 25.0 g sample are 385 W irradiation power, 40 min microwave extraction time and 1:12 solid-liquid ratio. The yields of essential oil and lignans are 12.12±0.37 ml/kg and 250.2±38.2 mg/kg under the optimum conditions. The composition of the essential oil extracted by hydro-distillation, steam-distillation and ILMAE is analyzed by GC-MS. With ILMAE method, the energy consumption time has not only been shortened to 40 min (hydro-distillation 3.0 h for extracting essential oil and reflux extraction 4.0 h for extracting lignans, respectively), but also the extraction efficiency has been improved (extraction of lignans and distillation of essential oil at the same time) and reduces the environmental pollution. S. chinensis materials treated by different methods are observed by scanning electronic microscopy. Micrographs provide more evidence to prove that ILMAE is a better and faster method. The experimental results also indicate that ILMAE is a simple and efficient technique for sample preparation. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. Determination of flumequine and oxolinic acid in sediments and soils by microwave-assisted extraction and liquid chromatography-fluorescence

    International Nuclear Information System (INIS)

    Prat, M.D.; Ramil, D.; Compano, R.; Hernandez-Arteseros, J.A.; Granados, M.

    2006-01-01

    A method is reported for the determination of the quinolones oxolinic acid and flumequine in aquatic sediments and agricultural soils. The analytes are extracted by liquid-liquid partitioning between a sample homogenated in an aqueous buffer solution and dichloromethane. Microwave-assisted extraction (MAE) was tested to improve the speed and efficiency of the extraction process. The parameters affecting the efficiency of MAE, such as irradiation time and temperature, were studied. The clean-up consists of back-extraction in 1 M sodium hydroxide. The determination is carried out by reversed phase liquid chromatography on an octyl silica-based column and fluorimetric detection. The optimised method was applied to the analysis of two sediments and one agricultural soil spiked with the analytes. The absolute recovery rates for the whole process range from 79% to 94% (RSD 3-7%), and detection limits are in the low μg kg -1 level

  6. Liquid Membrane System for Extraction and Electrodeposition of Lead(II During Electrodialysis

    Directory of Open Access Journals (Sweden)

    Sadyrbaeva Tatiana

    2017-05-01

    Full Text Available A novel method for lead(II removal from aqueous acidic solutions is presented. The method involves electrodialysis through bulk liquid membranes accompanied by electrodeposition of metal from the cathodic solution. Solutions of di(2-ethylhexylphosphoric acid with admixtures of tri-n-octylamine in 1,2-dichloroethane were used as the liquid membranes. The effects of the main electrodialysis parameters as well as of the composition of the liquid membranes and aqueous solutions on the lead(II transport rate are studied. The optimal conditions are determined. A possibility of effective single-stage transfer of lead(II through the liquid membrane into dilute solutions of perchloric, nitric and acetic acids is demonstrated. Dense and adherent lead electrodeposits are obtained from perchloric acid solutions. Maximum extraction degree of 93 % and electrodeposition degree of ~60 % are obtained during 5 h of electrodialysis.

  7. Air-assisted liquid-liquid microextraction using floating organic droplet solidification for simultaneous extraction and spectrophotometric determination of some drugs in biological samples through chemometrics methods

    Science.gov (United States)

    Farahmand, Farnaz; Ghasemzadeh, Bahar; Naseri, Abdolhossein

    2018-01-01

    An air assisted liquid-liquid microextraction by applying the solidification of a floating organic droplet method (AALLME-SFOD) coupled with a multivariate calibration method, namely partial least squares (PLS), was introduced for the fast and easy determination of Atenolol (ATE), Propanolol (PRO) and Carvedilol (CAR) in biological samples via a spectrophotometric approach. The analytes would be extracted from neutral aqueous solution into 1-dodecanol as an organic solvent, using AALLME. In this approach a low-density solvent with a melting point close to room temperature was applied as the extraction solvent. The emulsion was immediately formed by repeatedly pulling in and pushing out the aqueous sample solution and extraction solvent mixture via a 10-mL glass syringe for ten times. After centrifugation, the extractant droplet could be simply collected from the aqueous samples by solidifying the emulsion at a lower than the melting point temperature. In the next step, analytes were back extracted simultaneously into the acidic aqueous solution. Derringer and Suich multi-response optimization were utilized for simultaneous optimizing the parameters of three analytes. This method incorporates the benefits of AALLME and dispersive liquid-liquid microextraction considering the solidification of floating organic droplets (DLLME-SFOD). Calibration graphs under optimized conditions were linear in the range of 0.30-6.00, 0.32-2.00 and 0.30-1.40 μg mL- 1 for ATE, CAR and PRO, respectively. Other analytical parameters were obtained as follows: enrichment factors (EFs) were found to be 11.24, 16.55 and 14.90, and limits of detection (LODs) were determined to be 0.09, 0.10 and 0.08 μg mL- 1 for ATE, CAR and PRO, respectively. The proposed method will require neither a highly toxic chlorinated solvent for extraction nor an organic dispersive solvent in the application process; hence, it is more environmentally friendly.

  8. Liquid and solid self-microemulsifying drug delivery systems for improving the oral bioavailability of andrographolide from a crude extract of Andrographis paniculata.

    Science.gov (United States)

    Sermkaew, Namfa; Ketjinda, Wichan; Boonme, Prapaporn; Phadoongsombut, Narubodee; Wiwattanapatapee, Ruedeekorn

    2013-11-20

    The purpose of this study was to develop self-microemulsifying formulations of an Andrographis paniculata extract in liquid and pellet forms for an improved oral delivery of andrographolide. The optimized liquid self-microemulsifying drug delivery system (SMEDDS) was composed of A. paniculata extract (11.1%), Capryol 90 (40%), Cremophor RH 40 (40%) and Labrasol (8.9%). This liquid SMEDDS was further adsorbed onto colloidal silicon dioxide and microcrystalline cellulose, and converted to SMEDDS pellets by the extrusion/spheronization technique. The microemulsion droplet sizes of the liquid and pellet formulations after dilution with water were in the range of 23.4 and 30.3 nm. The in vitro release of andrographolide from the liquid SMEDDS and SMEDDS pellets was 97.64% (SD 1.97%) and 97.74% (SD 3.36%) within 15 min, respectively while the release from the initial extract was only 10%. The oral absorption of andrographolide was determined in rabbits. The C(max) value of andrographolide from the A. paniculata extract liquid SMEDDS and SMEDDS pellet formulations (equivalent to 17.5mg/kg of andrographolide) was 6-fold and 5-fold greater than the value from the initial extract in aqueous suspension (equivalent to 35 mg/kg of andrographolide), respectively. In addition, the AUC(0-12h) was increased 15-fold by the liquid SMEDDS and 13-fold by the SMEDDS pellets compared to the extract in aqueous suspension, respectively. The results clearly indicated that the liquid and solid SMEDDS could be effectively used to improve the dissolution and oral bioavailability that would also enable a reduction in the dose of the poorly water soluble A. paniculata extract. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Extraction of triazole fungicides in environmental waters utilizing poly (ionic liquid)-functionalized magnetic adsorbent.

    Science.gov (United States)

    Liu, Cheng; Liao, Yingmin; Huang, Xiaojia

    2017-11-17

    This work prepared a new poly (ionic liquid)-functionalized magnetic adsorbent (PFMA) for the extraction of triazole fungicides (TFs) in environmental waters prior to determination by high performance liquid chromatography/diode array detection (HPLC-DAD). A polymerizable ionic liquid, 1-methyl-3-allylimidazolium bis(trifluoromethylsulfonyl)imide was employed to copolymerize with divinylbenzene on the surface of modified magnetite to fabricate the PFMA. The morphology, spectroscopic and magnetic properties of the new adsorbent were investigated by different techniques. A series of key parameters that influence the extraction performance including the amount of PFMA, desorption solvent, adsorption and desorption time, sample pH value and ionic strength were optimized in detail. Under the optimum conditions, the prepared PFMA could extract targeted TFs effectively and quickly under the format of magnetic solid-phase extraction (MSPE). Satisfactory linearities were achieved in the range of 0.1-200.0μg/L for triadimenol and 0.05-200.0μg/L for other TFs with good coefficients of determination above 0.99 for all analytes. The limits of detection (S/N=3) and limits of quantification (S/N=10) for TFs were in the range of 0.0050-0.0078μg/L and 0.017-0.026μg/L, respectively. Environmental waters including lake, river and well waters were used to demonstrate the applicability of developed MSPE-HPLC-DAD method, and satisfactory recoveries and repeatability were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Salting-Out Assisted Liquid-Liquid Extraction for Quantification of Febuxostat in Plasma Using RP-HPLC and Its Pharmacokinetic Application.

    Science.gov (United States)

    Tandel, Devang; Shah, Purvi; Patel, Kalpana; Thakkar, Vaishali; Patel, Kirti; Gandhi, Tejal

    2016-11-01

    A rapid and sensitive reversed-phase high-performance liquid chromatography (HPLC) method using novel salting-out assisted liquid-liquid extraction technique has been developed for the quantitative determination of febuxostat (FEB), used for the treatment of gout, in rat plasma. The method was validated according to US FDA guideline. Separation was achieved using a Phenomenex Luna-C 18 (250 × 4.60 mm, 5 µm) column and mobile phase composed of potassium dihydrogen orthophosphate buffer 25 mM, adjusted to pH 6.8 with triethylamine:methanol in a ratio of 35:65 (v/v) showing retention time 5.56 and 8.86 min for FEB and internal standard, respectively. The optimal salting-out parameters; 1 mL of acetonitrile and 200 µL of 2 M ammonium acetate salt showed extraction recovery >90% for FEB from plasma. This extraction procedure afforded clear samples resulting in convenient and cost-saving procedure and showed good linear relationship (r > 0.9997) between peak area ratio and concentration from 0.3 to 20 µg/mL. The results of pharmacokinetic study showed that absorption profile of spherical agglomerate of FEB compared to marketed formulation was higher indicating greater systemic absorption. In conclusion, the developed SALLE-HPLC method with simple ultraviolet detection offered a number of advantages including good quantitative ability, wide linear range, high recovery, short analysis time as well as low cost. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  11. Simultaneous extraction and clean-up of polychlorinated biphenyls and their metabolites from small tissue samples using pressurized liquid extraction

    Science.gov (United States)

    Kania-Korwel, Izabela; Zhao, Hongxia; Norstrom, Karin; Li, Xueshu; Hornbuckle, Keri C.; Lehmler, Hans-Joachim

    2008-01-01

    A pressurized liquid extraction-based method for the simultaneous extraction and in situ clean-up of polychlorinated biphenyls (PCBs), hydroxylated (OH)-PCBs and methylsulfonyl (MeSO2)-PCBs from small (< 0.5 gram) tissue samples was developed and validated. Extraction of a laboratory reference material with hexane:dichloromethane:methanol (48:43:9, v/v) and Florisil as fat retainer allowed an efficient recovery of PCBs (78–112%; RSD: 13–37%), OH-PCBs (46±2%; RSD: 4%) and MeSO2-PCBs (89±21%; RSD: 24%). Comparable results were obtained with an established analysis method for PCBs, OH-PCBs and MeSO2-PCBs. PMID:19019378

  12. Fundamental study on the extraction of transuranium elements from high-level liquid waste

    International Nuclear Information System (INIS)

    Kubota, Masumitsu; Morita, Yasuji; Tochiyama, Osamu; Inoue, Yasushi.

    1988-01-01

    A great many extractants have been studied for the separation of transuranium elements. The present study deals with the survey and classification of the extractants appearing in literature, bearing in mind the relationship between the molecular structure of extractants and their extractability for the transuranium elements from the standpoint of their selective separation from high-level liquid waste (HLW) generated from fuel reprocessing. The extractants surveyed were classified into six groups; unidentate neutral organophosphorus compounds, bidentate neutral organophosphorus compounds, acidic organophosphorus compounds, amines and ammonium salts, N,N-disubstituted amides and the other compounds. These extractants are not always applicable to the separation of transuranium elements from HLW because of their limitations in extractability and radiation durability. Only a limited number of extractants belonging to the bidentate neutral organophosphorus compounds and the acidic organophosphorus compounds are considered to be suitable for the present purpose. (author)

  13. Electrochemical assessment of water|ionic liquid biphasic systems towards cesium extraction from nuclear waste.

    Science.gov (United States)

    Stockmann, T Jane; Zhang, Jing; Montgomery, Anne-Marie; Ding, Zhifeng

    2014-04-22

    A room temperature ionic liquid (IL) composed of a quaternary alkylphosphonium (trihexyltetradecylphosphonium, P66614(+)) and tetrakis(pentafluorophenyl)borate anion (TB(-)) was employed within a water|P66614TB (w|P66614TB or w|IL) biphasic system to evaluate cesium ion extraction in comparison to that with a traditional water|organic solvent (w|o) combination. (137)Cs is a major contributor to the radioactivity of spent nuclear fuel as it leaves the reactor, and its extraction efficiency is therefore of considerable importance. The extraction was facilitated by the ligand octyl(phenyl)-N,N'-diisobutylcarbamoylphosphine oxide (CMPO) used in TRans-Uranium EXtraction processes and investigated through well established liquid|liquid electrochemistry. This study gave access to the metal ion to ligand (1:n) stoichiometry and overall complexation constant, β, of the interfacial complexation reaction which were determined to be 1:3 and 1.6×10(11) at the w|P66614TB interface while the study at w|o elicited an n equal to 1 with β equal to 86.5. Through a straightforward relationship, these complexation constant values were converted to distribution coefficients, δ(α), with the ligand concentrations studied for comparison to other studies present in the literature; the w|o and w|IL systems gave δ(α) of 2 and 8.2×10(7), respectively, indicating a higher overall extraction efficiency for the latter. For the w|o system, the metal ion-ligand stoichiometries were confirmed through isotopic distribution analysis of mass spectra obtained by the direct injection of an emulsified water-organic solvent mixture into an electron spray ionization mass spectrometer. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Magnetic graphene oxide modified by imidazole-based ionic liquids for the magnetic-based solid-phase extraction of polysaccharides from brown alga.

    Science.gov (United States)

    Wang, Xiaoqin; Li, Guizhen; Row, Kyung Ho

    2017-08-01

    Magnetic graphene oxide was modified by four imidazole-based ionic liquids to synthesize materials for the extraction of polysaccharides by magnetic solid-phase extraction. Fucoidan and laminarin were chosen as the representative polysaccharides owing to their excellent pharmaceutical value and availability. Fourier transform infrared spectroscopy, field-emission scanning electron microscopy, and thermogravimetric analysis were applied to characterize the synthesized materials. Single-factor experiments showed that the extraction efficiency of polysaccharides was affected by the amount of ionic liquids for modification, solid-liquid ratio of brown alga and ethanol, the stirring time of brown alga and ionic liquid-modified magnetic graphene oxide materials, and amount of 1-(3-aminopropyl)imidazole chloride modified magnetic graphene oxide materials added to the brown alga sample solution. The results indicated that 1-(3-aminopropyl)imidazole chloride modified magnetic graphene oxide possessed better extraction ability than graphene oxide, magnetic graphene oxide, and other three ionic-liquid-modified magnetic graphene oxide materials. The highest extraction recoveries of fucoidan and laminarin extracted by 1-(3-aminopropyl)imidazole chloride modified magnetic graphene oxide were 93.3 and 87.2%, respectively. In addition, solid materials could be separated and reused easily owing to their magnetic properties. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Separation by liquid-liquid extraction of actinides(III) from lanthanides(III) using new molecules: the picolinamides

    International Nuclear Information System (INIS)

    Cordier, P.Y.

    1996-07-01

    In the field of long-lived radionuclides separation from waste generated during spent fuel reprocessing, the picolinamides have been chosen as potential extractants for the selective extraction of actinides (III) from lanthanides (III). The first studies initiated on the most simple molecule of the picolinamide family, namely 2-pyridinecarboxamide, pointed out that in an aqueous media the complexation stability constant between this ligand and Am(III) is roughly 10 times higher than the ones corresponding to Ln(III). The synthesis of lipophilic derivatives of 2-pyridinecarboxamide leaded to extraction experiments. The extraction of metallic cation by lipophilic picolinamides, according to a solvatation mechanism, is strongly dependent on the nature of the amide function: a primary amide function (group I) leads to a good extraction; on the contrary, there is a decrease for secondary (group II) and tertiary (group III) amide functions. From a theoretical point of view, this work leads finally to the following conclusions: confirmation of the importance of the presence of soft donor atoms within the extractants (nitrogen in our case) for An(III)/Ln(III). Also, sensitivity of this soft donor atom regarding the protonation reaction; prevalence in our case of the affinity of the extractant for the metallic cation over the lipophilia of the extractant to ensure good distribution coefficients. The extraction and Am(III)/Ln(III) separation performances of the picolinamides from pertechnetic media leads to the design of a possible flowsheet for the reprocessing of high level liquid waste, with the new idea of an integrated technetium reflux. (author)

  16. Genotoxicity, mutagenicity and cytotoxicity of carotenoids extracted from ionic liquid in multiples organs of Wistar rats.

    Science.gov (United States)

    Larangeira, Paula Martins; de Rosso, Veridiana Vera; da Silva, Victor Hugo Pereira; de Moura, Carolina Foot Gomes; Ribeiro, Daniel Araki

    2016-11-01

    The ionic liquid or melted salt 1-Butyl-3-methylimidazolium is an alternative process to extract natural pigments, such as carotenoids. Lycopene represents 80-90% of total of carotenoids presents in tomatoes and it has been widely studied due its potent antioxidant action. The aim of this study was to evaluate genotoxicity, mutagenicity and cytotoxicity of carotenoids extracted from ionic liquid using experimental model in vivo. For this purpose, a total of 20 male Wistar rats were distributed into four groups (n=5), as follows: control group; received a corresponding amount of corn oil for 7days by intragastric gavage (i.g.), ionic liquid group, received 10mgkg -1 body weight for 7days by gavage; 10mg carotenoids group, received 10mgkg -1 bw dissolved in corn oil for 7days by gavage and 500mg carotenoids group, received 500mgkg -1 bw dissolved in corn oil for 7days by gavage. Rat liver treated with ionic liquid exhibited moderate histopathological changes randomly distributed in the parenchyma, such as cytoplasmic eosinophilia, apoptotic bodies, inflammatory infiltrate and focal necrosis. DNA damage was found in peripheral blood and liver cells of rats treated with ionic liquid or carotenoids at 500mg. An increase of micronucleated cells and 8-OhDG immunopositive cells were also detected in rats treated with carotenoids at 500mg. In summary, our results demonstrate that recommended dose for human daily intake of carotenoids extracted by ionic liquid did not induce genotoxicity, mutagenicity and cytotoxicity in multiple organs of rats. Copyright © 2016 Elsevier GmbH. All rights reserved.

  17. Ion-pair vortex assisted liquid-liquid microextraction with back extraction coupled with high performance liquid chromatography-UV for the determination of metformin in plasma.

    Science.gov (United States)

    Alshishani, Anas; Makahleh, Ahmad; Yap, Hui Fang; Gubartallah, Elbaleeq Adam; Salhimi, Salizawati Muhamad; Saad, Bahruddin

    2016-12-01

    A new sample preparation method, ion-pair vortex assisted liquid-liquid microextraction (VALLME-BE), for the determination of a highly polar anti-diabetic drug (metformin) in plasma sample was developed. The VALLME-BE was performed by diluting the plasma in borate buffer and extracted to 150µL 1-octanol containing 0.2M di-(2-ethylhexyl)phosphoric acid as intermediate phase. The drug was next back-extracted into 20µL of 0.075M HCl solution. The effects of pH, ion-pair concentration, type of organic solvent, volume of extraction phases, ionic strength, vortexing and centrifugation times on the extraction efficiency were investigated. The optimum conditions were at pH 9.3, 60s vortexing and 2min centrifugation. The microextract, contained metformin and buformin (internal standard), was directly injected into a HPLC unit using C1 column (250mm×4.6mm×10µm) and detected at 235nm. The method was validated and calibration curve was linear with r 2 >0.99 over the range of 20-2000µgL -1 . The limits of detection and quantitation were 1.4 and 4.1µgL -1 , respectively. The accuracy was within 94.8-108% of the nominal concentration. The relative standard deviation for inter- and intra-day precision was less than 10.8%. The method was conveniently applied for the determination of metformin in plasma samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Liquid-Liquid Equilibrium data for mono ethylene glycol extraction from water with the new ionic liquid tetraoctyl ammonium 2-methyl-1-naphtoate as solvent

    NARCIS (Netherlands)

    Garcia Chavez, L.Y.; Schuur, Boelo; de Haan, A.B.

    2012-01-01

    Thermal recovery of mono ethylene glycol (MEG) from aqueous streams is one of the most energy demanding operations in industry, because of the large amount of water that needs to be evaporated. The use of alternative technologies such as liquid–liquid extraction could save energy. A new tailor made

  19. Liquid-liquid equilibrium data for mono ethylene glycol extraction from water with the new ionic liquid tetraoctyl ammonium 2-methyl-1-naphtoate as solvent

    NARCIS (Netherlands)

    Garcia Chavez, L.Y.; Schuur, B.; Haan, de A.B.

    2012-01-01

    Thermal recovery of mono ethylene glycol (MEG) from aqueous streams is one of the most energy demanding operations in industry, because of the large amount of water that needs to be evaporated. The use of alternative technologies such as liquid–liquid extraction could save energy. A new tailor made

  20. Experimental and Model Studies on Continuous Separation of 2-Phenylpropionic Acid Enantiomers by Enantioselective Liquid-Liquid Extraction in Centrifugal Contactor Separators.

    Science.gov (United States)

    Feng, Xiaofeng; Tang, Kewen; Zhang, Pangliang; Yin, Shuangfeng

    2016-03-01

    Multistage enantioselective liquid-liquid extraction (ELLE) of 2-phenylpropionic acid (2-PPA) enantiomers using hydroxypropyl-β-cyclodextrin (HP-β-CD) as extractant was studied experimentally in a counter-current cascade of centrifugal contactor separators (CCSs). Performance of the process was evaluated by purity (enantiomeric excess, ee) and yield (Y). A multistage equilibrium model was established on the basis of single-stage model for chiral extraction of 2-PPA enantiomers and the law of mass conservation. A series of experiments on the extract phase/washing phase ratio (W/O ratio), extractant concentration, the pH value of aqueous phase, and the number of stages was conducted to verify the multistage equilibrium model. It was found that model predictions were in good agreement with the experimental results. The model was applied to predict and optimize the symmetrical separation of 2-PPA enantiomers. The optimal conditions for symmetric separation involves a W/O ratio of 0.6, pH of 2.5, and HP-β-CD concentration of 0.1 mol L(-1) at a temperature of 278 K, where eeeq (equal enantiomeric excess) can reach up to 37% and Yeq (equal yield) to 69%. By simulation and optimization, the minimum number of stages was evaluated at 98 and 106 for eeeq > 95% and eeeq > 97%. © 2016 Wiley Periodicals, Inc.

  1. Ultra-high performance liquid chromatography with fluorescence detection following salting-out assisted liquid-liquid extraction for the analysis of benzimidazole residues in farm fish samples.

    Science.gov (United States)

    Tejada-Casado, Carmen; Lara, Francisco J; García-Campaña, Ana M; Del Olmo-Iruela, Monsalud

    2018-03-30

    Ultra-high performance liquid chromatography (UHPLC) coupled with fluorescence detection (FL) has been proposed for the first time to determine thirteen benzimidazoles (BZs) in farmed fish samples. In order to optimize the chromatographic separation, parameters such as mobile phase composition and flow rate were carefully studied, establishing a gradient mode with a mobile phase consisted of water (solvent A) and acetonitrile (solvent B) at a flow rate of 0.4 mL/min. The separation was performed on a Zorbax Eclipse Plus RRHD C 18 column (50 × 2.1 mm, 1.8 μm), involving a total analysis time lower than 12 min. Salting-out assisted liquid-liquid extraction (SALLE) was applied as sample treatment to different types of farmed fish (trout, sea bream and sea bass). To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized including the amount of sample, type and volume of the extraction solvent, and the nature and amount of the salt used. Characterization of the method in terms of performance characteristics was carried out, obtaining satisfactory results for the linearity (R 2  ≥ 0.997), repeatability (RSD ≤ 6.1%), reproducibility (RSD ≤ 10.8%) and recoveries (R ≥ 79%; RSD ≤ 7.8%). Detection limits between 0.04-29.9 μg kg -1 were obtained, demonstrating the applicability of this fast, simple and environmentally friendly method. Copyright © 2018 Elsevier B.V. All rights reserved.

  2. Long-chain ionic liquid based mixed hemimicelles and magnetic dispersed solid-phase extraction for the extraction of fluorescent whitening agents in paper materials.

    Science.gov (United States)

    Wang, Qing; Qiu, Bin; Chen, Xianbo; Wang, Bin; Zhang, Hui; Zhang, Xiaoyuan

    2017-06-01

    A novel mixed hemimicelles and magnetic dispersive solid-phase extraction method based on long-chain ionic liquids for the extraction of five fluorescent whitening agents was established. The factors influenced on extraction efficiency were investigated. Under the optimal conditions, namely, the pH of sample solution at 8.0, the concentration of long chain ionic liquid at 0.5 mmol/L, the amount of Fe 3 O 4 nanoparticle at 12 mg, extraction time at 10 min, pH 6.0 of methanol as eluent, and the desorption time at 1 min, satisfactory results were obtained. Wide linear ranges (0.02-10 ng/mL) and good linearity were attained (0.9997-0.9999). The intraday and interday RSDs were 2.1-8.3%. Limits of detection were 0.004-0.01 ng/mL, which were decreased by almost an order of magnitude compared to direct detection without extraction. The present method was applied to extract the fluorescent whitening agents in two kinds of paper samples, obtaining satisfactory results. All showed results illustrated that the detection sensitivity was improved and the proposed method was a good choice for the enriching and monitoring of trace fluorescent whitening agents. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Extraction separation of toluene/cyclohexane with hollow fiber supported ionic liquid membrane

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Fan; Sun, Wei; Liu, Junteng; Zhang, Weidong; Ren, Zhongqi [Beijing University of Chemical Technology, Beijing (China)

    2014-06-15

    A supported liquid membrane with ionic liquid was used for the separation of toluene/cyclohexane. The interactions of ionic liquid with toluene and cyclohexane were calculated and experimentally studied by quantum chemical calculation and liquid-liquid extraction process. The results showed [BPy][BF{sub 4}] have stronger interaction with toluene than that with cyclohexane. The selectivity of SILM processes was larger than 10 at the temperature of 323 K and the flow rate of 13.5 mL·min{sup -1} on both shell side and lumen side. Due to the higher viscosity of IL, SILM process had good long-term stability. As the effects of mass transfer driving force of SILM process, the flux and removal efficiency increased with increase of initial toluene concentration, while the selectivity decreased because of the competitive transport. Base on the resistance in-series model and experimental results, the mass transfer resistance was mainly lay liquid membrane phase. The influence of flow rates on both sides was slight. The higher temperature could enhance the mass transfer performance significantly. The removal efficiency increased from 28.2% to 45.1% with the increasing of operation temperature from 298 K to 323 K.

  4. Molecular Dynamics Simulations on the solvation and interfacial behaviour of hydrophobic species. Applications to the TATB hypothesis and to the liquid/liquid extraction of cations to supercritical CO2

    International Nuclear Information System (INIS)

    Schurhammer, R.

    2001-12-01

    We report molecular dynamics studies on the solvation of charged hydrophobic molecules in pure liquids and at liquid / liquid interfaces. The first part of the thesis deals with the TATB hypothesis according to which the Asφ 4 + (TA + ) and Bφ 4 - (TB - ) ions have the same free energy of solvation in any solvent. The two ions are found to be solvated differently in pure liquids (water, chloroform, acetonitrile) as at a chloroform / water interface. These results are confirmed by free energy calculations and by simulations on iso-volume spherical S + and S - ions, which perfectly meet the TATB criteria. The many methodological tests performed show the importance of (i) the corrected treatment of 'long range interactions' (ii) the precise repartition of atomic charges (iii) the solvent models, especially for water, on the + / - charge discrimination by solvent. In the second part, in relation to the liquid / liquid extraction of cations from water to supercritical CO 2 , we report the behaviour of ions (Cs + , UO 2 2+ , Eu 3+ ), of un-complexed extractants molecules (tri-n-butylphosphate, calixarene), of their complexes with the cations and nitric acid at a preformed chloroform / water interface and during de-mixing simulations which started from a perfectly mixed CO 2 / water solutions. These studies demonstrate the importance of interfacial phenomena, of simulation conditions and acid and extractant concentrations, in assisted ion extraction to supercritical CO 2 . (author)

  5. Direct extraction of genomic DNA from maize with aqueous ionic liquid buffer systems for applications in genetically modified organisms analysis.

    Science.gov (United States)

    Gonzalez García, Eric; Ressmann, Anna K; Gaertner, Peter; Zirbs, Ronald; Mach, Robert L; Krska, Rudolf; Bica, Katharina; Brunner, Kurt

    2014-12-01

    To date, the extraction of genomic DNA is considered a bottleneck in the process of genetically modified organisms (GMOs) detection. Conventional DNA isolation methods are associated with long extraction times and multiple pipetting and centrifugation steps, which makes the entire procedure not only tedious and complicated but also prone to sample cross-contamination. In recent times, ionic liquids have emerged as innovative solvents for biomass processing, due to their outstanding properties for dissolution of biomass and biopolymers. In this study, a novel, easily applicable, and time-efficient method for the direct extraction of genomic DNA from biomass based on aqueous-ionic liquid solutions was developed. The straightforward protocol relies on extraction of maize in a 10 % solution of ionic liquids in aqueous phosphate buffer for 5 min at room temperature, followed by a denaturation step at 95 °C for 10 min and a simple filtration to remove residual biopolymers. A set of 22 ionic liquids was tested in a buffer system and 1-ethyl-3-methylimidazolium dimethylphosphate, as well as the environmentally benign choline formate, were identified as ideal candidates. With this strategy, the quality of the genomic DNA extracted was significantly improved and the extraction protocol was notably simplified compared with a well-established method.

  6. 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.

  7. chemical studies on the extraction of certain metal ions from aqueous solution by liquid emulsion membrane

    International Nuclear Information System (INIS)

    Kassem, A.T.

    2011-01-01

    In this thesis four systems are addressed related to the use of liquid emulsion membranes (ELM) based on Co(III)dicarbiolide and. The system was dedicated for permeation of cadmium , cobalt Nickel and lead for use of this system for preconcentration and separation of cadmium, cobalt, nickel and lead. The work carried out in this thesis is presented in three parts, namely; introduction, experimental and results and discussion.The first chapter is the introduction which includes aim of work, basic concepts of liquid membranes; liquid emulsion membranes; different models of emulsion permeation, literature survey of extraction chemistry of cadmium, cobalt, nickel and lead. Chapter two includes the experimental part. In this part detailed outlines on the chemicals and different elements used were given. Different instruments as well as analytical techniques were outlines. The preparation of liquid emulsion membrane and the permeation techniques were presented in details. The third chapter deals with the results and discussion. This chapter is divided into four main parts, the four parts is concerned with cadmium/Co(III) dicarbolide/NTA, EDTA, DPTA and DCTA systems. In this part the permeation of Cd(II) aqueous solution by the membrane used was experimented based on liquid-liquid extraction studies of cadmium from different sodium chloride molarities (from 0.01 to 0.1 M) by 0.01 M Cobalt(III) dicarbolides. It was found that the extraction of with cadmium is higher following in the first system, the permeation of the toxic elements, Cd(II) from HCl/sodium chloride medium was carried out using liquid emulsion membrane containing Co(III)dicarbiolide in xylene as carrier, Spain 80/ Spain 85(1:3) as surfactant and NTA, EDTA, DPTA and DCTA as a stripping solutions.

  8. Automated on-line liquid–liquid extraction system for temporal mass spectrometric analysis of dynamic samples

    Energy Technology Data Exchange (ETDEWEB)

    Hsieh, Kai-Ta; Liu, Pei-Han [Department of Applied Chemistry, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China); Urban, Pawel L. [Department of Applied Chemistry, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China); Institute of Molecular Science, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China)

    2015-09-24

    Most real samples cannot directly be infused to mass spectrometers because they could contaminate delicate parts of ion source and guides, or cause ion suppression. Conventional sample preparation procedures limit temporal resolution of analysis. We have developed an automated liquid–liquid extraction system that enables unsupervised repetitive treatment of dynamic samples and instantaneous analysis by mass spectrometry (MS). It incorporates inexpensive open-source microcontroller boards (Arduino and Netduino) to guide the extraction and analysis process. Duration of every extraction cycle is 17 min. The system enables monitoring of dynamic processes over many hours. The extracts are automatically transferred to the ion source incorporating a Venturi pump. Operation of the device has been characterized (repeatability, RSD = 15%, n = 20; concentration range for ibuprofen, 0.053–2.000 mM; LOD for ibuprofen, ∼0.005 mM; including extraction and detection). To exemplify its usefulness in real-world applications, we implemented this device in chemical profiling of pharmaceutical formulation dissolution process. Temporal dissolution profiles of commercial ibuprofen and acetaminophen tablets were recorded during 10 h. The extraction-MS datasets were fitted with exponential functions to characterize the rates of release of the main and auxiliary ingredients (e.g. ibuprofen, k = 0.43 ± 0.01 h{sup −1}). The electronic control unit of this system interacts with the operator via touch screen, internet, voice, and short text messages sent to the mobile phone, which is helpful when launching long-term (e.g. overnight) measurements. Due to these interactive features, the platform brings the concept of the Internet-of-Things (IoT) to the chemistry laboratory environment. - Highlights: • Mass spectrometric analysis normally requires sample preparation. • Liquid–liquid extraction can isolate analytes from complex matrices. • The proposed system automates

  9. Automated on-line liquid–liquid extraction system for temporal mass spectrometric analysis of dynamic samples

    International Nuclear Information System (INIS)

    Hsieh, Kai-Ta; Liu, Pei-Han; Urban, Pawel L.

    2015-01-01

    Most real samples cannot directly be infused to mass spectrometers because they could contaminate delicate parts of ion source and guides, or cause ion suppression. Conventional sample preparation procedures limit temporal resolution of analysis. We have developed an automated liquid–liquid extraction system that enables unsupervised repetitive treatment of dynamic samples and instantaneous analysis by mass spectrometry (MS). It incorporates inexpensive open-source microcontroller boards (Arduino and Netduino) to guide the extraction and analysis process. Duration of every extraction cycle is 17 min. The system enables monitoring of dynamic processes over many hours. The extracts are automatically transferred to the ion source incorporating a Venturi pump. Operation of the device has been characterized (repeatability, RSD = 15%, n = 20; concentration range for ibuprofen, 0.053–2.000 mM; LOD for ibuprofen, ∼0.005 mM; including extraction and detection). To exemplify its usefulness in real-world applications, we implemented this device in chemical profiling of pharmaceutical formulation dissolution process. Temporal dissolution profiles of commercial ibuprofen and acetaminophen tablets were recorded during 10 h. The extraction-MS datasets were fitted with exponential functions to characterize the rates of release of the main and auxiliary ingredients (e.g. ibuprofen, k = 0.43 ± 0.01 h"−"1). The electronic control unit of this system interacts with the operator via touch screen, internet, voice, and short text messages sent to the mobile phone, which is helpful when launching long-term (e.g. overnight) measurements. Due to these interactive features, the platform brings the concept of the Internet-of-Things (IoT) to the chemistry laboratory environment. - Highlights: • Mass spectrometric analysis normally requires sample preparation. • Liquid–liquid extraction can isolate analytes from complex matrices. • The proposed system automates the

  10. A simple liquid extraction protocol for overcoming the ion suppression of triacylglycerols by phospholipids in liquid chromatography mass spectrometry studies.

    Science.gov (United States)

    Araujo, Pedro; Tilahun, Ephrem; Breivik, Joar Fjørtoft; Abdulkader, Bashir M; Frøyland, Livar; Zeng, Yingxu

    2016-02-01

    It is well-known that triacylglycerol (TAG) ions are suppressed by phospholipid (PL) ions in regiospecific analysis of TAG by mass spectrometry (MS). Hence, it is essential to remove the PL during sample preparation prior to MS analysis. The present article proposes a cost-effective liquid-liquid extraction (LLE) method to remove PL from TAG in different kinds of biological samples by using methanol, hexane and water. High performance thin layer chromatography confirmed the lack of PL in krill oil and salmon liver samples, submitted to the proposed LLE protocol, and liquid chromatography tandem MS confirmed that the identified TAG ions were highly enhanced after implementing the LLE procedure. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Application of an efficient strategy based on liquid-liquid extraction, high-speed counter-current chromatography, and preparative HPLC for the rapid enrichment, separation, and purification of four anthraquinones from Rheum tanguticum.

    Science.gov (United States)

    Chen, Tao; Liu, Yongling; Zou, Denglang; Chen, Chen; You, Jinmao; Zhou, Guoying; Sun, Jing; Li, Yulin

    2014-01-01

    This study presents an efficient strategy based on liquid-liquid extraction, high-speed counter-current chromatography, and preparative HPLC for the rapid enrichment, separation, and purification of four anthraquinones from Rheum tanguticum. A new solvent system composed of petroleum ether/ethyl acetate/water (4:2:1, v/v/v) was developed for the liquid-liquid extraction of the crude extract from R. tanguticum. As a result, emodin, aloe-emodin, physcion, and chrysophanol were greatly enriched in the organic layer. In addition, an efficient method was successfully established to separate and purify the above anthraquinones by high-speed counter-current chromatography and preparative HPLC. This study supplies a new alternative method for the rapid enrichment, separation, and purification of emodin, aloe-emodin, physcione, and chrysophanol. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Separation of thorium and uranium by liquid-liquid extraction from mixed aqueous nitric acidic-methanolic solutions

    International Nuclear Information System (INIS)

    Schmid, E.R.; Kenndler, E.

    1976-01-01

    A method is described for the separation of Th and U from each other and from other elements, usually occuring in minerals, by liquid-liquid extraction with Aliquat Nitrate (tricaprylmethyl ammoniumnitrate, 6 vol%) in benzene from a mixed solution of 2.5 M HNO 3 and methanol (1:1 volume ratio). Permissible upper concentration ratios of interfering elements, such as Li, Na, K, Mg, Ca, Al, Cu, Co(II), Fe(III), Mn(II), Ti(IV), La(III), U(VI), Cl - , ClO 4 - , SO 4 2- , PO 4 3- , have been determined. Following the separation, Th has been determined by spectrophotometry using Thorin, and U by fluorometry. Results for yield under varying conditions, together with elemental concentrations in the ppm range for U and Th in minerals, are given. (B.T.)

  13. Solid-phase extraction followed by dispersive liquid-liquid microextraction for the sensitive determination of ecstasy compounds and amphetamines in biological samples

    Directory of Open Access Journals (Sweden)

    H. A. Mashayekhi

    2014-09-01

    Full Text Available A novel approach for the determination of ecstasy and amphetamines (3,4-methylenedioxymethylamphetamine (MDMA, Ecstasy, 3,4-methylenedioxyamphetamine (MDA, 3,4-methylenedioxyethylamphetamine (MDEA and 3,4-methylenedioxypropylamphetamine (MDPA in biological samples is presented. The analytes were extracted from the matrix and transferred to a small volume of a high density, water insoluble solvent using solid-phase extraction (SPE followed by dispersive liquid-liquid microextraction (DLLME. This combination not only resulted in a high enrichment factor, but also it could be used in complex matrices (biological samples. Some important extraction parameters, such as sample solution flow rate, sample pH, type and volume of extraction and disperser solvents as well as the salt addition, were studied and optimized. Under the optimized conditions, the calibration graphs were linear in the range of 0.5-500 µg L-1 and 1.0-500 µg L-1 with detection limits in the range of 0.1-0.3 µg L-1 and 0.2-0.7 µg L-1 in urine and plasma samples, respectively. The results showed that SPE-DLLME is a suitable method for the determination of ecstasy components and amphetamines in biological and water samples. DOI: http://dx.doi.org/10.4314/bcse.v28i3.3

  14. Polonium-210 assay using a background-rejecting extractive liquid-scintillation method

    International Nuclear Information System (INIS)

    Case, C.N.; McDowell, W.J.

    1981-01-01

    This paper describes a procedure which combines solvent extraction with alpha liquid scintillation spectrometry. Pulse shape discrimination electronics are used to reject beta and gamma pulses and to lower the background count to acceptable levels. Concentration of 210 Po and separation from interferring elements are accomplished using a H 3 Po 4 -HCl solution with TOPO combined with a scintillor in toluene

  15. Ultrasound assisted extraction combined with dispersive liquid-liquid microextraction (US-DLLME)-a fast new approach to measure phthalate metabolites in nails.

    Science.gov (United States)

    Alves, Andreia; Vanermen, Guido; Covaci, Adrian; Voorspoels, Stefan

    2016-09-01

    A new, fast, and environmentally friendly method based on ultrasound assisted extraction combined with dispersive liquid-liquid microextraction (US-DLLME) was developed and optimized for assessing the levels of seven phthalate metabolites (including the mono(ethyl hexyl) phthalate (MEHP), mono(2-ethyl-5-hydroxyhexyl) phthalate (5-OH-MEHP), mono(2-ethyl-5-oxohexyl) phthalate (5-oxo-MEHP), mono-n-butyl phthalate (MnBP), mono-isobutyl phthalate (MiBP), monoethyl phthalate (MEP), and mono-benzyl phthalate (MBzP)) in human nails by UPLC-MS/MS. The optimization of the US-DLLME method was performed using a Taguchi combinatorial design (L9 array). Several parameters such as extraction solvent, solvent volume, extraction time, acid, acid concentration, and vortex time were studied. The optimal extraction conditions achieved were 180 μL of trichloroethylene (extraction solvent), 2 mL trifluoroacetic acid in methanol (2 M), 2 h extraction and 3 min vortex time. The optimized method had a good precision (6-17 %). The accuracy ranged from 79 to 108 % and the limit of method quantification (LOQm) was below 14 ng/g for all compounds. The developed US-DLLME method was applied to determine the target metabolites in 10 Belgian individuals. Levels of the analytes measured in nails ranged between <12 and 7982 ng/g. The MEHP, MBP isomers, and MEP were the major metabolites and detected in every sample. Miniaturization (low volumes of organic solvents used), low costs, speed, and simplicity are the main advantages of this US-DLLME based method. Graphical Abstract Extraction and phase separation of the US-DLLME procedure.

  16. Selection of optimum ionic liquid solvents for flavonoid and phenolic acids extraction

    Science.gov (United States)

    Rahman, N. R. A.; Yunus, N. A.; Mustaffa, A. A.

    2017-06-01

    Phytochemicals are important in improving human health with their functions as antioxidants, antimicrobials and anticancer agents. However, the quality of phytochemicals extract relies on the efficiency of extraction process. Ionic liquids (ILs) have become a research phenomenal as extraction solvent due to their unique properties such as unlimited range of ILs, non-volatile, strongly solvating and may become either polarity. In phytochemical extraction, the determination of the best solvent that can extract highest yield of solute (phytochemical) is very important. Therefore, this study is conducted to determine the best IL solvent to extract flavonoids and phenolic acids through a property prediction modeling approach. ILs were selected from the imidazolium-based anion for alkyl chains ranging from ethyl > octyl and cations consisting of Br, Cl, [PF6], BF4], [H2PO4], [SO4], [CF3SO3], [TF2N] and [HSO4]. This work are divided into several stages. In Stage 1, a Microsoft Excel-based database containing available solubility parameter values of phytochemicals and ILs including its prediction models and their parameters has been established. The database also includes available solubility data of phytochemicals in IL, and activity coefficient models, for solid-liquid phase equilibrium (SLE) calculations. In Stage 2, the solubility parameter values of the flavonoids (e.g. kaempferol, quercetin and myricetin) and phenolic acids (e.g. gallic acid and caffeic acid) are determined either directly from database or predicted using Stefanis and Marrero-Gani group contribution model for the phytochemicals. A cation-anion contribution model is used for IL. In Stage 3, the amount of phytochemicals extracted can be determined by using SLE relationship involving UNIFAC-IL model. For missing parameters (UNIFAC-IL), they are regressed using available solubility data. Finally, in Stage 4, the solvent candidates are ranked and five ILs, ([OMIM] [TF2N], [HeMIM] [TF2N], [HMIM] [TF2N

  17. Extraction of Biomolecules Using Phosphonium-Based Ionic Liquids + K3PO4 Aqueous Biphasic Systems

    Science.gov (United States)

    Louros, Cláudia L. S.; Cláudio, Ana Filipa M.; Neves, Catarina M. S. S.; Freire, Mara G.; Marrucho, Isabel M.; Pauly, Jérôme; Coutinho, João A. P.

    2010-01-01

    Aqueous biphasic systems (ABS) provide an alternative and efficient approach for the extraction, recovery and purification of biomolecules through their partitioning between two liquid aqueous phases. In this work, the ability of hydrophilic phosphonium-based ionic liquids (ILs) to form ABS with aqueous K3PO4 solutions was evaluated for the first time. Ternary phase diagrams, and respective tie-lines and tie-lines length, formed by distinct phosphonium-based ILs, water, and K3PO4 at 298 K, were measured and are reported. The studied phosphonium-based ILs have shown to be more effective in promoting ABS compared to the imidazolium-based counterparts with similar anions. Moreover, the extractive capability of such systems was assessed for distinct biomolecules (including amino acids, food colourants and alkaloids). Densities and viscosities of both aqueous phases, at the mass fraction compositions used for the biomolecules extraction, were also determined. The evaluated IL-based ABS have been shown to be prospective extraction media, particularly for hydrophobic biomolecules, with several advantages over conventional polymer-inorganic salt ABS. PMID:20480041

  18. Preconcentration of uranium in water samples using dispersive liquid-liquid micro- extraction coupled with solid-phase extraction and determination with inductively coupled plasma-optical emission spectrometry

    Directory of Open Access Journals (Sweden)

    M. Rezaee,

    2015-10-01

    Full Text Available A new liquid phase microextraction method based on the dispersion of an extraction solvent into aqueous phase coupled with solid-phase extraction was investigated for the extraction, preconcentration and determination of uranium in water samples. 1-(2-Pyridylazo-2-naphthol reagent (PAN at pH 6.0 was used as a chelating agent prior to extraction. After concentration and purification of the samples in SPE C18 sorbent, 1.5 mL elution sample containing 40.0 µL chlorobenzene was injected into the 5.0 mL pure water. After extraction and centrifuging, the sedimented phase was evaporated and the residue was dissolved in nitric acid (0.5 M and was injected by injection valve into the ICP-OES. Some important extraction parameters, such as sample solution flow rate, sample pH, type and volume of extraction and disperser solvents as well as the salt addition were studied and optimized. Under the optimum conditions, the calibration graph was linear in the range of 0.5-500 µg L-1. The detection limit was 0.1 µg L-1. The relative standard deviation (RSD at 5.0 µg L-1 concentration level was 6.6%. Finally, the developed method was successfully applied to the extraction and determination of uranium in the well, river, mineral, waste and tap water samples and satisfactory results were obtained.DOI: http://dx.doi.org/10.4314/bcse.v29i3.4

  19. Separation and Recycling for Rare Earth Elements by Homogeneous Liquid-Liquid Extraction (HoLLE Using a pH-Responsive Fluorine-Based Surfactant

    Directory of Open Access Journals (Sweden)

    Shotaro Saito

    2015-08-01

    Full Text Available A selective separation and recycling system for metal ions was developed by homogeneous liquid-liquid extraction (HoLLE using a fluorosurfactant. Sixty-two different elemental ions (e.g., Ag, Al, As, Au, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cr, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Hg, Ho, In, Ir, La, Lu, Mg, Mn, Mo, Nb, Nd, Ni, Os, P, Pb, Pd, Pr, Pt, Re, Rh, Ru, Sb, Sc, Se, Si, Sm, Sn, Sr, Ta, Tb, Te, Ti, Tl, Tm, V, W, Y, Yb, Zn, and Zr were examined. By changing pH from a neutral or alkaline solution (pH ≥ 6.5 to that of an acidic solution (pH < 4.0, gallium, zirconium, palladium, silver, platinum, and rare earth elements were extracted at >90% efficiency into a sedimented Zonyl FSA® (CF3(CF2n(CH22S(CH22COOH, n = 6–8 liquid phase. Moreover, all rare earth elements were obtained with superior extraction and stripping percentages. In the recycling of rare earth elements, the sedimented phase was maintained using a filter along with a mixed solution of THF and 1 M sodium hydroxide aqueous solution. The Zonyl FSA® was filtrated and the rare earth elements were recovered on the filter as a hydroxide. Furthermore, the filtrated Zonyl FSA was reusable by conditioning the subject pH.

  20. Extracting energy and structure properties of glass-forming liquids from structural relaxation time.

    Science.gov (United States)

    Wang, Lianwen

    2012-04-18

    A comprehensive examination of the kinetic liquid model (Wang et al 2010 J. Phys.: Condens. Matter 22 455104) is carried out by fitting the structural relaxation time of 26 different glass-forming liquids in a wide temperature range, including most of the well-studied materials. Careful analysis of the compiled reported data reveals that experimental inaccuracies should not be overlooked in any 'benchmark test' of relating theories or models (e.g. in Lunkenheimer et al 2010 Phys. Rev. E 81 051504). The procedure, accuracy, ability, and efficiency of the kinetic liquid model are discussed in detail and in comparison with other available fitting methods. In general, the kinetic liquid model could be verified by 17 of the 26 compiled data sets and can serve as a meaningful approximative method for analyzing these liquids. Nonetheless, further experimental examinations in a wide temperature range are needed and are called for. Through fitting, the microscopic details of these liquids are extracted, namely, the enthalpy, entropy, and cooperativity in structural relaxation, which may facilitate further quantitative analysis to both the liquidus and glassy states of these materials.

  1. Quantification of VX Nerve Agent in Various Food Matrices by Solid-Phase Extraction Ultra-Performance Liquid ChromatographyTime-of-Flight Mass Spectrometry

    Science.gov (United States)

    2016-04-01

    QUANTIFICATION OF VX NERVE AGENT IN VARIOUS FOOD MATRICES BY SOLID - PHASE EXTRACTION ULTRA-PERFORMANCE...TITLE AND SUBTITLE Quantification of VX Nerve Agent in Various Food Matrices by Solid - Phase Extraction Ultra-Performance Liquid Chromatography...QUANTIFICATION OF VX NERVE AGENT IN VARIOUS FOOD MATRICES BY SOLID - PHASE EXTRACTION ULTRA-PERFORMANCE LIQUID CHROMATOGRAPHY–TIME-OF-FLIGHT MASS

  2. Parallel artificial liquid membrane extraction as an efficient tool for removal of phospholipids from human plasma

    DEFF Research Database (Denmark)

    Ask, Kristine Skoglund; Bardakci, Turgay; Parmer, Marthe Petrine

    2016-01-01

    Generic Parallel Artificial Liquid Membrane Extraction (PALME) methods for non-polar basic and non-polar acidic drugs from human plasma were investigated with respect to phospholipid removal. In both cases, extractions in 96-well format were performed from plasma (125μL), through 4μL organic...

  3. Simultaneous micro-electromembrane extractions of anions and cations using multiple free liquid membranes and acceptor solutions

    Czech Academy of Sciences Publication Activity Database

    Kubáň, Pavel; Boček, Petr

    2016-01-01

    Roč. 908, FEB (2016), s. 113-120 ISSN 0003-2670 R&D Projects: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : free liquid membranes * micro-electromembrane extraction * simultaneous extractions Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.950, year: 2016

  4. Simultaneous micro-electromembrane extractions of anions and cations using multiple free liquid membranes and acceptor solutions

    Czech Academy of Sciences Publication Activity Database

    Kubáň, Pavel; Boček, Petr

    2016-01-01

    Roč. 908, FEB (2016), s. 113-120 ISSN 0003-2670 R&D Projects: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : free liquid membranes * micro-electromembrane extraction * simultaneous extractions Subject RIV: CB - Analytical Chemistry , Separation Impact factor: 4.950, year: 2016

  5. Skin whitening and anti-corrugation activities of glycoprotein fractions from liquid extracts of boiled sea cucumber.

    Science.gov (United States)

    Kim, So Jung; Park, So Yun; Hong, Sun-Mee; Kwon, Eun-Hye; Lee, Taek-Kyun

    2016-10-01

    To determine skin whitening and wrinkle improvement efficacy, glycoprotein fractions were extracted from liquid extracts of boiled sea cucumber and their effects on tyrosine and elastase inhibitory activities were assayed. Fractions above and below 50 kDa (>50 kDa and 50 kDa enhanced tyrosinase and elastase inhibitory activities by 50.84% and 28.78%, respectively. Correlations of the >50 kDa concentration with tyrosinase inhibitory (R2 = 0.968) and elastase inhibitory (R2 = 0.983) efficacy were significant. >50 kDa glycoprotein fraction isolated from liquid extracts of boiled sea cucumber, which can serve as a functional cosmetic ingredient for whitening and wrinkle improvement of skin. Copyright © 2016 Hainan Medical University. Production and hosting by Elsevier B.V. All rights reserved.

  6. Recovery of Ni Metal from Spent Catalyst with Emulsion Liquid Membrane Using Cyanex 272 as Extractant

    Science.gov (United States)

    Yuliusman; Huda, M.; Ramadhan, I. T.; Farry, A. R.; Wulandari, P. T.; Alfia, R.

    2018-03-01

    In this study was conducted to recover nickel metal from spent nickel catalyst resulting from hydrotreating process in petroleum industry. The nickel extraction study with the emulsion liquid membrane using Cyanex 272 as an extractant to extract and separate nickel from the feed phase solution. Feed phase solution was preapred from spent catalyst using sulphuric acid. Liquid membrane consists of a kerosene as diluent, a Span 80 as surfactant, a Cyanex 272 as carrier and sulphuric acid solutions have been used as the stripping solution. The important parameters governing the permeation of nickel and their effect on the separation process have been studied. These parameters are surfactant concentration, extractant concentration feed phase pH. The optimum conditions of the emulsion membrane making process is using 0.06 M Cyanex 272, 8% w/v SPAN 80, 0.05 M H2SO4, internal phase extractant / phase volume ratio: 1/1, and stirring speed 1150 rpm for 60 Minute that can produce emulsion membrane with stability level above 90% after 4 hours. In the extraction process with optimum condition pH 6 for feed phase, ratio of phase emulsion/phase of feed: 1/2, and stirring speed 175 rpm for 15 minutes with result 81.51% nickel was extracted.

  7. Rapid determination of alkaloids in Macleaya cordata using ionic liquid extraction followed by multiple reaction monitoring UPLC-MS/MS analysis.

    Science.gov (United States)

    Li, Linqiu; Huang, Mingyuan; Shao, Junli; Lin, Bokun; Shen, Qing

    2017-02-20

    The ultrasonic-assisted extraction (UAE) and ionic liquid based dispersive liquid-liquid microextraction (IL-DLLME) have been successfully applied in extracting of six alkaloids from M. cordata. 1-hexyl-3-methylimidazolium tetrafluoroborate ([C 6 MIM][BF 4 ]) aqueous solution was used as extraction solvent. The target analytes in raw material were deposited into a single drop of 1-hexyl-3-methylimidazolium hexafluorophosphate ([C 6 MIM][PF 6 ]), which was in situ formed by mixing [C 6 MIM][BF 4 ] and potassium hexafluorophosphate ([K][PF 6 ]. Afterwards, the extract was analyzed by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) in multiple-reaction monitoring (MRM) mode. The proposed method was fully validated in terms of linearity (0.9983-0.9992), LOD (0.080ngmL -1 ), LOQ (0.25ngmL -1 ), intra-day precision (MS/MS is powerful and practical for analyzing alkaloids in M. cordata., and it also has great potential for comprehensive quality control of other herbal medicines. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. 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.

  9. Liquid-liquid extraction of strongly protein bound BMS-299897 from human plasma and cerebrospinal fluid, followed by high-performance liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Xue, Y J; Pursley, Janice; Arnold, Mark

    2007-04-11

    BMS-299897 is a gamma-secretase inhibitor that is being developed for the treatment of Alzheimer's disease. Liquid-liquid extraction (LLE), chromatographic/tandem mass spectrometry (LC/MS/MS) methods have been developed and validated for the quantitation of BMS-299897 in human plasma and cerebrospinal fluid (CSF). Both methods utilized (13)C6-BMS-299897, the stable label isotope analog, as the internal standard. For the human plasma extraction method, two incubation steps were required after the addition of 5 mM ammonium acetate and the internal standard in acetonitrile to release the analyte bound to proteins prior to LLE with toluene. For the human CSF extraction method, after the addition of 0.5 N HCl and the internal standard, CSF samples were extracted with toluene and no incubation was required. The organic layers obtained from both extraction methods were removed and evaporated to dryness. The residues were reconstituted and injected into the LC/MS/MS system. Chromatographic separation was achieved isocratically on a MetaChem C18 Hypersil BDS column (2.0 mm x 50 mm, 3 microm). The mobile phase contained 10 mM ammonium acetate pH 5 and acetonitrile. Detection was by negative ion electrospray tandem mass spectrometry. The standard curves ranged from 1 to 1000 ng/ml for human plasma and 0.25-100 ng/ml for human CSF. Both standard curves were fitted to a 1/x weighted quadratic regression model. For both methods, the intra-assay precision was within 8.2% CV, the inter-assay precision was within 5.4% CV, and assay accuracy was within +/-7.4% of the nominal values. The validation and sample analysis results demonstrated that both methods had acceptable precision and accuracy across the calibration ranges.

  10. A highly selective dispersive liquid-liquid microextraction approach based on the unique fluorous affinity for the extraction and detection of per- and polyfluoroalkyl substances coupled with high performance liquid chromatography tandem-mass spectrometry.

    Science.gov (United States)

    Wang, Juan; Shi, Yali; Cai, Yaqi

    2018-04-06

    In the present study, a highly selective fluorous affinity-based dispersive liquid-liquid microextraction (DLLME) technique was developed for the extraction and analysis of per- and polyfluoroalkyl substances (PFASs) followed by high performance liquid chromatography tandem-mass spectrometry. Perfluoro-tert-butanol with multiple C-F bonds was chosen as the extraction solvent, which was injected into the aqueous samples with a dispersive solvent (acetonitrile) in a 120:800 (μL, v/v) mixture for PFASs enrichment. The fluorous affinity-based extraction mechanism was confirmed by the significantly higher extraction recoveries for PFASs containing multiple fluorine atoms than those for compounds with fewer or no fluorine atoms. The extraction recoveries of medium and long-chain PFASs (CF 2  > 5) exceeded 70%, except perfluoroheptanoic acid, while those of short-chain PFASs were lower than 50%, implying that the proposed DLLME may not be suitable for their extraction due to weak fluorous affinity. This highly fluoroselective DLLME technique can greatly decrease the matrix effect that occurs in mass spectrometry detection when applied to the analysis of urine samples. Under the optimum conditions, the relative recoveries of PFASs with CF 2  > 5 ranged from 80.6-121.4% for tap water, river water and urine samples spiked with concentrations of 10, 50 and 100 ng/L. The method limits of quantification for PFASs in water and urine samples were in the range of 0.6-8.7 ng/L. Furthermore, comparable concentrations of PFASs were obtained via DLLME and solid-phase extraction, confirming that the developed DLLME technique is a promising method for the extraction of PFASs in real samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Hydrogen extraction from liquid lithium-lead alloy by bubbling with rotational jet nozzle

    International Nuclear Information System (INIS)

    Xie Bo; Yang Tongzai; Guan Rui; Weng Kuiping

    2010-01-01

    The technology of tritium extraction from lithium-lead alloy has been simulated, hydrogen extraction from lithium-lead alloy by bubbling with rotational jet nozzle being used to simulate tritium in the study based on the introduction of fluid dynamics to establish algebraic model. The results show that the higher than lithium-lead melting temperature, the higher cumulative hydrogen extraction efficiency, and gas holdup of bubble column is little affected by the impeller diameter. Gas holdup when using small aperture is slightly higher when using large aperture only at a high helium flow rate, but the smaller the aperture, the greater the bubble surface area, and a marked increase in intensity of flow circulation for liquid lithium-lead with the increase of helium flow rate, hydrogen extraction rate increases too. Moreover, influence of the jet rotational velocity on hydrogen extraction is limited. (authors)

  12. Extraction and preconcentration of trace Al and Cr from vegetable samples by vortex-assisted ionic liquid-based dispersive liquid-liquid microextraction prior to atomic absorption spectrometric determination.

    Science.gov (United States)

    Altunay, Nail; Yıldırım, Emre; Gürkan, Ramazan

    2018-04-15

    In the study, a simple, and efficient microextraction approach, which is termed as vortex-assisted ionic liquid-based dispersive liquid-liquid microextraction (VA-IL-DLLME), was developed for flame atomic absorption spectrometric analysis of aluminum (Al) and chromium (Cr) in vegetables. The method is based on the formation of anionic chelate complexes of Al(III) and Cr(VI) with o-hydroxy azo dye, at pH 6.5, and then extraction of the hydrophobic ternary complexes formed in presence of cetyltrimethylammonium bromide (CTAB) into a 125 μL volume of 1-butyl-3-methylimidazolium bis(trifluorosulfonyl)imide [C 4 mim][Tf 2 N]) as extraction solvent. Under optimum conditions, the detection limits were 0.02 µg L -1 in linear working range of 0.07-100 µg L -1 for Al(III), and 0.05 µg L -1 in linear working range of 0.2-80 µg L -1 for Cr(VI). After the validation by analysis of a certified reference material (CRM), the method was successfully applied to the determination of Al and Cr in vegetables using standard addition method. Copyright © 2017 Elsevier Ltd. All rights reserved.

  13. The TRUEX [TRansUranium EXtraction] process and the management of liquid TRU [transuranic] waste

    International Nuclear Information System (INIS)

    Schulz, W.W.; Horwitz, E.P.

    1987-01-01

    The TRUEX process is a new generic liquid-liquid extraction process for removal of all actinides from acidic nitrate or chloride nuclear waste solutions. Because of its high efficiency and great flexibility, the TRUEX process appears destined to be widely used in the US and possibly in other countries for cost-effective management and disposal of transuranic (TRU) wastes. In the US, TRU wastes are those that contain ≥3.7 x 10 6 Bq/kg) of TRU elements with half-lives greater than 20 y. This paper gives a brief review of the relevant chemistry and summarizes the current status of development and deployment of the TRUEX (TRansUranium EXtraction) process flowsheets to treat specific acidic waste solutions at several US Department of Energy sites. 19 refs., 4 figs., 4 tabs

  14. Mathematical Modeling for the Extraction of Uranium and Molybdenum with Emulsion Liquid Membrane, Including Industrial Application and Cost Evaluation of the Uranium Recovery

    International Nuclear Information System (INIS)

    Kris Tri Basuki

    2008-01-01

    Emulsion liquid membrane systems are double emulsion drops. Two immiscible phases are separated by a third phase which is immiscible with the other two phases. The liquid membrane systems were classified into two types: (1) carrier mediated mass transfer, (2) mass transfer without any reaction involved. Uranium extraction, molybdenum extraction and solvent extraction were used as purposed elements for each type of the membrane systems in the derivation of their mathematical models. Mass transfer in emulsion liquid membrane (ELM) systems has been modeled by several differential and algebraic equations. The models take into account the following : mass transfer of the solute from the bulk external phase to the external phase-membrane interface; an equilibrium reaction between the solute and the carrier to form the solute-carrier complex at the interface; mass transfer by diffusion of the solute-carrier complex in the membrane phase to the membrane-internal phase interface; another equilibrium reaction of the solute-carrier complex to release the solute at the membrane-internal phase interface into the internal phase. Models with or without the consideration of film resistances were developed and compared. The models developed in this study can predict the extraction rate through emulsion liquid membranes theoretically. All parameters required in the models can be determined before an experimental extraction run. Experimental data from literature (uranium extraction) and (molybdenum extraction and solvent extraction) were used to test the models. The agreements between the theoretical predictions and the experimental data were very good. The advantages of emulsion liquid membrane systems over traditional methods were discussed. The models developed in this research can be used directly for the design of emulsion liquid membrane systems. The results of this study represent a very significant step toward the practical applications of the emulsion liquid membrane

  15. Liquid-liquid extraction/headspace/gas chromatographic/mass spectrometric determination of benzene, toluene, ethylbenzene, (o-, m- and p-)xylene and styrene in olive oil using surfactant-coated carbon nanotubes as extractant.

    Science.gov (United States)

    Carrillo-Carrión, Carolina; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel

    2007-11-09

    BTEX-S compounds are widely distributed in the environment and can be present in different foodstuffs, including olive oil. Taking into account the risks of the exposure to these compounds, analytical methods for their determination in different matrices are mandatory. In this paper, the use of surfactant-coated multiwalled carbon nanotubes as additive in liquid-liquid extraction is applied for the determination of single-ring aromatic compounds in olive oil samples. After sample treatment, the aqueous extracts are subsequently analyzed by headspace/gas chromatography/mass spectrometry allowing the determination of BTEX-S within ca. 15 min. Each stage of the proposed LLE/HS/GC/MS configuration involves a selectivity enhancement avoiding the interference of other compounds of the sample matrix. Limits of detection were in the range 0.25 ng mL(-1) (obtained for ethylbenzene) and 0.43 ng mL(-1) (for benzene). The repeatability of the proposed method expressed as RSD varied between 1.9% (styrene) and 3.3% (benzene) (n=11).

  16. Electronic simulation of the supported liquid membrane in electromembrane extraction systems: Improvement of the extraction by precise periodical reversing of the field polarity

    International Nuclear Information System (INIS)

    Moazami, Hamid Reza; Nojavan, Saeed; Zahedi, Pegah; Davarani, Saied Saeed Hosseiny

    2014-01-01

    Highlights: • A simple equivalent circuit has been proposed for a supported liquid membrane. • A dual charge transfer mechanism was proposed for electromembrane extraction. • An improvement was observed by precise periodical reversing of the field polarity. - Abstract: In order to understand the limitations of electromebrane extraction procedure better, a simple equivalent circuit has been proposed for a supported liquid membrane consisting of a resistor and a low leakage capacitor in series. To verify the equivalent circuit, it was subjected to a simulated periodical polarity changing potential and the resulting time variation of the current was compared with that of a real electromembrane extraction system. The results showed a good agreement between the simulated current patterns and those of the real ones. In order to investigate the impact of various limiting factors, the corresponding values of the equivalent circuit were estimated for a real electromembrane extraction system and were attributed to the physical parameters of the extraction system. A dual charge transfer mechanism was proposed for electromembrane extraction by combining general migration equation and fundamental aspects derived from the simulation. Dual mechanism comprises a current dependent contribution of analyte in total current and could support the possibility of an improvement in performance of an electromembrane extraction by application of an asymmetric polarity changing potential. The optimization of frequency and duty cycle of the asymmetric polarity exchanging potential resulted in a higher recovery (2.17 times greater) in comparison with the conventional electromebrane extraction. The simulation also provided more quantitative approaches toward the investigation of the mechanism of extraction and contribution of different limiting factors in electromembrane extraction. Results showed that the buildup of the double layer is the main limiting factor and the Joule heating has

  17. Extraction and Liquid Chromatography-Tandem Mass Spectrometry Detection of 3-Monochloropropanediol Esters and Glycidyl Esters in Infant Formula.

    Science.gov (United States)

    Leigh, Jessica K; MacMahon, Shaun

    2016-12-14

    A method was developed for the extraction of fatty acid esters of 3-chloro-1,2-propanediol (3-MCPD) and glycidol from infant formula, followed by quantitative analysis of the extracts using liquid chromatography-tandem mass spectrometry (LC-MS/MS). These process-induced chemical contaminants are found in refined vegetable oils, and studies have shown that they are potentially carcinogenic and/or genotoxic, making their presence in edible oils (and processed foods containing these oils) a potential health risk. The extraction procedure involves a liquid-liquid extraction, where powdered infant formula is dissolved in water and extracted with ethyl acetate. Following shaking, centrifugation, and drying of the organic phase, the resulting fat extract is cleaned-up using solid-phase extraction and analyzed by LC-MS/MS. Method performance was confirmed by verifying the percent recovery of each 3-MCPD and glycidyl ester in a homemade powdered infant formula reference material. Average ester recoveries in the reference material ranged from 84.9 to 109.0% (0.6-9.5% RSD). The method was also validated by fortifying three varieties of commercial infant formulas with a 3-MCPD and glycidyl ester solution. Average recoveries of the esters across all concentrations and varieties of infant formula ranged from 88.7 to 107.5% (1.0-9.5% RSD). Based on the validation results, this method is suitable for producing 3-MCPD and glycidyl ester occurrence data in all commercially available varieties of infant formula.

  18. Determination of twelve herbicides in tobacco by a combination of solid–liquid–solid dispersive extraction using multi-walled carbon nanotubes, dispersive liquid-liquid micro-extraction, and detection by GC with triple quadrupole mass spectrometry

    International Nuclear Information System (INIS)

    Liao, Qie Gen; Zhou, Yao Min; Luo, Lin Guang; Wang, Li Bing; Feng, Xiao Hu

    2014-01-01

    We report on a method for the determination of twelve herbicides using solid–liquid–solid dispersive extraction (SLSDE), followed by dispersive liquid-liquid micro-extraction (DLLME) and quantitation by gas chromatography with triple quadrupole mass spectrometric detection. SLSDE was applied to the extraction of herbicides from tobacco samples using multi-walled carbon nanotubes (MWCNTs) as clean-up adsorbents. The effect of the quantity of MWCNTs on SLSDE, and of type and volume of extraction and disperser solvents and of salt effect on DLLME were optimized. Good linearity is obtained in the 5.0 - 500 μg kg −1 concentration range, with regression coefficients of >0.99. Intra-day and inter-day repeatability, expressed as relative standard deviations, are between 3 and 9 %. The recoveries in case of herbicide-spiked tobacco at concentration levels of 20.0, 50.0 and 100.0 g kg −1 ranged from 79 to 105 %, and LODs are between 1.5 and 6.1 μg kg −1 . All the tobacco samples were found to contain butralin and pendimethalin at levels ranging from 15.8 to 500.0 μg kg −1 . (author)

  19. The removal of dinitrochlorobenzene from industrial residuals by liquid-liquid extraction with chemical reaction

    Directory of Open Access Journals (Sweden)

    G. C. M. Ferreira

    2007-09-01

    Full Text Available Nitrochlorobenzenes (NCBs are very important in the chemical industry since they have been used as raw material for the manufacture of crop protection products, as active ingredients in the pharmaceutical industry, as pigments and as antioxidants as well as for other uses. In industrial processes, NCBs are produced by monochlorobenzene (MCB nitration reactions and one of the main residuals formed is dinitrochlorobenzene (DNCB, which is mainly composed of the isomer 2,4DNCB. This subproduct, although of commercial interest when in its pure state, is generally incinerated due to the high costs of recovery treatment and purification. The objective of this study is to present an alternative to the treatment of industrial residuals containing DNCB. The technique consists of converting DNCB into sodium dinitrophenolate, which is very soluble in water and is also easy to reuse. For this purpose, liquid-liquid extraction with chemical reaction (alkaline hydrolysis with a rotating disc contactor (RDC is used. Experimental data on MCB nitration reactions as well as alkaline hydrolysis using a rotating disc contactor are presented.

  20. A modified approach for isolation of essential oil from fruit of Amorpha fruticosa Linn using microwave-assisted hydrodistillation concatenated liquid-liquid extraction.

    Science.gov (United States)

    Chen, Fengli; Jia, Jia; Zhang, Qiang; Gu, Huiyan; Yang, Lei

    2017-11-17

    In this work, a modified technique was developed to separate essential oil from the fruit of Amorpha fruticosa using microwave-assisted hydrodistillation concatenated liquid-liquid extraction (MHD-LLE). The new apparatus consists of two series-wound separation columns for separating essential oil, one is the conventional oil-water separation column, and the other is the extraction column of components from hydrosol using an organic solvent. Therefore, the apparatus can simultaneously collect the essential oil separated on the top of hydrosol and the components extracted from hydrosol using an organic solvent. Based on the yield of essential oil in the first and second separation columns, the effects of parameters were investigated by single factor experiments and Box-Behnken design. Under the optimum conditions (2mL ethyl ether as the extraction solvent in the second separation column, 12mL/g liquid-solid ratio, 4.0min homogenate time, 35min microwave irradiation time and 540W microwave irradiation power), satisfactory yields for the essential oil in the first separation column (10.31±0.33g/kg) and second separation column (0.82±0.03g/kg) were obtained. Compared with traditional methods, the developed method gave a higher yield of essential oil in a shorter time. In addition, GC-MS analysis of the essential oil indicated significant differences of the relative contents of individual volatile components in the essential oils obtained in the two separation columns. Therefore, the MHD-LLE technique developed here is a good alternative for the isolation of essential oil from A. fruticosa fruit as well as other herbs. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Determination of species activities in organic phase. Modelling of liquid-liquid extraction system using uniquac and unifac models; Determination des activites des especes en phase organique. Application d`uniquac et unifac a la modelisation des systemes d`extraction liquide-liquide

    Energy Technology Data Exchange (ETDEWEB)

    Rat, B. [CEA Saclay, 91 - Gif-sur-Yvette (France). Dept. de Recherche en Retraitement et en Vitrification]|[Paris-6 Univ., 75 (France)

    1998-12-31

    The aim of nuclear fuel reprocessing is to separate reusable elements, uranium and plutonium from the other elements, fission products and minor actinides. PUREX process uses liquid-liquid extraction as separation method. Numerical codes for modelling the extraction operations of PUREX process use a semi-empirical model to represent the partition of species. To improve the precision and precision and predictive nature of the models, we looked for a theoretical tool which permits to quantify medium effects, especially in the organic phase, for which few models are available. The Sergeivskii-Dannus model permits to quantify deviations from ideality in organic phase equilibrated with aqueous phase, but with parameters depending on extractant/diluent ratio. We decided to investigate UNIQUAC and UNIFAC models which permit to estimate activity coefficients in non-electrolytic phases taking account of the mutual interactions of molecules and their morphology. UNIFAC is based on UNIQUAC but molecules are considered as structural groups assemblies. Before applying these model to extraction systems, we investigate their abilities to describe simple systems, binary and ternary systems. UNIQUAC has been applied to TBP/diluent mixtures and permits to estimate activity coefficients for diluents whose interactions with TPB are very different in nature and strength. Group contribution (UNIFAC) applied to TBP/alkane mixtures permits to represent the effect of lengthening alkane chain but not the effect of branching. UNIQUAC fails to describe the TBP/diluent/water/non-extractable-salt systems in case of strong TBP diluent interactions. In order to obtain a correct description of these systems, we used the Chem-UNIFAC model, where the INIFAC equation is supplemented with chemical equilibria allowing explicitly for complexes formation and where group contribution is used to describes complexes. We have with Chem-UNIFAC a model available which can take the effect of the diluent into

  2. Solvent extraction of Th(IV) from aqueous solution with methylimidazole in ionic liquid

    Energy Technology Data Exchange (ETDEWEB)

    Li, Wenkui; Lv, Hui; Liu, Ziyi; Wu, Jianrong; Li, Shun; Shen, Yinglin [Lanzhou Univ. (China). Radiochemistry Lab.; Yang, Shenghua [State Key Laboratory of Applied Organic Chemistry, Lanzhou (China)

    2016-07-01

    An extraction of Th(IV) was performed using 1-methylimidazole (1-MIM) or 2-methylimidazole (2-MIM) as the extractant in imidazolium type ionic liquids (ILs) or n-pentanol. The extractability for Th{sup 4+} in ILs was by far higher than that obtained in n-pentanol. The extraction mechanism was determined by slope analysis and ESI-MS. The transfer of Th{sup 4+} with MIM into ILs proceeded through both a cationic exchange and a neutral solvation mechanism, whereas the partitioning of Th{sup 4+} with MIM into n-pentanol only underwent a neutral solvation mechanism. The thermodynamic parameters values (ΔH, ΔS and ΔG) for extraction of Th{sup 4+} with 1-MIM in IL were calculated and the results indicated the extraction reaction was spontaneous and went through endothermic process. Separation of Th{sup 4+} from the solution of lanthanides (III) and uranium was also carried out by 1-MIM in ILs and n-pentanol.

  3. 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.

  4. Molecular Dynamics Simulations on the solvation and interfacial behaviour of hydrophobic species. Applications to the TATB hypothesis and to the liquid/liquid extraction of cations to supercritical CO{sub 2}; Simulations par dynamique moleculaire de la solvatation et du comportement interfacial d'especes hydrophobes: application a l'hypothese TATB et a l'extraction liquide/liquide de cations par le CO{sub 2} supercritique

    Energy Technology Data Exchange (ETDEWEB)

    Schurhammer, R

    2001-12-15

    We report molecular dynamics studies on the solvation of charged hydrophobic molecules in pure liquids and at liquid / liquid interfaces. The first part of the thesis deals with the TATB hypothesis according to which the As{phi}{sub 4}{sup +} (TA{sup +}) and B{phi}{sub 4}{sup -} (TB{sup -}) ions have the same free energy of solvation in any solvent. The two ions are found to be solvated differently in pure liquids (water, chloroform, acetonitrile) as at a chloroform / water interface. These results are confirmed by free energy calculations and by simulations on iso-volume spherical S{sup +} and S{sup -} ions, which perfectly meet the TATB criteria. The many methodological tests performed show the importance of (i) the corrected treatment of 'long range interactions' (ii) the precise repartition of atomic charges (iii) the solvent models, especially for water, on the + / - charge discrimination by solvent. In the second part, in relation to the liquid / liquid extraction of cations from water to supercritical CO{sub 2}, we report the behaviour of ions (Cs{sup +}, UO{sub 2}{sup 2+}, Eu{sup 3+}), of un-complexed extractants molecules (tri-n-butylphosphate, calixarene), of their complexes with the cations and nitric acid at a preformed chloroform / water interface and during de-mixing simulations which started from a perfectly mixed CO{sub 2} / water solutions. These studies demonstrate the importance of interfacial phenomena, of simulation conditions and acid and extractant concentrations, in assisted ion extraction to supercritical CO{sub 2}. (author)

  5. Evaluation and application of microwave-assisted extraction and dispersive liquid-liquid microextraction followed by high-performance liquid chromatography for the determination of polar heterocyclic aromatic amines in hamburger patties.

    Science.gov (United States)

    Aeenehvand, Saeed; Toudehrousta, Zahra; Kamankesh, Marzieh; Mashayekh, Morteza; Tavakoli, Hamid Reza; Mohammadi, Abdorreza

    2016-01-01

    This study developed an analytical method based on microwave-assisted extraction and dispersive liquid-liquid microextraction followed by high-performance liquid chromatography for the determination of three polar heterocyclic aromatic amines from hamburger patties. Effective parameters controlling the performance of the microextraction process, such as the type and volume of extraction and disperser solvents, microwave time, nature of alkaline aqueous solution, pH and salt amount, were optimized. The calibration graphs were linear in the range of 1-200 ng g(-1), with a coefficient of determination (R(2)) better than 0.9993. The relative standard deviations (RSD) for seven analyses were between 3.2% and 6.5%. The recoveries of those compounds in hamburger patties were from 90% to 105%. Detection limits were between 0.06 and 0.21 ng g(-1). A comparison of the proposed method with the existing literature demonstrates that it is a simple, rapid, highly selective and sensitive, and it gives good enrichment factors and detection limits for determining HAAs in real hamburger patties samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

    Science.gov (United States)

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

    2016-05-15

    A simple, sensitive and environmentally friendly method using polymeric ionic liquid-based stir cake sorptive extraction followed by high performance liquid chromatography with diode array detection (HPLC/DAD) has been developed for efficient quantification of six selected estrogens in environmental waters. To extract trace estrogens effectively, a poly (1-ally-3-vinylimidazolium chloride-co-ethylene dimethacrylate) monolithic cake was prepared and used as the sorbent of stir cake sorptive extraction (SCSE). The effects of preparation conditions of sorbent and extraction parameters of SCSE for estrogens were investigated and optimized. Under optimal conditions, the developed method showed satisfactory analytical performance for targeted analytes. Low limits of detection (S/N=3) and quantification limits (S/N=10) were achieved within the range of 0.024-0.057 µg/L and 0.08-0.19 µg/L, respectively. Good linearity of method was obtained for analytes with the correlation coefficients (R(2)) above 0.99. At the same time, satisfactory method repeatability and reproducibility was achieved in terms of intra- and inter-day precisions, respectively. Finally, the established SCSE-HPLC/DAD method was successfully applied for the determination of estrogens in different environmental water samples. Recoveries obtained for the determination of estrogens in spiked samples ranged from 71.2% to 108%, with RSDs below 10% in all cases. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Recovery of salicylic acid from aqueous solution by solvent extraction and supported liquid membrane using TOMAC as carrier

    International Nuclear Information System (INIS)

    Kouki, Noura; Tayeb, Rafik; Dhahbi, Mahmoud

    2009-01-01

    Conventional sewage treatment plants do not fully degrade residues of pharmaceuticals, so that they are introduced into the aquatic environment. On this basis, the demand for the development of efficient systems for removing these compounds from water has assumed a great research interest. Membrane operations are increasingly employed in many industrial sectors as important alternative technologies to the classical processes of separation. Among membrane-based separation processes, the use of supported liquid membranes (SLMs) has received growing attention during recent years. In our work we had tried to recover a pharmaceutical product, salicylic acid (S.A), from an aqueous solution by solvent extraction and supported liquid membrane using an ionic liquid: the tri octylmethylammonium chloride (TOMAC) as carrier. Ionic liquids has been revealed as interesting clean alternatives to classical solvents and their use as a liquid phase results in the stabilization of the SLMs duo to their negligible vapour pressure, the possibility of minimising their solubility in the surrounding phases by adequate selection of the cation and anion, and the greater capillary force associated with their high viscosity. For this reason we had studied the influence of different parameters which could affect the efficiency of the transport: pH of the feed phase, the nature of the strippant, the concentration of the strippant, the nature of the support and the initial concentration of the salicylic acid in the feed phase. We had noticed that the pH of the feed solution had no effect of the percentage extraction and after 24 hours we can extract completely our solute. TOMAC seemed to be a good extractant but we found difficult to strip salicylic acid from the TOMAC phase and this could be related to the formation of water micro environments in the ionic liquid membrane.

  8. The Influence of Lactic Acid Concentration on the Separation of Light Rare Earth Elements by Continuous Liquid-Liquid Extraction with 2-Ethylhexyl Phosphonic Acid Mono-2-ethylhexyl Ester

    Science.gov (United States)

    de Carvalho Gomes, Rafael; Seruff, Luciana Amaral; Scal, Maira Labanca Waineraich; Vera, Ysrael Marrero

    2018-02-01

    The separation of rare earth elements (REEs) using solvent extraction adding complexing agents appears to be an alternative to saponification of the extractant. We evaluated the effect of lactic acid concentration on didymium (praseodymium and neodymium) and lanthanum extraction with 2-ethylhexyl phosphonic acid mono-2-ethyl hexyl ester [HEH(EHP)] as extractant. First, we investigated in batch experiments the separation of lanthanum (La) and didymium (Pr and Nd) using McCabe-Thiele diagrams to estimate the number of extraction stages when the feed solution was or was not conditioned with lactic acid. Additionally, we conducted continuous liquid-liquid extraction experiments and evaluated the influence of lactic acid concentration on the REE extraction and separation. The tests showed that the extraction percentage of REEs and the separation factor Pr/La increased when the lactic acid concentration increased, but the didymium purity decreased. Lanthanum, praseodymium, and neodymium extraction rate were 23.0, 89.7, and 99.2 pct, respectively, with 1:1 aqueous/organic volume flow rate and feed solution doped with 0.52 mol L-1 lactic acid. The highest didymium purity reached was 92.0 pct with 0.26 mol L-1 lactic acid concentration.

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