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Sample records for extracted organic phase

  1. Conformational analysis of amide extractants by NMR in organic phase

    International Nuclear Information System (INIS)

    Berthon, C.

    1993-08-01

    This study deals with nuclear fuel reprocessing. We have essentially used NMR spectroscopy. We want to understand which kind of conformational parameters control selectivity and efficiency of amide extractant. The symmetric monoamides used are DOBA (C 3 H 7 CON (CH 2 CH(C 2 H 5 ) C 4 H 9 ) 2 ), DOiBA ((CH 3 ) 2 CCHON (CH 2 CH(C 2 H 5 )C 4 H 9 ) 2 ) and DOTA ((CH 3 ) 3 CCH 2 CON(CH 2 CH(C 2 H 5 )C 4 H 9 ) 2 ). Each gives two quasi equivalent conformers (cis and trans) in organic phases. The selected malonamide DMDBTDMA ((C 4 H 9 (CH 3 )NCO) 2 CHC 14 H 29 ) has four conformers because of its twice disymmetric amide functions. Weak interactions between monoamides which yield to dimer formation. The malonamide also gives dimers but forms aggregates too. Nitric acid extraction is due to the competitive formation of six species L, L 2 , L 2 (HNO 3 ), L(HNO 3 ), L(HNO 3 ) 2 , L(HNO 3 ) 3 (L: monoamide). Complexation between lanthanides (III) and monoamides yields to the stoichiometries L 3 Ln(NO 3 ) 3 and L 2 Ln(NO 3 ) 3 . Their ratio depend of steric hindrance on the carbonyl and the metal ionic radius. The same thing is observed of Pu 4+ and Th 4+ extraction in non acidic media. L 2 An(NO 3 ) 4 is the main stoichiometric except for the Th 4+ - DOBA system where the species (DOBA) 3 Th(NO 3 ) 4 appear. Exchange rates between the ligand and the complex are pointed out. The monoamide conformations obtained with lanthanide and plutonium nitrate can explain the difference in extracting power of this molecule between An 4+ and Ln 3+ . (author). 162 refs., 87 figs., 44 tabs., 7 annexes

  2. 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.

  3. Influence of the extracted solute on the aggregation of malonamide extractant in organic phases: Consequences for phase stability

    International Nuclear Information System (INIS)

    Berthon, L.; Martinet, L.; Testard, F.; Madic, Ch.; Zem, Th.

    2010-01-01

    Due to their amphiphilic properties, malonamide molecules in alkane are organized in reverse micelle type aggregates, composed of a polar core formed by the malonamide polar heads and the extracted solutes, and surrounded by a hydrophobic shell made up of the extractant alkyl chains. The aggregates interact with one another through an attractive potential, leading to the formation of a third phase. This occurs with the splitting of the organic phase into a light phase composed mostly of diluent, and a heavy third phase containing highly concentrated extractant and solutes. In this article, we show that the aggregation (monomer concentration, domain of stability, and attractive potential between micelles) greatly depends on the nature of the extracted solute, whereas the size of aggregate (aggregation number) is only slightly influenced by this. We describe the extraction of water, nitric acid, neodymium nitrate and uranyl nitrate. Strongly polarizable species induce consistently large attraction potentials and a small stability domain for the dispersion of nano-droplets in the solvent. Highly polarizable ions such as lanthanides or uranyl induce more long-range attractive interactions than do protons. (authors)

  4. Supramolecular organization of organic phases for DIAMEX solvent extraction process; Organisation supramoleculaire des phases organiques de malonamides du procede d'extraction DIAMEX

    Energy Technology Data Exchange (ETDEWEB)

    Martinet, L

    2005-04-15

    In the frame of nuclear waste cycle, supramolecular organization of organic phases has been studied for DIAMEX solvent extraction process. A general methodology has been developed in order to determine surfactant properties of an extractant at high concentration. An illustration is given by a malonamide (DMDBTDMA) at 0.7 mol/L, in dodecane and contacted with water, at 23 deg C. The concentrations of monomers (0.3 mol/L) and aggregates (0.4 mol/L), c.m.c. (0.25 mol/L), aggregation number (4,4), aggregation constant (7.7) and finally aggregates interactions (U/kT = -1.6) are quantified. The method is based on simultaneous utilization of four experimental techniques (small X-ray and neutron scattering, vapour pressure osmometry and tensiometry) added to the model of Baxter. The structure of malonamide organic phase is depending on extractant concentration. (i) Below 0.2 mol/L, it is a quasi-molecular liquid fluid, extracting few amount of solutes. (ii) From 0.2 to 1 mol/L, it is a complex liquid fluid, containing small spherical aggregates of 5 extractant molecules in coexistence with monomers. This phase behaves like typical microemulsions with reverse micelles, through its stabilizing effect of penetrating oil and steric repulsion between extractants. (iii) Above 1 mol/L, the organic phase is able to extract huge amount of solutes. When HNO{sub 3} or Nd(NO{sub 3} ){sub 3} are extracted, a gel with a pseudo-lamellar structure is observed. With UO{sub 2} (NO{sub 3} ){sub 2} a solid crystal with a ratio DMDBTDMA/UO{sub 2} (NO{sub 3} ){sub 2} equal to 1/1 is characteristic of the organic phase. The 'third phase' due to attractive interactions between aggregates has exactly the same supramolecular structure than an 'unsplitted organic phase' of the same composition. Aggregates interactions are independent on the chemical affinity of the extractant for solutes. (author)

  5. Supramolecular organization of organic phases for DIAMEX solvent extraction process; Organisation supramoleculaire des phases organiques de malonamides du procede d'extraction DIAMEX

    Energy Technology Data Exchange (ETDEWEB)

    Martinet, L

    2005-04-15

    In the frame of nuclear waste cycle, supramolecular organization of organic phases has been studied for DIAMEX solvent extraction process. A general methodology has been developed in order to determine surfactant properties of an extractant at high concentration. An illustration is given by a malonamide (DMDBTDMA) at 0.7 mol/L, in dodecane and contacted with water, at 23 deg C. The concentrations of monomers (0.3 mol/L) and aggregates (0.4 mol/L), c.m.c. (0.25 mol/L), aggregation number (4,4), aggregation constant (7.7) and finally aggregates interactions (U/kT = -1.6) are quantified. The method is based on simultaneous utilization of four experimental techniques (small X-ray and neutron scattering, vapour pressure osmometry and tensiometry) added to the model of Baxter. The structure of malonamide organic phase is depending on extractant concentration. (i) Below 0.2 mol/L, it is a quasi-molecular liquid fluid, extracting few amount of solutes. (ii) From 0.2 to 1 mol/L, it is a complex liquid fluid, containing small spherical aggregates of 5 extractant molecules in coexistence with monomers. This phase behaves like typical microemulsions with reverse micelles, through its stabilizing effect of penetrating oil and steric repulsion between extractants. (iii) Above 1 mol/L, the organic phase is able to extract huge amount of solutes. When HNO{sub 3} or Nd(NO{sub 3} ){sub 3} are extracted, a gel with a pseudo-lamellar structure is observed. With UO{sub 2} (NO{sub 3} ){sub 2} a solid crystal with a ratio DMDBTDMA/UO{sub 2} (NO{sub 3} ){sub 2} equal to 1/1 is characteristic of the organic phase. The 'third phase' due to attractive interactions between aggregates has exactly the same supramolecular structure than an 'unsplitted organic phase' of the same composition. Aggregates interactions are independent on the chemical affinity of the extractant for solutes. (author)

  6. Synergistic extraction of transition metal cations from aqueous media by two separated organic phases

    International Nuclear Information System (INIS)

    Goldberg, I.

    1991-12-01

    We have therefore initiated novel approaches to the study of the mechanism of the synergistic extraction of metal ions by means of two separated organic phases, which are brought in contact with the same aqueous phase. The present work is concerned with the extraction of transition metals and actinides ions from nitric acid by chelating agents e.g., HTTA thenoyltrifluoroacetone in a diluent - the first organic phase, and by natural donor, e.g., TBP, tri-butyl phosphate in a diluent the second organic phase. The adduct formation was studied by means of spectrochemical and radiochemical methods. In the first approach the aqueous phase was attacked with both organic phases simultanously (the static or parallel extraction). In this method organic phase are separated one from the other. It was shown that even in the absence of mixing, synergism is observed under this experimental conditions. The results indicate, that adduct formation occurs in both organic phases. Nevertheless the enhanchment of extraction in the TBP phase is by far greater than that in the HTTA containing phase. This approach has one disadvatage, viz., the experiments are very time consuming, a typical experiment requiring over 10 days. In order to overcome this difficulty, the following experiments were carried out: the aqueous phase were first shaken with diluent containing an anionic ligand and the phases were allowed to separate. Then the aqueous solution were shaken with diluent containing a netural donor and the phase again were allowed to separate. The concentration of the metal ions in all the phases were determined. The experiments were repeated with an other diluent replacing the first diluent in one or both organic phases. In this way eight sequences of experiments were carried out for each concentration set chosen. The results thus point out that this experimental approach open new possibilities to investigate the mechanism and the kinetics of synergistic extraction processes. (author) the

  7. Improved light extraction from white organic light-emitting devices using a binary random phase array

    Energy Technology Data Exchange (ETDEWEB)

    Inada, Yasuhisa, E-mail: inada.yasuhisa@jp.panasonic.com; Nishiwaki, Seiji; Hirasawa, Taku; Nakamura, Yoshitaka; Hashiya, Akira; Wakabayashi, Shin-ichi; Suzuki, Masa-aki [R and D Division, Panasonic Corporation, 1006 Kadoma, Kadoma City, Osaka 571-8501 (Japan); Matsuzaki, Jumpei [Device Development Center, Eco Solutions Company, Panasonic Corporation, 1048 Kadoma, Osaka 571-8686 Japan (Japan)

    2014-02-10

    We have developed a binary random phase array (BRPA) to improve the light extraction performance of white organic light-emitting devices (WOLEDs). We demonstrated that the scattering of incoming light can be controlled by employing diffraction optics to modify the structural parameters of the BRPA. Applying a BRPA to the substrate of the WOLED leads to enhanced extraction efficiency and suppression of angle-dependent color changes. Our systematic study clarifies the effect of scattering on the light extraction of WOLEDs.

  8. Improved light extraction from white organic light-emitting devices using a binary random phase array

    International Nuclear Information System (INIS)

    Inada, Yasuhisa; Nishiwaki, Seiji; Hirasawa, Taku; Nakamura, Yoshitaka; Hashiya, Akira; Wakabayashi, Shin-ichi; Suzuki, Masa-aki; Matsuzaki, Jumpei

    2014-01-01

    We have developed a binary random phase array (BRPA) to improve the light extraction performance of white organic light-emitting devices (WOLEDs). We demonstrated that the scattering of incoming light can be controlled by employing diffraction optics to modify the structural parameters of the BRPA. Applying a BRPA to the substrate of the WOLED leads to enhanced extraction efficiency and suppression of angle-dependent color changes. Our systematic study clarifies the effect of scattering on the light extraction of WOLEDs

  9. Determination of volatile organic hydrocarbons in water samples by solid-phase dynamic extraction.

    Science.gov (United States)

    Jochmann, Maik A; Yuan, Xue; Schmidt, Torsten C

    2007-03-01

    In the present study a headspace solid-phase dynamic extraction method coupled to gas chromatography-mass spectrometry (HS-SPDE-GC/MS) for the trace determination of volatile halogenated hydrocarbons and benzene from groundwater samples was developed and evaluated. As target compounds, benzene as well as 11 chlorinated and brominated hydrocarbons (vinyl chloride, dichloromethane, cis-1,2-dichloroethylene, trans-1,2-dichloroethylene, carbon tetrachloride, chloroform, trichloroethylene, tetrachloroethylene, bromoform) of environmental and toxicological concern were included in this study. The analytes were extracted using a SPDE needle device, coated with a poly(dimethylsiloxane) with 10% embedded activated carbon phase (50-microm film thickness and 56-mm film length) and were analyzed by GC/MS in full-scan mode. Parameters that affect the extraction yield such as extraction and desorption temperature, salting-out, extraction and desorption flow rate, extraction volume and desorption volume, the number of extraction cycles, and the pre-desorption time have been evaluated and optimized. The linearity of the HS-SPDE-GC/MS method was established over several orders of magnitude. Method detection limits (MDLs) for the compounds investigated ranged between 12 ng/L for cis-dichloroethylene and trans-dichloroethylene and 870 ng/L for vinyl chloride. The method was thoroughly validated, and the precision at two concentration levels (0.1 mg/L and a concentration 5 times above the MDL) was between 3.1 and 16% for the analytes investigated. SPDE provides high sensitivity, short sample preparation and extraction times and a high sample throughput because of full automation. Finally, the applicability to real environmental samples is shown exemplarily for various groundwater samples from a former waste-oil recycling facility. Groundwater from the site showed a complex contamination with chlorinated volatile organic compounds and aromatic hydrocarbons.

  10. Determination of volatile organic hydrocarbons in water samples by solid-phase dynamic extraction

    Energy Technology Data Exchange (ETDEWEB)

    Jochmann, Maik A.; Schmidt, Torsten C. [Eberhard-Karls-Universitaet Tuebingen, Center for Applied Geoscience (ZAG), Tuebingen (Germany); Chair of Instrumental Analysis, University Duisburg-Essen, Duisburg (Germany); Yuan, Xue [Eberhard-Karls-Universitaet Tuebingen, Center for Applied Geoscience (ZAG), Tuebingen (Germany)

    2007-03-15

    In the present study a headspace solid-phase dynamic extraction method coupled to gas chromatography-mass spectrometry (HS-SPDE-GC/MS) for the trace determination of volatile halogenated hydrocarbons and benzene from groundwater samples was developed and evaluated. As target compounds, benzene as well as 11 chlorinated and brominated hydrocarbons (vinyl chloride, dichloromethane, cis-1,2-dichloroethylene, trans-1,2-dichloroethylene, carbon tetrachloride, chloroform, trichloroethylene, tetrachloroethylene, bromoform) of environmental and toxicological concern were included in this study. The analytes were extracted using a SPDE needle device, coated with a poly(dimethylsiloxane) with 10% embedded activated carbon phase (50-{mu}m film thickness and 56-mm film length) and were analyzed by GC/MS in full-scan mode. Parameters that affect the extraction yield such as extraction and desorption temperature, salting-out, extraction and desorption flow rate, extraction volume and desorption volume, the number of extraction cycles, and the pre-desorption time have been evaluated and optimized. The linearity of the HS-SPDE-GC/MS method was established over several orders of magnitude. Method detection limits (MDLs) for the compounds investigated ranged between 12 ng/L for cis-dichloroethylene and trans-dichloroethylene and 870 ng/L for vinyl chloride. The method was thoroughly validated, and the precision at two concentration levels (0.1 mg/L and a concentration 5 times above the MDL) was between 3.1 and 16% for the analytes investigated. SPDE provides high sensitivity, short sample preparation and extraction times and a high sample throughput because of full automation. Finally, the applicability to real environmental samples is shown exemplarily for various groundwater samples from a former waste-oil recycling facility. Groundwater from the site showed a complex contamination with chlorinated volatile organic compounds and aromatic hydrocarbons. (orig.)

  11. Polarographic behaviour and determination of uranium(VI) in alcoholic solutions from organic extraction phases

    International Nuclear Information System (INIS)

    Degueldre, C.; Taibi, K.

    1996-01-01

    The determination of U(VI) in organic extraction phases: hydrocarbon-diethyl-2-hexyl phosphoric acid-trioctylphosphine oxide and hydrocarbon-tri-n-octylamine, diluted by an alcohol has been studied by direct current polarography, as well as by differential pulse polarography (DPP). In order to optimise the analytical procedure, miscibility and conductivity studies of the mixtures hydrocarbon-alcohol (ethanol, n- and isopropanol and n- and isobutanol) were made after addition of sulphuric acid as a supporting electrolyte. In the solutions of sulphuric acid in the alcohol-extractant-hydrocarbon phases, U(VI) gives rise to well defined polarograms. Its electroreduction involves a single electron step in all cases. The DPP peak height is proportional to the U(VI) concentration between 2x10 -6 and 2x10 -3 M, and the 3σ detection limit is ca. 10 -6 M

  12. Studies on avoiding second organic phase in DHDECMP-TBP/kerosene with the extraction of HNO3-Gd

    International Nuclear Information System (INIS)

    Huang Zilin; Zhao Hugen; Hu Jingxin

    1998-01-01

    The bidentate extractant of DHDECMP (CMP) may by more practical in the treatment of high-level liquid waste (HLLW) if it could be diluted by kerosene. Bu it is difficult to avoid the formation of second organic phase in CMP/kerosene with the extraction of HNO 3 and RE. It is advantageous to avoid the formation of second organic phase after the extraction of HNO 3 and Gd by adding TBP. The formation conditions of second organic phase are studied and the loaded capacity of RE-HNO 3 is measured. The results are as follows. Raising temperature has a slight advantage to avoid formation of second organic phase. The addition of TBP is beneficial to avoid second organic phase. An organic system of 0.60 mol/L CMP-1.20 mol/L TBP/kerosene contacting with an aqueous solution containing 6.0 mol/L HNO 3 does not appear second organic phase. The extraction of RE leads to form second organic phase which does not occur when it only extracts HNO 3 . It is able to avoid second organic phase with a low concentration of CMP. The higher concentration of CMP, the higher loaded capacity of Gd 3+ and HNO 3 . It is advantageous to avoid second organic phase formation and also to get a higher loaded capacity of Gd 3+ and HNO 3 with increasing concentration of TBP. The loaded capacity of Gd decreases with an increasing initial concentration of HNO 3 in aqueous phase because of an increasing concentration of HNO 3 in the organic phase. The loaded capacity of Gd increases with raising temperature. To treat HLLW, the organic system containing 0.60 mol/L CMP and 1.40 mol/L TBP is recommended

  13. Formation of the second organic phase during uranyl nitrate extraction from aqueous solution by 30% tributylphosphate solution in paraffin

    International Nuclear Information System (INIS)

    Yhrkin, V.G.

    1996-01-01

    For extraction systems aqueous solution of uranyl nitrate-30% solution of tributylphosphate in individual paraffins from C 13 to C 17 the influence of the second organic phase of uranyl nitrate concentration in aqueous and organic phases, the length of hydrocarbon chain of paraffin hydrocarbon and temperature from 25 to 50 deg C on formation conditions has been defected. A special method of achieving the conditions of organic phase stratification from three-phase region, involving definition of equilibrium phases composition by density and refractive index, has been elaborated for more precise definition of organic phase homogeneity region. It has been revealed that without addition of nitric acid to uranyl nitrate solution the organic phase homogeneity limits can be achieved solely on paraffins C 15 , C 16 and C 17 and only under conditions similar to equeous phase saturation in terms of uranyl nitrate. 16 refs., 2 figs

  14. [Optimization of solid-phase extraction for enrichment of toxic organic compounds in water samples].

    Science.gov (United States)

    Zhang, Ming-quan; Li, Feng-min; Wu, Qian-yuan; Hu, Hong-ying

    2013-05-01

    A concentration method for enrichment of toxic organic compounds in water samples has been developed based on combined solid-phase extraction (SPE) to reduce impurities and improve recoveries of target compounds. This SPE method was evaluated in every stage to identify the source of impurities. Based on the analysis of Waters Oasis HLB without water samples, the eluent of SPE sorbent after dichloromethane and acetone contributed 85% of impurities during SPE process. In order to reduce the impurities from SPE sorbent, soxhlet extraction of dichloromethane followed by acetone and lastly methanol was applied to the sorbents for 24 hours and the results had proven that impurities were reduced significantly. In addition to soxhlet extraction, six types of prevalent SPE sorbents were used to absorb 40 target compounds, the lgK(ow) values of which were within the range of 1.46 and 8.1, and recovery rates were compared. It was noticed and confirmed that Waters Oasis HLB had shown the best recovery results for most of the common testing samples among all three styrenedivinylbenzene (SDB) polymer sorbents, which were 77% on average. Furthermore, Waters SepPak AC-2 provided good recovery results for pesticides among three types of activated carbon sorbents and the average recovery rates reached 74%. Therefore, Waters Oasis HLB and Waters SepPak AC-2 were combined to obtain a better recovery and the average recovery rate for the tested 40 compounds of this new SPE method was 87%.

  15. Enhancement in extraction rates by addition of organic acids to aqueous phase in solvent extraction of rare earth metals in presence of diethylenetriaminepentaacetic acid

    International Nuclear Information System (INIS)

    Matsuyama, Hideto; Azis, A.; Fujita, Mamoru; Teramoto, Masaaki.

    1996-01-01

    It is well known that the selectivity of rare earth metals by solvent extraction is increased by the addition of a chelating agent such as diethylenetriaminepentaacetic acid (DTPA) in the aqueous phase. One of the disadvantages of this method is the decrease in extraction rates due to complexation in the aqueous phase. In this paper, further addition of organic acids to the aqueous phase was examined for the purpose of enhancing the extraction rates in solvent extraction with DTPA. The addition of several kind of organic acids such as formic acid, acetic acid, malonic acid, lactic acid and citric acid was investigated for a Er/Y separation system. A remarkable enhancement in extraction rates was observed with a slight decrease in the selectivity by the addition of citric acid or lactic acid. Extraction rates in the presence of both DTPA and citric acid increased with the increase in citric acid concentration and with the increase in proton concentration. A 150 times enhancement in extraction rates was found in the low proton concentration condition. In order to analyze the extraction rates and selectivities obtained, mass transfer equations were presented by considering both the dissociation reaction of rare earth metal-DTPA complexes and the complex formation between rare earth metal and organic acid in the aqueous phase. The experimental data were analyzed by these equations. (author)

  16. Sorption behavior of charged and neutral polar organic compounds on solid phase extraction materials: which functional group governs sorption?

    NARCIS (Netherlands)

    Bäuerlein, P.S.; Mansell, J.E.; ter Laak, T.L.; de Voogt, P.

    2012-01-01

    Numerous polar anthropogenic organic chemicals have been found in the aqueous environment. Solid phase extraction (SPE) has been applied for the isolation of these from aqueous matrices, employing various materials. Nevertheless, little is known about the influence of functional groups on the

  17. Simultaneous quantification of dissolved organic carbon fractions and copper complexation using solid-phase extraction

    International Nuclear Information System (INIS)

    McElmurry, Shawn P.; Long, David T.; Voice, Thomas C.

    2010-01-01

    Trace metal cycling in natural waters is highly influenced by the amount and type of dissolved organic C (DOC). Although determining individual species of DOC is unrealistic, there has been success in classifying DOC by determining operationally defined fractions. However, current fractionation schemes do not allow for the simultaneous quantification of associated trace metals. Using operational classifications, a scheme was developed to fractionate DOC based on a set of seven solid-phase extraction (SPE) cartridges. The cartridges isolated fractions based on a range of specific mechanisms thought to be responsible for DOC aggregation in solution, as well as molecular weight. The method was evaluated to determine if it can identify differences in DOC characteristics, including differences in Cu-DOC complexation. Results are that: (1) cartridge blanks were low for both DOC and Cu, (2) differences are observed in the distribution of DOC amongst the fractions from various sources that are consistent with what is known about the DOC materials and the mechanisms operative for each cartridge, (3) when present as a free cation, Cu was not retained by non-cationic cartridges allowing the method to be used to assess Cu binding, (4) the capability of the method to provide quantitative assessment of Cu-DOC complexation was demonstrated for a variety of DOC standards, (5) Cu was found to preferentially bind with high molecular weight fractions of DOC, and (6) estimated partitioning coefficients and conditional binding constants for Cu were similar to those reported elsewhere. The method developed describes DOC characteristics based on specific bonding mechanisms (hydrogen, donor-acceptor, London dispersion, and ionic bonding) while simultaneously quantifying Cu-DOC complexation. The method provides researchers a means of describing not only the extent of DOC complexation but also how that complex will be behave in natural waters.

  18. Head Space Solid Phase Micro-Extraction (HS - SPME of volatile organic compounds produced by Sporidiobolus salmonicolor (CBS 2636

    Directory of Open Access Journals (Sweden)

    Eunice Valduga

    2010-12-01

    Full Text Available The aim of the present study was the assessment of volatile organic compounds produced by Sporidiobolus salmonicolor (CBS 2636 using methyl and ethyl ricinoleate, ricinoleic acid and castor oil as precursors. The analysis of the volatile organic compounds was carried out using Head Space Solid Phase Micro-Extraction (HS - SPME. Factorial experimental design was used for investigating extraction conditions, verifying stirring rate (0-400 rpm, temperature (25-60 ºC, extraction time (10-30 minutes, and sample volume (2-3 mL. The identification of volatile organic compounds was carried out by Gas Chromatography with Mass Spectrum Detector (GC/MSD. The conditions that resulted in maximum extraction were: 60 ºC, 10 minutes extraction, no stirring, sample volume of 2.0 mL, and addition of saturated KCl (1:10 v/v. In the bio-production of volatile organic compounds the effect of stirring rate (120-200 rpm, temperature (23-33 ºC, pH (4.0-8.0, precursor concentration (0.02-0.1%, mannitol (0-6%, and asparagine concentration (0-0.2% was investigated. The bio-production at 28 ºC, 160 rpm, pH 6,0 and with the addition of 0.02% ricinoleic acid to the medium yielded the highest production of VOCs, identified as 1,4-butanediol, 1,2,2-trimethylciclopropilamine, beta-ionone; 2,3-butanodione, pentanal, tetradecane, 2-isononenal, 4-octen-3-one, propanoic acid, and octadecane.

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

    Energy Technology Data Exchange (ETDEWEB)

    Fiscal-Ladino, Jhon A.; Obando-Ceballos, Mónica; Rosero-Moreano, Milton [Grupo de Investigación en Cromatografía y Técnicas Afines GICTA, Departamento de Química, Facultad de Ciencias Exactas y Naturales, Universidad de Caldas, Calle 65 No. 26-10, Manizales (Colombia); Montaño, Diego F.; Cardona, Wilson; Giraldo, Luis F. [Química de Plantas Colombianas, Instituto de Química, Escuela de Ciencias Exactas y Naturales, Universidad de Antioquia, Calle 70 No. 52-21, A.A, 1226, Medellín (Colombia); Richter, Pablo, E-mail: prichter@ciq.uchile.cl [Departamento de Química Inorgánica y Analítica, Facultad de Ciencias Químicas y Farmacéuticas, Universidad de Chile, Casilla 233, Santiago (Chile)

    2017-02-08

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

  20. Magnetic metal-organic frameworks for fast and efficient solid-phase extraction of six Sudan dyes in tomato sauce.

    Science.gov (United States)

    Shi, Xin-Ran; Chen, Xue-Lei; Hao, Yu-Lan; Li, Li; Xu, Hou-Jun; Wang, Man-Man

    2018-06-01

    Magnetic solid-phase extraction is an effective and useful technique to preconcentrate trace analytes from food samples. In this study, a magnetic trimeric chromium octahedral metal-organic framework (Fe 3 O 4 -NH 2 @MIL-101) was fabricated and characterized. Fe 3 O 4 -NH 2 @MIL-101 was applied as an adsorbent of magnetic solid-phase extraction combined with high performance liquid chromatography to effectively isolate and simultaneously determine six Sudan dyes (Para Red, Sudan I-IV, and Sudan Red 7B) from tomato sauce. Potential factors affecting the MSPE were investigated in detail, and adsorption efficiency of Fe 3 O 4 -NH 2 @MIL-101 was compared with those of conventional adsorbents, such as neutral alumina, HLB, and C 18 . The developed method facilitated the extraction with using only 3 mg of adsorbent in 2 min. In addition, enhancement factors of 50, linear range of 0.01-25 μg/mL, and detection limit (S/N = 3) of 0.5-2.5 μg/kg were obtained. The intra-day and inter-day recoveries for spiked Sudan dyes were in the range of 72.6%-92.9% and 69.6%-91.6%, respectively, with relative standard deviations of ≤9.2%. Copyright © 2018 Elsevier B.V. All rights reserved.

  1. Pyrolytic in situ magnetization of metal-organic framework MIL-100 for magnetic solid-phase extraction.

    Science.gov (United States)

    Huo, Shu-Hui; An, Hai-Yan; Yu, Jing; Mao, Xue-Feng; Zhang, Zhe; Bai, Lei; Huang, Yan-Feng; Zhou, Peng-Xin

    2017-09-29

    In this study, we report a facile, environmental friendly fabrication of a type of magnetic metal-organic framework (MOF) MIL-100 that can be used for magnetic solid-phase extraction (MSPE). The magnetic MOF composites were fabricated using in situ calcination method. The as-synthesized materials exhibited both high porosity and magnetic characteristics. They used for the MSPE of polycyclic aromatic hydrocarbons (PAHs) from water samples. Such MOF-based magnetic solid-phase extraction in combination with gas chromatography equipped with a flame ionization detector (GC-FID), exhibited wide linearity (0.02-250μgL -1 ), low detection limits (4.6-8.9ngL -1 ), and high enrichment factors (452-907) for PAHs. The relative standard deviations (RSDs) for intra- and inter-day extractions of PAHs were ranging from 1.7% to 9.8% and 3.8% to 9.2%, respectively. The recoveries for spiked PAHs (1μgL -1 ) in water samples were in the range of 88.5% to 106.6%. The results showed that the special anion-π orbital (electron donor-acceptor) interaction and π-π stacking between magnetic MIL-100 and PAHs play an important role in the adsorption of PAHs. Copyright © 2017. Published by Elsevier B.V.

  2. Third phase formation in organic solutions in the extraction of mono-acids by tertiary trialcoyl-amines diluted in very slightly polar organic solvents

    International Nuclear Information System (INIS)

    Robaglia, Michele

    1973-01-01

    The phenomena of third phase formation which can occur during the extraction of an acid with a tertiary amine diluted in a low polarity diluent are studied. In the first part a system including water (TnOA - C 6 H 12 - HCl - H 2 O) is compared with an anhydrous system (TnOA - C 6 H 12 - HCl - N 2 ). There are two kinds of gaps. One during amine salification, another one during the extraction of excess acid. The important part of the water content of the organic phase is demonstrated. The presence of water enhances the gaps. The polar water molecules are dissolved inside the tri-octylamine salt micelles. The heavy phase is formed by aggregates, the light phase represents the solubility of the non soluble species in the medium. In the second part are studied the influence of some parameters (like nature of diluent, acid, amine and temperature) on the gaps formation and on the extraction of excess acid and water. In every cases the part played by water remains the same. Finally some comparisons are made between tertiary systems and binary systems which formed them. The binary systems were studied by the mean of crystallization curves. (author) [fr

  3. Solid phase extraction membrane

    Science.gov (United States)

    Carlson, Kurt C [Nashville, TN; Langer, Roger L [Hudson, WI

    2002-11-05

    A wet-laid, porous solid phase extraction sheet material that contains both active particles and binder and that possesses excellent wet strength is described. The binder is present in a relatively small amount while the particles are present in a relatively large amount. The sheet material is sufficiently strong and flexible so as to be pleatable so that, for example, it can be used in a cartridge device.

  4. Liquid-liquid extraction of ruthenium(III) thiocyanate with hexamethylphosphoramide: direct spectrophotometric determination in the organic phase

    International Nuclear Information System (INIS)

    Mitra, B.K.; Pal, B.K.; Chowdhury, R.P.

    1982-01-01

    Ru(III) thiocyanate has been extracted with hexamethylphosphoramide(HMPA) in methyl isobutyl ketone (MIBK). Thus the extractability, sensitivity and selectivity are improved over the simple binary Ru(III) thiocyanate system in spectrophotometric determination of ruthenium in the organic phase. The maximum colour develops on the steam bath, at the acidity range of 1.5 - 2.5 M with HCl and ammonium thiocyanate concentration range of 0.25 - O.5 M. The colour is completely extractable in MIBK when 1.5 - 3.0 ml HMPA is used and show maximum absorbance at 570 nm. The colour system obeys Beer's law for 0.7 - 13 μg Ru/ml and the optimum concentration range is 2 - 13 μg/ml. The molar absorptivity and sensitivity are 6940 l . mole -1 cm -1 and 0.0145 μg/cm 2 respectively. The percent relative error is 2.72%. The method is very simple and does not require oxidation and subsequent distillation. The method can be applied in the presence of osmium. (Author)

  5. Organic Contaminants Associated with the Extraction of Unconventional Gas. Risk Analysis in the Initial Phases of the Project

    International Nuclear Information System (INIS)

    Xu, L.; Hurtado, A.; Recreo, F.; Eguilior, S.

    2015-01-01

    The latest technological advances in hydraulic fracturing and horizontal drilling are promoting a commercial scale extraction of unconventional fossil fuels in several regions of the world. Although there is still no commercial scale extraction in the Member States of the EU, potential stocks in some of them, as in the case of Spain, stimulate the need to carry out precautionary previous studies. These, based on the experience in the USA, will allow to define the characteristics that a priori should include a project of unconventional gas extraction, so that their safety is maximized by minimizing the likelihood of adverse effects on the environment. In unconventional gas production a fracturing fluid, typically water, with different types of additives is injected into the reservoir at very high pressure in order to create fractures to increase the porosity and permeability of the rock. In this scenario the flowback and produced water (water brought to the surface during the extraction of gas or oil) is usually a mixture of fluids injected and brines present in the repository. The quality of the flowback and produced water is variable. Its salinity varies from similar to drinking water to several times more saline than seawater. Furthermore, different compounds other than salt can be present in various amounts in the flowback and produced water: oil and other organic compounds, solids in suspension, bacteria, naturally occurring radioactive elements (NORM), and any of the elements injected with the hydraulic fracturing fluid. Due to the high variability of contaminants in the flowback and produced water as well as potentially large volumes involved, composition of flowback and produced water and the analysis of the risks associated with them is an important aspect to consider from the initial phases of project development of unconventional gas extraction. This report covers the risk analysis of an unconventional gas extraction project, the initial assessment of the

  6. The use of solid sorbents for direct accumulation of organic compounds from water matrices : a review of solid-phase extraction techniques

    NARCIS (Netherlands)

    Liska, I.; Krupcik, J.; Leclercq, P.A.

    1989-01-01

    The main principles of solid-phase extraction techniques are reviewed in this paper. Various solid sorbents can be used as a suitable trap for direct accumulation of organic compounds from aqueous solutions. The trapped analytes can be desorbed by elution with suitably chosen liquid phases. These

  7. Analysis of Mars Analogue Soil Samples Using Solid-Phase Microextraction, Organic Solvent Extraction and Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Orzechowska, G. E.; Kidd, R. D.; Foing, B. H.; Kanik, I.; Stoker, C.; Ehrenfreund, P.

    2011-01-01

    Polycyclic aromatic hydrocarbons (PAHs) are robust and abundant molecules in extraterrestrial environments. They are found ubiquitously in the interstellar medium and have been identified in extracts of meteorites collected on Earth. PAHs are important target molecules for planetary exploration missions that investigate the organic inventory of planets, moons and small bodies. This study is part of an interdisciplinary preparation phase to search for organic molecules and life on Mars. We have investigated PAH compounds in desert soils to determine their composition, distribution and stability. Soil samples (Mars analogue soils) were collected at desert areas of Utah in the vicinity of the Mars Desert Research Station (MDRS), in the Arequipa region in Peru and from the Jutland region of Denmark. The aim of this study was to optimize the solid-phase microextraction (SPME) method for fast screening and determination of PAHs in soil samples. This method minimizes sample handling and preserves the chemical integrity of the sample. Complementary liquid extraction was used to obtain information on five- and six-ring PAH compounds. The measured concentrations of PAHs are, in general, very low, ranging from 1 to 60 ng g(sup -1). The texture of soils is mostly sandy loam with few samples being 100% silt. Collected soils are moderately basic with pH values of 8-9 except for the Salten Skov soil, which is slightly acidic. Although the diverse and variable microbial populations of the samples at the sample sites might have affected the levels and variety of PAHs detected, SPME appears to be a rapid, viable field sampling technique with implications for use on planetary missions.

  8. Using solid phase micro extraction to determine salting-out (Setschenow) constants for hydrophobic organic chemicals.

    NARCIS (Netherlands)

    Jonker, M.T.O.; Muijs, B.

    2010-01-01

    With increasing ionic strength, the aqueous solubility and activity of organic chemicals are altered. This so-called salting-out effect causes the hydrophobicity of the chemicals to be increased and sorption in the marine environment to be more pronounced than in freshwater systems. The process can

  9. Development of an on-line analyzer for organic phase uranium concentration in extraction process

    International Nuclear Information System (INIS)

    Dong Yanwu; Song Yufen; Zhu Yaokun; Cong Peiyuan; Cui Songru

    1998-10-01

    The working principle, constitution, performance of an on-line analyzer and the development characteristic of immersion sonde, data processing system and examination standard are reported. The performance of this instrument is reliable. For identical sample, the signal fluctuation in continuous monitoring for four months is less than +-1%. According to required measurement range by choosing appropriate length of sample cell the precision of measurement is better than 1% at uranium concentration 100 g/L. The detection limit is (50 +- 10) mg/L. The uranium concentration in process stream can be automatically displayed and printed out in real time and 4∼20 mA current signal being proportional to the uranium concentration can be presented. So the continuous control and computer management for the extraction process can be achieved

  10. Multi-layer solid-phase extraction and evaporation-enrichment methods for polar organic chemicals from aqueous matrices.

    Science.gov (United States)

    Köke, Niklas; Zahn, Daniel; Knepper, Thomas P; Frömel, Tobias

    2018-03-01

    Analysis of polar organic chemicals in the aquatic environment is exacerbated by the lack of suitable and widely applicable enrichment methods. In this work, we assessed the suitability of a novel combination of well-known solid-phase extraction (SPE) materials in one cartridge as well as an evaporation method and for the enrichment of 26 polar model substances (predominantly log D evaporation method were investigated for the recovery and matrix effects of the model substances and analyzed with hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS). In total, 65% of the model substances were amenable (> 10% recovery) to the mlSPE method with a mean recovery of 76% while 73% of the model substances were enriched with the evaporation method achieving a mean recovery of 78%. Target and non-target screening comparison of both methods with a frequently used reversed-phase SPE method utilizing "hydrophilic and lipophilic balanced" (HLB) material was performed. Target analysis showed that the mlSPE and evaporation method have pronounced advantages over the HLB method since the HLB material retained only 30% of the model substances. Non-target screening of a ground water sample with the investigated enrichment methods showed that the median retention time of all detected features on a HILIC system decreased in the order mlSPE (3641 features, median t R 9.7 min), evaporation (1391, 9.3 min), HLB (4414, 7.2 min), indicating a higher potential of the described methods to enrich polar analytes from water compared with HLB-SPE. Graphical abstract Schematic of the method evaluation (recovery and matrix effects) and method comparison (target and non-target analysis) of the two investigated enrichment methods for very polar chemicals in aqueousmatrices.

  11. Utilizing thin-film solid-phase extraction to assess the effect of organic carbon amendments on the bioavailability of DDT and dieldrin to earthworms

    Science.gov (United States)

    Improved approaches are needed to rapidly and accurately assess the bioavailability of persistent, hydrophobic organic compounds in soils at contaminated sites. The performance of a thin-film solid-phase extraction (TF-SPE) assay using vials coated with ethylene vinyl acetate polymer was compared to...

  12. New sorbent in the dispersive solid phase extraction step of quick, easy, cheap, effective, rugged, and safe for the extraction of organic contaminants in drinking water treatment sludge.

    Science.gov (United States)

    Cerqueira, Maristela B R; Caldas, Sergiane S; Primel, Ednei G

    2014-04-04

    Recent studies have shown a decrease in the concentration of pesticides, pharmaceuticals and personal care products (PCPs) in water after treatment. A possible explanation for this phenomenon is that these compounds may adhere to the sludge; however, investigation of these compounds in drinking water treatment sludge has been scarce. The sludge generated by drinking water treatment plants during flocculation and decantation steps should get some special attention not only because it has been classified as non-inert waste but also because it is a very complex matrix, consisting essentially of inorganic (sand, argil and silt) and organic (humic substances) compounds. In the first step of this study, three QuEChERS methods were used, and then compared, for the extraction of pesticides (atrazine, simazine, clomazone and tebuconazole), pharmaceuticals (amitriptyline, caffeine, diclofenac and ibuprofen) and PCPs (methylparaben, propylparaben, triclocarban and bisphenol A) from drinking water treatment sludge. Afterwards, the study of different sorbents in the dispersive solid phase extraction (d-SPE) step was evaluated. Finally, a new QuEChERS method employing chitin, obtained from shrimp shell waste, was performed in the d-SPE step. After having been optimized, the method showed limits of quantification (LOQ) between 1 and 50 μg kg(-1) and the analytical curves showed r values higher than 0.98, when liquid chromatography tandem mass spectrometry was employed. Recoveries ranged between 50 and 120% with RSD≤15%. The matrix effect was evaluated and compensated with matrix-matched calibration. The method was applied to drinking water treatment sludge samples and methylparaben and tebuconazole were found in concentration

  13. 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

  14. Solid-phase extraction element based on epoxy polymer monolith for determination of polar organic compounds in aqueous media.

    Science.gov (United States)

    Takahashi, Tadashi; Odagiri, Kayo; Watanabe, Atsushi; Watanabe, Chuichi; Kubo, Takuya; Hosoya, Ken

    2011-10-01

    A solid-phase extraction element based on epoxy polymer monolith was fabricated for sorptive enrichment of polar compounds from liquid and gaseous samples. After ultrasonication of the element in an aqueous solution for a given period of time, the thermal desorption (TD) using a pyrolyzer with gas chromatography/mass spectrometry (GC/MS), in which TD temperature was programmed from 50 to 250 °C for the analytes absorbed in the element, was used to evaluate the element for basic extraction performance using the aqueous standard mixtures consisting of compounds having varied polarities such as hexanol, isoamyl acetate, linalool, furfural and decanoic acid, in concentrations ranging from 10 μg/L to 1 mg/L. Excellent linear relationships were observed for all compounds in the standard mixture, except decanoic acid. In the extraction of beverages such as red wine, the extraction element showed stronger adsorption characteristics for polar compounds such as alcohols and acids than a non-polar polydimethylsiloxane-based element. This feature is derived from the main polymer structure along with hydroxyl and amino groups present in the epoxy-based monolith polymer matrix. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Metal-organic framework based in-syringe solid-phase extraction for the on-site sampling of polycyclic aromatic hydrocarbons from environmental water samples.

    Science.gov (United States)

    Zhang, Xiaoqiong; Wang, Peiyi; Han, Qiang; Li, Hengzhen; Wang, Tong; Ding, Mingyu

    2018-04-01

    In-syringe solid-phase extraction is a promising sample pretreatment method for the on-site sampling of water samples because of its outstanding advantages of portability, simple operation, short extraction time, and low cost. In this work, a novel in-syringe solid-phase extraction device using metal-organic frameworks as the adsorbent was fabricated for the on-site sampling of polycyclic aromatic hydrocarbons from environmental waters. Trace polycyclic aromatic hydrocarbons were effectively extracted through the self-made device followed by gas chromatography with mass spectrometry analysis. Owing to the excellent adsorption performance of metal-organic frameworks, the analytes could be completely adsorbed during one adsorption cycle, thus effectively shortening the extraction time. Moreover, the adsorbed analytes could remain stable on the device for at least 7 days, revealing the potential of the self-made device for on-site sampling of degradable compounds in remote regions. The limit of detection ranged from 0.20 to 1.9 ng/L under the optimum conditions. Satisfactory recoveries varying from 84.4 to 104.5% and relative standard deviations below 9.7% were obtained in real samples analysis. The results of this study promote the application of metal-organic frameworks in sample preparation and demonstrate the great potential of in-syringe solid-phase extraction for the on-site sampling of trace contaminants in environmental waters. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. 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.

  17. Hydrolysis in the organic phase during the extraction of alkali metal halides and water by copper bis(2-ethylhexyl)phosphate

    International Nuclear Information System (INIS)

    Golovanov, V.I.; Kuznetsov, S.M.

    2001-01-01

    Experimental data on extraction of halides, among which are LiCl and CsCl, and water by copper di-(2-ethylhexyl)phosphate solutions in respect to hydrolysis mechanism of reaction are generalized. Copper di-(2-ethylhexyl)phosphate manifests properties of ionogen colloidal surfactant in water. Extraction of halides by copper di-(2-ethylhexyl)phosphate was shown to be visualized by the process of capsule formation in MHal molecules, as well as in hydrolyzed MOH and HHal forms of electrolyte by Cu 4 (D2EHF) 8 · hH 2 O clathrate-like micellar associates. The model of hydrolysis mechanism is not different from proposed earlier model of electrolyte extraction with their partial dissociation in organic phase [ru

  18. Influence of the organic phase property on the extraction of tenoil - trifluoroacetonate uranyl, Annex 6; Prilog 6: Uticaj prirode organske faze na ekstrakciju tenoil - trifluoracetonata uranila

    Energy Technology Data Exchange (ETDEWEB)

    Milic, N; Petruhin, O M; Zolotov, J A [Institute of Nuclear Sciences Boris Kidric, Laboratorija za visoku aktivnost, Vinca, Beograd (Serbia and Montenegro)

    1963-12-15

    This paper describes the study of of uranium (VI) (2.5 10{sup -4}M) extraction from acetate puffer solutions with 0.01 M solution of tenoil trifluoroacetonate in benzene, chloroform, carbon tetrachloride, amyl acetate, cyclohexanon, n-butyl alcohol with the additions of 0.036 M TBP and 2.7 M acetone solution with 0.01 M solution of TTA. It was verified that the extraction depends on the property of the organic phase. Distribution coefficients for uranium when extracted by solvents containing oxygen is higher compared to the distribution coefficients obtained by solvents without oxygen (benzene, chloroform and carbon tetrachloride). TBP cyclohexanon, and acetone additions in the CCl{sub 4} cause more significant increase of distribution coefficients.

  19. Zinc and palladium traces separation from uranium by tri-n-octylamine extraction. Direct determination in organic phase by atomic absorption

    Energy Technology Data Exchange (ETDEWEB)

    de Moraes, S; Cipriani, M; Abrao, A

    1974-12-01

    A procedure for the extraction and determination of Zn and Pd as traces from nuclear grade uranium ADU, UO/sub 2/, UO/sub 3/, U/sub 3/O/sub 8/ is introduced. The elements are extracted from UO/sub 2/Cl/sub 2/-HCl-KI solution with tri-n-octylamine in benzene and determined by atomic absorption spectrophotometry. The adition of potassium iodide to the UO/sub 2/Cl/sub 2/-HCl solutions improved the extraction of both elements. Direct burn of the organic phase in the atomic absorption spectrophotometer using hydrogen-air flame provided enhancement of the absorbance for both elements. The relative standard deviations were Zn, 3% and Pd, 2.9%.

  20. Screening of a Combinatorial Library of Organic Polymers for the Solid-Phase Extraction of Patulin from Apple Juice

    Science.gov (United States)

    Giovannoli, Cristina; Spano, Giulia; Di Nardo, Fabio; Anfossi, Laura; Baggiani, Claudio

    2017-01-01

    Patulin is a water-soluble mycotoxin produced by several species of fungi. Governmental bodies have placed it under scrutiny for its potential negative health effects, and maximum residue limits are fixed in specific food matrices to protect consumers’ health. Confirmatory analysis of patulin in complex food matrices can be a difficult task, and sample clean-up treatments are frequently necessary before instrumental analyses. With the aim of simplifying the clean-up step, we prepared a 256-member combinatorial polymeric library based on 16 functional monomers, four cross-linkers and four different porogenic solvents. The library was screened for the binding towards patulin in different media (acetonitrile and citrate buffer at pH 3.2), with the goal of identifying polymer formulations with good binding properties towards the target compound. As a proof of concept, a methacrylic acid-co-pentaerithrytole tetraacrylate polymer prepared in chloroform was successfully used as a solid-phase extraction material for the clean-up and extraction of patulin from apple juice. Clean chromatographic patterns and acceptable recoveries were obtained for juice spiked with patulin at concentration levels of 25 (64 ± 12%), 50 (83 ± 5.6%) and 100 μg L−1 (76 ± 4.5%). The within-day and between-day reproducibility evaluated at a concentration level of 25 μg L−1 were 5.6 and 7.6%, respectively. PMID:28531103

  1. Use of chelating agents as immovable phase in extraction chromatography

    International Nuclear Information System (INIS)

    Sebesta, F.

    1978-01-01

    Extraction chromatography using chelating agents is reviewed. The theory of element extraction by chelating agents and factors influencing this process (pH, extracting agent concentration in organic phase, masking agent concentration in aqueous phase) are briefly considered. The effect of kinetic factors on the extraction chromatography process is discussed. Ways of preparing columns are emphasized. Examples of using chelating reagents in various extraction chromatography systems are given. β-Diketones, oximes, hydroxamic acids, dithizon, diethyl dithiocarbamic acid are chosen as chelating agents

  2. Utilizing thin-film solid-phase extraction to assess the effect of organic carbon amendments on the bioavailability of DDT and dieldrin to earthworms

    Science.gov (United States)

    Andrade, Natasha A.; Centofanti, Tiziana; McConnell, Laura L.; Hapeman, Cathleen J.; Torrents, Alba; Anh, Nguyen; Beyer, W. Nelson; Chaney, Rufus L.; Novak, Jeffrey M.; Anderson, Marya O.; Cantrell, Keri B.

    2014-01-01

    Improved approaches are needed to assess bioavailability of hydrophobic organic compounds in contaminated soils. Performance of thin-film solid-phase extraction (TF-SPE) using vials coated with ethylene vinyl acetate was compared to earthworm bioassay (Lumbricus terrestris). A DDT and dieldrin contaminated soil was amended with four organic carbon materials to assess the change in bioavailability. Addition of organic carbon significantly lowered bioavailability for all compounds except for 4,4′-DDT. Equilibrium concentrations of compounds in the polymer were correlated with uptake by earthworms after 48d exposure (R2 = 0.97; p 40yr of aging. Results show that TF-SPE can be useful in examining potential risks associated with contaminated soils and to test effectiveness of remediation efforts.

  3. Determination of residual volatile organic compounds migrated from polystyrene food packaging into food simulant by headspace solid phase micro extraction-gas chromatography

    International Nuclear Information System (INIS)

    Mohd Marsin Sanagi; Ling, Susie Lu; Zalilah Nasir; Wan Aini Wan Ibrahim; Abu Naim, Ahmedy

    2008-01-01

    The residual styrene and other volatile organic compounds (VOCs) present in the polystyrene food packaging are of concern as these compounds have the potential to migrate into the food in contact. This work describes a method for quantitative determination of VOCs, namely styrene, toluene, ethyl benzene, iso-propylbenzene and n-propylbenzene that have migrated from polystyrene food packaging into food stimulant by gas chromatography-flame ionization detection (GC-FID). Headspace solid phase micro extraction (HS-SPME) technique was applied for migration test using water as food stimulant. The effects of extraction variables including sample volume, eluotropic strength, extraction temperature, extraction time, desorption time, sample agitation, and salt addition on the amounts of the extracted analyses were studied to obtain the optimal HS-SPME conditions. The optimized method was applied to test the VOCs migrated from polystyrene bowls and cups at storage temperatures ranging from 24 to 80 degree Celsius for 30 min. Styrene and ethyl benzene were found to migrate from the samples into the food stimulant. The migration of analyze was found to be strongly dependent upon the storage temperature. The HS-SPME is useful as an alternative method to determine the migration of VOCs from food packaging material into food stimulant. (author)

  4. Core-shell indium (III) sulfide@metal-organic framework nanocomposite as an adsorbent for the dispersive solid-phase extraction of nitro-polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Jia, Yuqian; Zhao, Yanfang; Zhao, Mei; Wang, Zhenhua; Chen, Xiangfeng; Wang, Minglin

    2018-05-25

    A core-shell discoid shaped indium (III) sulfide@metal-organic framework (MIL-125(Ti)) nanocomposite was synthesized by a solvothermal method and explored as an adsorbent material for dispersive solid-phase extraction (d-SPE). The as-synthesized sorbent was characterized by scanning electron microscopy, energy-dispersive spectroscopy, transmission electron microscopy, powder X-ray diffraction, N 2 adsorption-desorption analysis, and Fourier transform infrared spectroscopy. The extraction performance was evaluated by the d-SPE of 16 nitro-polycyclic aromatic hydrocarbons (NPAHs) from water samples. The analysis was carried out by gas chromatography (GC) coupled with triple quadruple mass spectrometer in negative chemical ionization (NCI) mode. The selected ion monitoring (SIM) was used in the quantification of the target NPAHs. Extraction factors affecting the d-SPE, including the ionic strength, extraction temperature, and extraction time were optimized by the response surface methodology. The developed d-SPE method showed good linear correlations from 10 to 1000 ng L -1 (r > 0.99), low detection limits (2.9-83.0 ng L -1 ), satisfactory repeatability (relative standard deviation of <10%, n = 6), and acceptable recoveries (71.3%-112.2%) for water samples. The developed method was used for the food and environmental sample analysis. The results demonstrated that the method could be used for sample preparation of trace NPAHs in real samples. Copyright © 2018. Published by Elsevier B.V.

  5. Polymeric Sorbent with Controlled Surface Polarity: An Alternate for Solid-Phase Extraction of Nerve Agents and Their Markers from Organic Matrix.

    Science.gov (United States)

    Roy, Kanchan Sinha; Purohit, Ajay Kumar; Chandra, Buddhadeb; Goud, D Raghavender; Pardasani, Deepak; Dubey, Devendra Kumar

    2018-06-05

    Extraction and identification of lethal nerve agents and their markers in complex organic background have a prime importance from the forensic and verification viewpoint of the Chemical Weapons Convention (CWC). Liquid-liquid extraction with acetonitrile and commercially available solid phase silica cartridges are extensively used for this purpose. Silica cartridges exhibit limited applicability for relatively polar analytes, and acetonitrile extraction shows limited efficacy toward relatively nonpolar analytes. The present study describes the synthesis of polymeric sorbents with tunable surface polarity, their application as a solid-phase extraction (SPE) material against nerve agents and their polar as well as nonpolar markers from nonpolar organic matrices. In comparison with the acetonitrile extraction and commercial silica cartridges, the new sorbent showed better extraction efficiency toward analytes of varying polarity. The extraction parameters were optimized for the proposed method, which included ethyl acetate as an extraction solvent and n-hexane as a washing solvent. Under optimized conditions, method linearity ranged from 0.10 to 10 μg mL -1 ( r 2 = 0.9327-0.9988) for organophosphorus esters and 0.05-20 μg mL -1 ( r 2 = 0.9976-0.9991) for nerve agents. Limits of detection (S:N = 3:1) in the SIM mode were found in the range of 0.03-0.075 μg mL -1 for organophosphorus esters and 0.015-0.025 μg mL -1 for nerve agents. Limits of quantification (S:N = 10:1) were found in the range of 0.100-0.25 μg mL -1 for organophosphorus esters and 0.05-0.100 μg mL -1 for nerve agents in the SIM mode. The recoveries of the nerve agents and their markers ranged from 90.0 to 98.0% and 75.0 to 95.0% respectively. The repeatability and reproducibility (with relative standard deviations (RSDs) %) for organophosphorus esters were found in the range of 1.35-8.61% and 2.30-9.25% respectively. For nerve agents, the repeatability range from 1.00 to 7.75% and reproducibility

  6. A tri-metal centered metal-organic framework for solid-phase microextraction of environmental contaminants with enhanced extraction efficiency

    International Nuclear Information System (INIS)

    Liu, Shuqin; Xie, Lijun; Hu, Qingkun; Yang, Huangsheng; Pan, Guanrui; Zhu, Fang; Yang, Shenghong; Ouyang, Gangfeng

    2017-01-01

    This study presents the preparation and the characterizations of six tri-metal centered metal-organic frameworks (tM-MOFs) as solid-phase microextraction (SPME) adsorbents. Possessing different proportions of Al, Ga and In atoms in their frameworks, the tM-MOF-based SPME coatings exhibited different extraction performance towards the organic pollutants. Extraction results showed that the M4 (Al 0.593 Ga 0.167 In 0.240 (O 2 C 2 H 4 )(h 2 fipbb)) coating exhibited the best enrichment ability among six tM-MOFs. In addition, it showed better extraction efficiency towards the analytes than three single-metal centered MOFs coatings and a commercial polydimethylsiloxane (PDMS) coating. The adsorption process of the M4 coating was physical adsorption and it was mainly affected by the diffusion process of the compound from the sample to the material, which is the same with the adsorption processes of the single-metal centered MOFs coatings. Under optimal conditions (extraction time, 3 min; NaCl concentration, 25% (w/v); desorption temperature, 270 °C; extraction temperature, 30 °C), the M4 coating achieved low detection limits (0.13–0.88 ng L −1 ) and good linearity (5–2000 and 5–5000 ng L −1 ) for benzene series compounds. The repeatabilities (n = 5) for single fiber were between 4.3 and 8.1%, while the reproducibilities (n = 3) of fiber-to-fiber were in the range of 7.9–12.7%. Finally, a M4 coated SPME fiber was successfully applied to the analysis of environmental water samples with satisfactory recoveries (80.8%–119.5%). - Highlights: • Six tri-metal centered metal-organic frameworks were synthesized and characterized. • Novel SPME fibers were fabricated with silicone sealant film and tri-metal centered metal-organic frameworks crystals. • The self-made fiber exhibited excellent extraction performance to organic pollutants. • The self-made fiber was used for analysis of benzene series compounds in environmental water samples.

  7. Submicrometric Magnetic Nanoporous Carbons Derived from Metal-Organic Frameworks Enabling Automated Electromagnet-Assisted Online Solid-Phase Extraction.

    Science.gov (United States)

    Frizzarin, Rejane M; Palomino Cabello, Carlos; Bauzà, Maria Del Mar; Portugal, Lindomar A; Maya, Fernando; Cerdà, Víctor; Estela, José M; Turnes Palomino, Gemma

    2016-07-19

    We present the first application of submicrometric magnetic nanoporous carbons (μMNPCs) as sorbents for automated solid-phase extraction (SPE). Small zeolitic imidazolate framework-67 crystals are obtained at room temperature and directly carbonized under an inert atmosphere to obtain submicrometric nanoporous carbons containing magnetic cobalt nanoparticles. The μMNPCs have a high contact area, high stability, and their preparation is simple and cost-effective. The prepared μMNPCs are exploited as sorbents in a microcolumn format in a sequential injection analysis (SIA) system with online spectrophotometric detection, which includes a specially designed three-dimensional (3D)-printed holder containing an automatically actuated electromagnet. The combined action of permanent magnets and an automatically actuated electromagnet enabled the movement of the solid bed of particles inside the microcolumn, preventing their aggregation, increasing the versatility of the system, and increasing the preconcentration efficiency. The method was optimized using a full factorial design and Doehlert Matrix. The developed system was applied to the determination of anionic surfactants, exploiting the retention of the ion-pairs formed with Methylene Blue on the μMNPC. Using sodium dodecyl sulfate as a model analyte, quantification was linear from 50 to 1000 μg L(-1), and the detection limit was equal to 17.5 μg L(-1), the coefficient of variation (n = 8; 100 μg L(-1)) was 2.7%, and the analysis throughput was 13 h(-1). The developed approach was applied to the determination of anionic surfactants in water samples (natural water, groundwater, and wastewater), yielding recoveries of 93% to 110% (95% confidence level).

  8. Magnetic solid-phase extraction of triazine herbicides from rice using metal-organic framework MIL-101(Cr) functionalized magnetic particles.

    Science.gov (United States)

    Liang, Li; Wang, Xinghua; Sun, Ying; Ma, Pinyi; Li, Xinpei; Piao, Huilan; Jiang, Yanxiao; Song, Daqian

    2018-03-01

    The metal-organic framework (MOF) functionalized magnetic graphene oxide/mesoporous silica composites (Fe 3 O 4 @SiO 2 -GO/MIL-101(Cr)) were synthesized and utilized as magnetic solid-phase extraction (MSPE) adsorbent for the extraction of seven triazine herbicides (terbuthylazine, secbumeton, terbumeton, atraton, atrazine, prometon and trietazine) in rice samples. Several experimental parameters, including type and volume of extraction solvent, amount of MIL-101(Cr), extraction time, volume of desorption solvent and desorption time were investigated and optimized. The limits of detection (LODs) of seven triazine herbicides obtained by using the proposed MSPE method combined with high performance liquid chromatography (HPLC) were in the range of 0.010-0.080µgkg -1 . The recoveries of the triazine herbicides in spiked rice samples ranged from of 83.9-103.5% with the relative standard deviations lower than 8.7%. The intra and inter-day (n = 6) precisions for all triazine herbicides at the spiked level of 100.0µgkg -1 were 1.4-5.9% and 2.6-7.8%, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Comparison of dialysis and solid-phase extraction for isolation and concentration of dissolved organic matter prior to Fourier transform ion cyclotron resonance mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tfaily, Malak M.; Cooper, William T. [Florida State University, Department of Chemistry and Biochemistry, Tallahassee, FL (United States); Hodgkins, Suzanne; Chanton, Jeffrey P. [Florida State University, Department of Earth, Ocean and Atmospheric Science, Tallahassee, FL (United States); Podgorski, David C. [Florida State University, Department of Chemistry and Biochemistry, Tallahassee, FL (United States); Florida State University, National High Magnetic Field Laboratory, Tallahassee, FL (United States)

    2012-08-15

    We compare two methods, solid-phase extraction (SPE) and dialysis, commonly used for extraction and concentration of dissolved organic matter (DOM) prior to molecular characterization by electrospray ionization (ESI) and ultrahigh-resolution Fourier transform ion cyclotron resonance mass spectrometry. Spectra of DOM samples from Minnesota and Sweden peatlands that were extracted with styrene divinyl benzene polymer SPE sorbents included ions with formulas that had higher oxygen to carbon (O/C) ratios than spectra of DOM from the same samples after de-salting by dialysis. The SPE method was not very effective in extracting several major classes of DOM compounds that had high ESI efficiencies, including carboxylic acids and organo-sulfur compounds, and that out-competed other less-functionalized compounds (e.g., carbohydrates) for charge in the ESI source. The large abundance of carboxylic acids in the dialysisextracted DOM, likely the result of in situ microbial production, makes it difficult to see other (mainly hydrophilic) compounds with high O/C ratios. Our results indicate that, while dialysis is generally preferable for the isolation of DOM, for samples with high microbial inputs, the use of both isolation methods is recommended for a more accurate molecular representation. (orig.)

  10. Extraction of scandium by organic substance melts

    International Nuclear Information System (INIS)

    Gladyshev, V.P.; Lobanov, F.I.; Zebreva, A.I.; Andreeva, N.N.; Manuilova, O.A.; Il'yukevich, Yu.A.

    1984-01-01

    Regularities of scandium extraction by the melts of octadecanicoic acid, n-carbonic acids of C 17 -C 20 commerical fraction and mixtures of tributylphosphate (TBP) with paraffin at (70+-1) deg C have been studied. The optimum conditions for scandium extraction in the melt of organic substances are determined. A scheme of the extraction by the melts of higher carbonic acids at ninitial metal concentrations of 10 -5 to 10 -3 mol/l has been suggested. The scandium compound has been isolated in solid form, its composition having been determined. The main advantages of extraction by melts are as follows: a possibility to attain high distribution coefficients, distinct separation of phases after extraction, the absence of emulsions, elimination of employing inflammable and toxic solvents, a possibility of rapid X-ray fluorescence determinatinon of scandium directly in solid extract

  11. Utilizing thin-film solid-phase extraction to assess the effect of organic carbon amendments on the bioavailability of DDT and dieldrin to earthworms

    International Nuclear Information System (INIS)

    Andrade, Natasha A.; Centofanti, Tiziana; McConnell, Laura L.; Hapeman, Cathleen J.; Torrents, Alba; Nguyen, Anh; Beyer, W. Nelson; Chaney, Rufus L.; Novak, Jeffrey M.; Anderson, Marya O.; Cantrell, Keri B.

    2014-01-01

    Improved approaches are needed to assess bioavailability of hydrophobic organic compounds in contaminated soils. Performance of thin-film solid-phase extraction (TF-SPE) using vials coated with ethylene vinyl acetate was compared to earthworm bioassay (Lumbricus terrestris). A DDT and dieldrin contaminated soil was amended with four organic carbon materials to assess the change in bioavailability. Addition of organic carbon significantly lowered bioavailability for all compounds except for 4,4′-DDT. Equilibrium concentrations of compounds in the polymer were correlated with uptake by earthworms after 48d exposure (R 2 = 0.97; p 40yr of aging. Results show that TF-SPE can be useful in examining potential risks associated with contaminated soils and to test effectiveness of remediation efforts. -- Highlights: • Bioavailability of pesticides in soil were assessed using TF-SPE and earthworms. • Soil from a historical orchard was used to examine aged residues of dieldrin and DDT. • TF-SPE results were strongly correlated with earthworm bioaccumulation factors. • Ethylene vinyl acetate polymer has sorptive capacity similar to earthworm lipid. • TF-SPE useful to estimate bioavailability of hydrophobic organic pesticides in soil. -- Capsule A thin-film polymer sampler proved to be efficient in estimating the differences in bioavailability to earthworms in a soil treated with organic amendments

  12. Ion-exchange solid-phase extraction combined with liquid chromatography-tandem mass spectrometry for the determination of veterinary drugs in organic fertilizers.

    Science.gov (United States)

    Zhao, Zhiyong; Zhang, Yanmei; Xuan, Yanfang; Song, Wei; Si, Wenshuai; Zhao, Zhihui; Rao, Qinxiong

    2016-06-01

    The analysis of veterinary drugs in organic fertilizers is crucial for an assessment of potential risks to soil microbial communities and human health. We develop a robust and sensitive method to quantitatively determine 19 veterinary drugs (amantadine, sulfonamides and fluoroquinolones) in organic fertilizers. The method involved a simple solid-liquid extraction step using the combination of acetonitrile and McIlvaine buffer as extraction solvent, followed by cleanup with a solid-phase extraction cartridge containing polymeric mixed-mode anion-exchange sorbents. Ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was used to separate and detect target analytes. We particularly focused on the optimization of sample clean-up step: different diluents and dilution factors were tested. The developed method was validated in terms of linearity, recovery, precision, sensitivity and specificity. The recoveries of all the drugs ranged from 70.9% to 112.7% at three concentration levels, with the intra-day and inter-day relative standard deviation lower than 15.7%. The limits of quantification were between 1.0 and 10.0μg/kg for all the drugs. Matrix effect was minimized by matrix-matched calibration curves. The analytical method was successfully applied for the survey of veterinary drugs contamination in 20 compost samples. The results indicated that fluoroquinolones had higher incidence rate and mean concentration levels ranging from 31.9 to 308.7μg/kg compared with other drugs. We expect the method will provide the basis for risk assessment of veterinary drugs in organic fertilizers. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Analysis of chemical warfare agents in organic liquid samples with magnetic dispersive solid phase extraction and gas chromatography mass spectrometry for verification of the chemical weapons convention.

    Science.gov (United States)

    Singh, Varoon; Purohit, Ajay Kumar; Chinthakindi, Sridhar; Goud, Raghavender D; Tak, Vijay; Pardasani, Deepak; Shrivastava, Anchal Roy; Dubey, Devendra Kumar

    2016-05-27

    A simple, sensitive and low temperature sample preparation method is developed for detection and identification of Chemical Warfare Agents (CWAs) and scheduled esters in organic liquid using magnetic dispersive solid phase extraction (MDSPE) followed by gas chromatography-mass spectrometry analysis. The method utilizes Iron oxide@Poly(methacrylic acid-co-ethylene glycol dimethacrylate) resin (Fe2O3@Poly(MAA-co-EGDMA)) as sorbent. Variants of these sorbents were prepared by precipitation polymerization of methacrylic acid-co-ethylene glycol dimethacrylate (MAA-co-EGDMA) onto Fe2O3 nanoparticles. Fe2O3@poly(MAA-co-EGDMA) with 20% MAA showed highest recovery of analytes. Extractions were performed with magnetic microspheres by MDSPE. Parameters affecting the extraction efficiency were studied and optimized. Under the optimized conditions, method showed linearity in the range of 0.1-3.0μgmL(-1) (r(2)=0.9966-0.9987). The repeatability and reproducibility (relative standard deviations (RSDs) %) were in the range of 4.5-7.6% and 3.4-6.2% respectively for organophosphorous esters in dodecane. Limits of detection (S/N=3/1) and limit of quantification (S/N=10/1) were found to be in the range of 0.05-0.1μgmL(-1) and 0.1-0.12μgmL(-1) respectively in SIM mode for selected analytes. The method was successfully validated and applied to the extraction and identification of targeted analytes from three different organic liquids i.e. n-hexane, dodecane and silicon oil. Recoveries ranged from 58.7 to 97.3% and 53.8 to 95.5% at 3μgmL(-1) and 1μgmL(-1) spiking concentrations. Detection of diethyl methylphosphonate (DEMP) and O-Ethyl S-2-diisopropylaminoethyl methylphosphonothiolate (VX) in samples provided by the Organization for Prohibition of Chemical Weapons Proficiency Test (OPCW-PT) proved the utility of the developed method for the off-site analysis of CWC relevant chemicals. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Development and Application of Solid Phase Extraction Method for ...

    African Journals Online (AJOL)

    NICO

    for the addition of organic modifier, sample load volume, conditioning solvent, washing solvent and ... Solid phase extraction, polycyclic aromatic hydrocarbons, water samples, ... such as polymeric, activated carbon or silica modified with.

  15. Magnetic solid-phase extraction of heterocyclic pesticides in environmental water samples using metal-organic frameworks coupled to high performance liquid chromatography determination.

    Science.gov (United States)

    Ma, Jiping; Wu, Gege; Li, Shuang; Tan, Weiqiang; Wang, Xiaoyan; Li, Jinhua; Chen, Lingxin

    2018-06-08

    A simple method of magnetic solid-phase extraction (MSPE) coupled to high performance liquid chromatography (HPLC) was developed for the simultaneous extraction and determination of four kinds of heterocyclic pesticides (carbendazim, triadimefon, chlorfenapyr and fenpyroximate) in environmental water samples. Magnetic metal-organic frameworks (MOFs) of type MOF-5 were prepared and used as adsorbents of MSPE. Several main parameters influencing MSPE efficiency were investigated, including amount of magnetic MOF-5, sample solution pH, extraction time, salt concentration, type and volume of desorption solvents and desorption time. Under optimal conditions, the MSPE-HPLC method presented fast simple separation and analysis, and excellent linearity in the range of 0.3-500.0 μg/L for carbendazim and triadimefon, and 0.1-500.0 μg/L for chlorfenapyr and fenpyroximate, with correlation coefficients (r) higher than 0.9992. High sensitivity with limits of detection and quantification ranging from 0.04-0.11 μg/L and 0.13-0.35 μg/L, respectively, were achieved, as well as good precision with relative standard deviations of 2.98-7.11% (intra-day) and 3.31-7.12% (inter-day). Furthermore, the method was successfully applied to reservoir and Yellow River water samples, and satisfactory recoveries at three spiked concentration levels were between 80.20% and 108.33%.The magnetic MOF-5 composites based MSPE followed by HPLC proved promising for convenient and efficient determination of heterocyclic pesticides in environmental water samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  16. Disinfection by-product formation during chlor(am)ination of algal organic matters (AOM) extracted from Microcystis aeruginosa: effect of growth phases, AOM and bromide concentration.

    Science.gov (United States)

    Chen, Juxiang; Gao, Naiyun; Li, Lei; Zhu, Mingqiu; Yang, Jing; Lu, Xian; Zhang, Yansen

    2017-03-01

    Algae organic matter (AOM), including extracellular organic matter (EOM) and intracellular organic matter (IOM), has caused a series of problems to the water quality, among which formation of disinfection by-products (DBPs) during subsequent chlor(am)ination process was especially serious and concerned. This study characterized physicochemical properties of the EOM and IOM solution extracted from different growth phases of Microcystis aeruginosa and investigated the corresponding formation potential of DBPs during chlor(am)ination process. Besides, the effects of initial concentration of xEOM, IOM, and Br - on the yields of disinfection by-product formation potential were studied. The results indicated that the specific UV absorbance (SUVA 254 ) values of IOM and EOM (1.09 and 2.66 L/mg m) were considerably lower than that of natural organic matter (NOM) (4.79 L/mg m). Fluorescence dates showed the soluble microbial by-product was dominant in both EOM and IOM, and the tryptophan was the main component of AOM. From the excitation-emission matrix figure of EOM and IOM, we found that the content of the high molecular weight protein substance in IOM was higher than EOM. During chlorination of EOM and IOM, the yields of four kinds of DBPs followed the order trichloroethene (TCM) > 1,1-DCP > dichloride acetonitrile (DCAN) > trichloronitromethane (TCNM), while the order was TCM > DCAN > TCNM > 1,1-DCP during chloramination process. The bromine substitution factor (BSF) value increased with the increasing of the concentration of Br - . When the concentration of Br - was 500 μg/L, the BSF values of chlorination EOM and IOM were 51.1 and 68.4%, respectively. As the concentration of Br - increased, the formation of Cl-DBPs was inhibited and the formation of Br-DBPs was promoted. Graphical abstract ᅟ.

  17. Magnetic solid phase extraction of typical polycyclic aromatic hydrocarbons from environmental water samples with metal organic framework MIL-101 (Cr) modified zero valent iron nano-particles.

    Science.gov (United States)

    Zhou, Qingxiang; Lei, Man; Wu, Yalin; Yuan, Yongyong

    2017-03-03

    Metal-organic framework material has been paid more attention because of its good physical and chemical properties. Nanoscale zero valent iron is also in the center of concern recently. Combination of their merits will give impressive results. Present study firstly synthesized a new magnetic nanomaterial nano-scale zero valent iron-functionalized metal-organic framworks MIL-101 (Fe@MIL-101) by co-precipitation method. The morphology and structure of the as-prepared Fe@MIL-101 were characterized by transmission electron microscopy and X-ray diffraction, etc. The experimental results showed that Fe@MIL-101 earned good adsorption ability to polycyclic aromatic hydrocarbons. The limits of detection of developed magnetic solid phase extraction were all below 0.064μgL -1 and precision can be expressed as relative standard deviation (RSD, %) and which was better than 4.4% (n=6). The real water analysis indicated that the spiked recoveries were satisfied, and Fe@MIL-101 earned excellent reusability. All these demonstrated that Fe@MIL-101 exhibited excellent adsorption capability to polycyclic aromatic hydrocarbons and would be a good adsorbent for development of new monitoring methods for environmental pollutants. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Extraction of lanthanides and actinides (III) by DI-2 ethyl dithiophosphoric acid and DI-2 ethyl hexyl monothiophosphoric acid. Structure of the complexes in the organic phase

    International Nuclear Information System (INIS)

    Pattee, D.; Musikas, C.; Faure, A.; Chachaty, C.

    1986-09-01

    To operate a trivalent actinide-lanthanide (III) group chemical separation from low pH nitric solutions we studied the extractive properties of the di-2 ethyl hexyl dithiophosphoric acid (HDEHDTP); this bidentate ligand which possesses a sulfur donor atom is a good extractant of soft acids. We so expect a better selectivity for the actinides (III) extraction. We also have investigated extractive properties of di-2 ethyl hexyl monothiophosphoric acid (HDEHTP) for trivalent actinides and lanthanides; HDEHDTP is a bidentate ligand with one oxygen donor atom and so is a better extractant for hard acids like actinides and lanthanides (III); but its selectivity is weak. The addition of TBP (tri-n butyl phosphate) to HDEHDTP deals to strong synergistic organic complexes with a great selectivity for Am(III). We explicited this phenomenon. When the metal is macroconcentrated the organic complexes aggregate and form inverted micelles

  19. Organization of extracting molecules of the diamide type: link with the extracting properties?

    International Nuclear Information System (INIS)

    Meridiano, Y.

    2009-02-01

    The aim of these studies is to establish a link between the different organizations of diamide extractants (used in the DIAMEX process) and their extracting properties. The effects of the key parameters leading the liquid-liquid extraction (concentration of extractant, nature of solute, activity of the aqueous phase, nature of the diluent and temperature) are studied: 1) at the supramolecular scale, with the characterization of the extractant organizations by vapor-pressure osmometry (VPO) and small angle neutron and X-ray scattering (SANS/SAXS) experiments; 2) at the molecular scale, with the quantification of the extracted solutes (water, nitric acid, metal nitrate) and the determination of extracted complexes stoichiometries by electro-spray mass spectrometry (ESI-MS) experiments. The DMDOHEMA molecule acts as a classical surfactant and forms aggregates of the reverse micelle type. Taking into account the established supramolecular diagrams, a quantitative link between the extractants structures and their extracting properties has been brought to light. To model the europium nitrate extraction, two approaches have been developed: - an approach based on mass action laws. Extractions equilibria have been proposed taking into account the supramolecular speciation; - an innovative approach considering the extracted ions as adsorbed on a specific surface of the extractant molecule which depends on the extractant organization state. The ion extraction can be considered as a sum of isotherms corresponding to the different states of organization. This approach allows to compare the extraction efficiency of an extracting molecule as a function of its organization state. (author)

  20. Extraction of metals such as Pu, U and Sr with an organic solvent or a solid phase containing a cis-syn-cis isomer of the crown ether DCH18C6

    International Nuclear Information System (INIS)

    Guy, A.; Foos, J.; Lemaire, M.; Guyon, V.; Chomel, R.; Doutreluigne, P.; Le Roy, H.

    1991-01-01

    The cis-syn-cis isomer of the crown ether DCH18C6 is used in solution in an organic diluent such as benzonitrile or dichlorethane, or on a solid phase such as silica. The use of this isomer increases the extraction ratio of plutonium and strontium of solution from spent fuel reprocessing or from aqueous effluents containing Sr or Pu [fr

  1. AUTOMATED ANALYSIS OF AQUEOUS SAMPLES CONTAINING PESTICIDES, ACIDIC/BASIC/NEUTRAL SEMIVOLATILES AND VOLATILE ORGANIC COMPOUNDS BY SOLID PHASE EXTRACTION COUPLED IN-LINE TO LARGE VOLUME INJECTION GC/MS

    Science.gov (United States)

    Data is presented on the development of a new automated system combining solid phase extraction (SPE) with GC/MS spectrometry for the single-run analysis of water samples containing a broad range of organic compounds. The system uses commercially available automated in-line 10-m...

  2. Preparation of ionic liquid modified magnetic metal-organic frameworks composites for the solid-phase extraction of α-chymotrypsin.

    Science.gov (United States)

    Wei, Xiaoxiao; Wang, Yuzhi; Chen, Jing; Xu, Panli; Zhou, Yigang

    2018-05-15

    A novel magnetic solid-phase extraction (MSPE) method based on 1-hexyl-3-methyl imidazolium chloride ionic liquid (IL) modified magnetic Fe 3 O 4 nanoparticles, hydroxylated multiwall carbon nanotubes (MWCNTs-OH) and zeolitic imidazolate frameworks (ZIFs) nanocomposites (Fe 3 O 4 -MWCNTs-OH@ZIF-67@IL) were proposed and applied to extract α-chymotrypsin. The magnetic materials were synthesized successfully and characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), thermal gravimetric analysis (TGA), fourier transform infrared spectrometry (FT-IR), vibrating sample magnetometer (VSM) and zeta potentials. Subsequently, the UV-vis spectrophotometer at about 280 nm was utilized to quantitatively analyze the α-chymotrypsin concentration in the supernatant. Furthermore, single factor experiments revealed that the extraction capacity was influenced by initial α-chymotrypsin concentration, ionic strength, extraction time, extraction temperature and pH value. The extraction capacity could reach up to about 635 mg g -1 under the optimized conditions, absolutely higher than that of extraction for Ovalbumin (OVA), Bovine serum albumin (BSA) and Bovine hemoglobin (BHb). In addition, the regeneration studies showed Fe 3 O 4 -MWCNTs-OH@ZIF-67@IL particles could be reused several times and kept a high extraction capacity. Besides, the study of enzymatic activity also indicated that the activity of the extracted α-chymotrypsin was well maintained 93% of initial activity. What's more, the proposed method was successfully applied to extract α-chymotrypsin in porcine pancreas crude extract with satisfactory results. All of above conclusions highlight the great potential of the proposed Fe 3 O 4 -MWCNTs-OH@ZIF-67@IL-MSPE method in the analysis of biomolecules. Copyright © 2018 Elsevier B.V. All rights reserved.

  3. Solid phase micro-extraction in environmental atmosphere

    International Nuclear Information System (INIS)

    Tao Ping; Wei Lifan; Tan Yun

    2002-01-01

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

  4. A hydrazone covalent organic polymer based micro-solid phase extraction for online analysis of trace Sudan dyes in food samples.

    Science.gov (United States)

    Zhang, Chengjiang; Li, Gongke; Zhang, Zhuomin

    2015-11-06

    Covalent organic polymers (COPs) connected by covalent bonds are a new class of porous network materials with large surface area and potential superiority in sample pretreatment. In this study, a new hydrazone linked covalent organic polymer (HL-COP) adsorbent was well-designed and synthesized based on a simple Schiff-base reaction. The condensation of 1,4-phthalaldehyde and 1,3,5-benzenetricarbohydrazide as organic building blocks led to the synthesis of HL-COP with uniform particle size and good adsorption performance. This HL-COP adsorbent with high hydrophobic property and rich stacking π electrons contained abundant phenyl rings and imine (CN) groups throughout the entire molecular framework. The adsorption mechanism was explored and discussed based on π-π affinity, hydrophobic effect, hydrogen bonding and electron-donor-acceptor (EDA) interaction, which contributed to its strong recognition affinity to target compounds. Enrichment factors were 305-757 for six Sudan dyes by HL-COP micro-solid phase extraction (μ-SPE), indicating its remarkable preconcentration ability. Furthermore, the adsorption amounts by HL-COP μ-SPE were 1.0-11.0 folds as those by three commonly used commercial adsorbents. Then, HL-COP was applied as adsorbent of online μ-SPE coupled with high performance liquid chromatography (HPLC) for enrichment and analysis of trace Sudan dyes in food samples with detection limit of 0.03-0.15μg/L. The method was successfully applied for online analysis of chilli powder and sausage samples. Sudan II and Sudan III in one positive chilli powder sample were actually found and determined with concentrations of 8.3 and 6.8μg/kg, respectively. The recoveries of chilli powder and sausage samples were in range of 75.8-108.2% and 73.8-112.6% with relative standard deviations of 1.2-8.5% and 1.9-9.4% (n=5), respectively. The proposed method was accurate, reliable and convenient for the online simultaneous analysis of trace Sudan dyes in food samples

  5. Basicity determination for neutral phosphorus organic extragents by NMR 31P-method in two-phase systems, and quantitative interrelations of acido-basic extractive properties

    International Nuclear Information System (INIS)

    Laskorin, B.N.; Yakshin, V.V.; Meshcheryakov, N.M.; Yagodin, V.G.

    1988-01-01

    Consideration is given to the method for determination of basicity of neutral organophosphorus compounds of XGZP=0 type (X, G, Z=C 4 H 9 , C 8 H 17 , C 6 H 5 ). The method is based on change of chemical shift of phosphorus-31 nuclei in two-phase extraction system depending on acidity function H O , H A , H PO . It is shown that the method can be used for evaluation and forecasting of phosphine oxide ability in the processes of UO 2 SO 4 solvent extraction from aqueous solutions of sulfuric acid

  6. Development of liquid phase microextraction method based on solidification of floated organic drop for extraction and preconcentration of organochlorine pesticides in water samples

    International Nuclear Information System (INIS)

    Farahani, Hadi; Yamini, Yadollah; Shariati, Shahab; Khalili-Zanjani, Mohammad Reza; Mansour-Baghahi, Saeed

    2008-01-01

    A simple and efficient liquid-phase microextraction (LPME) in conjunction with gas chromatography-electron capture detector (GC-ECD) has been developed for extraction and determination of 11 organochlorine pesticides (OCPs) from water samples. In this technique a microdrop of 1-dodecanol containing pentachloronitrobenzene (internal standard) is delivered to the surface of an aqueous sample while being agitated by a stirring bar in the bulk of solution. Following completion of extraction, the sample vial was cooled by putting it into an ice bath for 5 min. Finally 2 μL of the drop was injected into the GC for analysis. Factors relevant to the extraction efficiency were studied and optimized. Under the optimized extraction conditions (extraction solvent: 1-dodecanol; extraction temperature: 65 deg. C; sodium chloride concentration: 0.25 M; microdrop and sample volumes: 8 μL and 20 mL respectively; the stirring rate: 750 rpm and the extraction time: 30 min), figures of merit of the proposed method were evaluated. The detection limits of the method were in the range of 7-19 ng L -1 and the RSD% for analysis of 2 μg L -1 of OCPs was below 7.2% (n = 5). A good linearity (r 2 ≥ 0.993) and a relatively broad dynamic linear range (25-2000 ng L -1 ) were obtained. After 30 min of extraction, preconcentration factors were in the range of 708-1337 for different organochlorine pesticides and the relative errors ranged from -10.1 to 10.9%. Finally the proposed method was successfully utilized for preconcentration and determination of OCPs in different real samples

  7. Development of liquid phase microextraction method based on solidification of floated organic drop for extraction and preconcentration of organochlorine pesticides in water samples

    Energy Technology Data Exchange (ETDEWEB)

    Farahani, Hadi [Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Yamini, Yadollah [Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of)], E-mail: yyamini@modares.ac.ir; Shariati, Shahab [Department of Chemistry, Faculty of Sciences, Islamic Azad University, Rasht Branch, Rasht (Iran, Islamic Republic of); Khalili-Zanjani, Mohammad Reza [Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Mansour-Baghahi, Saeed [Department of Water Quality Control and Laboratories, Tehran Water and Sewerage Company, Tehran (Iran, Islamic Republic of)

    2008-09-26

    A simple and efficient liquid-phase microextraction (LPME) in conjunction with gas chromatography-electron capture detector (GC-ECD) has been developed for extraction and determination of 11 organochlorine pesticides (OCPs) from water samples. In this technique a microdrop of 1-dodecanol containing pentachloronitrobenzene (internal standard) is delivered to the surface of an aqueous sample while being agitated by a stirring bar in the bulk of solution. Following completion of extraction, the sample vial was cooled by putting it into an ice bath for 5 min. Finally 2 {mu}L of the drop was injected into the GC for analysis. Factors relevant to the extraction efficiency were studied and optimized. Under the optimized extraction conditions (extraction solvent: 1-dodecanol; extraction temperature: 65 deg. C; sodium chloride concentration: 0.25 M; microdrop and sample volumes: 8 {mu}L and 20 mL respectively; the stirring rate: 750 rpm and the extraction time: 30 min), figures of merit of the proposed method were evaluated. The detection limits of the method were in the range of 7-19 ng L{sup -1} and the RSD% for analysis of 2 {mu}g L{sup -1} of OCPs was below 7.2% (n = 5). A good linearity (r{sup 2} {>=} 0.993) and a relatively broad dynamic linear range (25-2000 ng L{sup -1}) were obtained. After 30 min of extraction, preconcentration factors were in the range of 708-1337 for different organochlorine pesticides and the relative errors ranged from -10.1 to 10.9%. Finally the proposed method was successfully utilized for preconcentration and determination of OCPs in different real samples.

  8. 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

  9. Soil and groundwater remediation using dual-phase extraction technology

    International Nuclear Information System (INIS)

    Miller, A.W.; Gan, D.R.

    1995-01-01

    A gasoline underground storage tank (UST) was formerly used to fuel vehicles for a hospital in Madison, Wisconsin. Elevated concentrations of gasoline range organics (GRO) were observed in soils and groundwater at the site during the tank removal and a subsequent site investigation. Based on the extent of soil and groundwater contamination, a dual-phase extraction technology was selected as the most cost effective alternative to remediate the site. The dual-phase extraction system includes one extraction well functioning both as a soil vapor extraction (SVE) and groundwater recovery well. After six months of operation, samples collected from the groundwater monitoring wells indicated that the groundwater has been cleaned up to levels below the Wisconsin preventative action limits. The dual-phase extraction system effectively remediated the site in a short period of time, saving both operation and maintenance costs and overall project cost

  10. 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.

  11. Solid Phase Extraction and Spectrophotometric Determination of ...

    African Journals Online (AJOL)

    NJD

    2005-04-15

    Apr 15, 2005 ... to the economy and has significant industrial applications. The development of a ... Waters Solid Phase Extraction (SPE) device (the device can carry out twenty ... HPLC grade dimethyl formamide (DMF) (Fisher. Corporation ...

  12. High-performance liquid chromatography - Ultraviolet method for the determination of total specific migration of nine ultraviolet absorbers in food simulants based on 1,1,3,3-Tetramethylguanidine and organic phase anion exchange solid phase extraction to remove glyceride.

    Science.gov (United States)

    Wang, Jianling; Xiao, Xiaofeng; Chen, Tong; Liu, Tingfei; Tao, Huaming; He, Jun

    2016-06-17

    The glyceride in oil food simulant usually causes serious interferences to target analytes and leads to failure of the normal function of the RP-HPLC column. In this work, a convenient HPLC-UV method for the determination of the total specific migration of nine ultraviolet (UV) absorbers in food simulants was developed based on 1,1,3,3-tetramethylguanidine (TMG) and organic phase anion exchange (OPAE) SPE to efficiently remove glyceride in olive oil simulant. In contrast to the normal ion exchange carried out in an aqueous solution or aqueous phase environment, the OPAE SPE was performed in the organic phase environments, and the time-consuming and challenging extraction of the nine UV absorbers from vegetable oil with aqueous solution could be readily omitted. The method was proved to have good linearity (r≥0.99992), precision (intra-day RSD≤3.3%), and accuracy(91.0%≤recoveries≤107%); furthermore, the lower limit of quantifications (0.05-0.2mg/kg) in five types of food simulants(10% ethanol, 3% acetic acid, 20% ethanol, 50% ethanol and olive oil) was observed. The method was found to be well suited for quantitative determination of the total specific migration of the nine UV absorbers both in aqueous and vegetable oil simulant according to Commission Regulation (EU) No. 10/2011. Migration levels of the nine UV absorbers were determined in 31 plastic samples, and UV-24, UV-531, HHBP and UV-326 were frequently detected, especially in olive oil simulant for UV-326 in PE samples. In addition, the OPAE SPE procedure was also been applied to efficiently enrich or purify seven antioxidants in olive oil simulant. Results indicate that this procedure will have more extensive applications in the enriching or purification of the extremely weak acidic compounds with phenol hydroxyl group that are relatively stable in TMG n-hexane solution and that can be barely extracted from vegetable oil. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Rapid determination of trace nitrophenolic organics in water by combining solid-phase extraction with surface-assisted laser desorption/ionization time-of-flight mass spectrometry.

    Science.gov (United States)

    Chen, Y C; Shiea, J; Sunner, J

    2000-01-01

    A rapid technique for the screening of trace compounds in water by combining solid-phase extraction (SPE) with activated carbon surface-assisted laser desorption/ionization (SALDI) time-of-flight mass spectrometry is demonstrated. Activated carbon is used both as the sorbent in SPE and as the solid in the SALDI matrix system. This eliminates the need for an SPE elution process. After the analytes have been adsorbed on the surfaces of the activated carbon during SPE extraction, the activated carbon is directly mixed with the SALDI liquid and mass spectrometric analysis is performed. Trace phenolic compounds in water were used to demonstrate the effectiveness of the method. The detection limit for these compounds is in the ppb to ppt range. Copyright 2000 John Wiley & Sons, Ltd.

  14. Effect of organic bases on extraction of gadolinium carboxylates

    International Nuclear Information System (INIS)

    Sukhan, V.V.; Frankovskij, V.A.

    1982-01-01

    The effect of pyridine, 2-aminopyridine, benzylamine, antipyrine and o-phenanthroline on the extraction of capronates and bromocapronates of gadolinium with chloroform is studied. Out of the studied organic bases benzylamine produces the highest synergetic effect. In the absence of organic bases gadolinium carboxylates, solvated by three molecules of carbonic acids, are extracted into organic phase. A possihility of extractional separation of gadolinium from comparable amounts of iron with the mixture of 1 M solutions of caproic or bromocaproic acids with 1 M benzylamine from 0.1 M solution of tartaric acids is shown [ru

  15. Solid-phase extraction with the metal-organic framework MIL-101(Cr) combined with direct analysis in real time mass spectrometry for the fast analysis of triazine herbicides.

    Science.gov (United States)

    Li, Xianjiang; Xing, Jiawei; Chang, Cuilan; Wang, Xin; Bai, Yu; Yan, Xiuping; Liu, Huwei

    2014-06-01

    MIL-101(Cr) is an excellent metal-organic framework with high surface area and nanoscale cavities, making it promising in solid-phase extraction. Herein, we used MIL-101(Cr) as a solid-phase extraction packing material combined with fast detection of direct analysis in real time mass spectrometry (DART-MS) for the analysis of triazine herbicides. After systematic optimization of the operation parameters, including the gas temperature of DART, the moving speed of the 1D platform, solvent for desorption, amount of MIL-101(Cr) extraction time, eluent volume and salt concentration, this method can realize the simultaneous detection of five kinds of triazine herbicides. The limits of detection were 0.1∼0.2 ng/mL and the linear ranges covered more than two orders of magnitude with the quantitation limits of 0.5∼1 ng/mL. Moreover, the developed method has been applied for the analysis of lake water samples and the recoveries for spiked analytes were in the range of 85∼110%. These results showed that solid-phase extraction with metal-organic frameworks is an efficient sample preparation approach for DART-MS analysis and could find more applications in environmental analysis. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Multiplexed Colorimetric Solid-Phase Extraction

    Science.gov (United States)

    Gazda, Daniel B.; Fritz, James S.; Porter, Marc D.

    2009-01-01

    Multiplexed colorimetric solid-phase extraction (MC-SPE) is an extension of colorimetric solid-phase extraction (C-SPE) an analytical platform that combines colorimetric reagents, solid phase extraction, and diffuse reflectance spectroscopy to quantify trace analytes in water. In CSPE, analytes are extracted and complexed on the surface of an extraction membrane impregnated with a colorimetric reagent. The analytes are then quantified directly on the membrane surface using a handheld diffuse reflectance spectrophotometer. Importantly, the use of solid-phase extraction membranes as the matrix for impregnation of the colorimetric reagents creates a concentration factor that enables the detection of low concentrations of analytes in small sample volumes. In extending C-SPE to a multiplexed format, a filter holder that incorporates discrete analysis channels and a jig that facilitates the concurrent operation of multiple sample syringes have been designed, enabling the simultaneous determination of multiple analytes. Separate, single analyte membranes, placed in a readout cartridge create unique, analyte-specific addresses at the exit of each channel. Following sample exposure, the diffuse reflectance spectrum of each address is collected serially and the Kubelka-Munk function is used to quantify each water quality parameter via calibration curves. In a demonstration, MC-SPE was used to measure the pH of a sample and quantitate Ag(I) and Ni(II).

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  18. Solid phase extraction of Cd(II) and Pb(II) using a magnetic metal-organic framework, and their determination by FAAS

    International Nuclear Information System (INIS)

    Sohrabi, Mahmoud Reza; Matbouie, Zahra; Asgharinezhad, Ali Akbar; Dehghani, Ali

    2013-01-01

    We describe a novel magnetic metal-organic framework (MOF) for the preconcentration of Cd(II) and Pb(II) ions. The MOF was prepared from the Fe 3 O 4 -pyridine conjugate and the copper(II) complex of trimesic acid. The MOF was characterized by IR spectroscopy, elemental analysis, SEM and XRD. A Box-Behnken design through response surface methodology and experimental design was used to identify the optimal parameters for preconcentration. Extraction time, amount of magnetic MOF and pH value were found to be critical factors for uptake, while type, volume, concentration of eluent, and elution time are critical in the elution step. The ions were then determined by FAAS. The limits of detection are 0.2 and 1.1 μg L −1 for Cd(II), and Pb(II) ions, respectively, relative standard deviations are −1 of Cd(II) and Pb(II) ions), and the enrichment capacity of the MOF is at around 190 mg g −1 for both ions which is higher than the conventional Fe 3 O 4 -pyridine material. The magnetic MOF was successfully applied to the rapid extraction of trace quantities of Cd(II) and Pb(II) ions in fish, sediment, and water samples. (author)

  19. Quantum Phase Extraction in Isospectral Electronic Nanostructures

    Energy Technology Data Exchange (ETDEWEB)

    Moon, Christopher

    2010-04-28

    Quantum phase is not a direct observable and is usually determined by interferometric methods. We present a method to map complete electron wave functions, including internal quantum phase information, from measured single-state probability densities. We harness the mathematical discovery of drum-like manifolds bearing different shapes but identical resonances, and construct quantum isospectral nanostructures possessing matching electronic structure but divergent physical structure. Quantum measurement (scanning tunneling microscopy) of these 'quantum drums' [degenerate two-dimensional electron states on the Cu(111) surface confined by individually positioned CO molecules] reveals that isospectrality provides an extra topological degree of freedom enabling robust quantum state transplantation and phase extraction.

  20. Methods of Analysis by the U.S. Geological Survey Organic Geochemistry Research Group - Determination of Glyphosate, Aminomethylphosphonic Acid, and Glufosinate in Water Using Online Solid-Phase Extraction and High-Performance Liquid Chromatography/Mass Spectrometry

    National Research Council Canada - National Science Library

    Lee, E. A; Strahan, A. P; Thurman, E. M

    2002-01-01

    ...). After derivatization, cleanup and concentration were accomplished using automated online solidphase extraction followed by elution with the mobile phase allowing for direct injection into a liquid...

  1. Factors influencing phase-disengagement rates in solvent-extraction systems employing tertiary amine extractants

    International Nuclear Information System (INIS)

    Moyer, B.A.; McDowell, W.J.

    1981-01-01

    The primary purpose of the present investigation was to examine the effects of amine size and structure on phase disengagement. Nine commercial tertiary amines were tested together with four laboratory-quality amines for uranium extraction and both organic-continuous (OC) and aqueous-continuous (AC) phase disengagement under Amex-type conditions. Synthetic acid sulfate solutions with and without added colloidal silica and actual ore leach solutions were used as the aqueous phases. Phase disengagement results were correlated with amine size and branching and solution wetting behavior on a silicate (glass) surface. The results suggest that the performance of some Amex systems may be improved by using branched chain tertiary amine extractants of higher molecular weight than are now normally used

  2. Methods of analysis by the U.S. Geological Survey Organic Geochemistry Research Group : determination of selected herbicides and their degradation products in water using solid-phase extraction and gas chromatography/mass spectrometry

    Science.gov (United States)

    Kish, J.L.; Thurman, E.M.; Scribner, E.A.; Zimmerman, L.R.

    2000-01-01

    A method for the extraction and analysis of eight herbicides and five degradation products using solid-phase extraction from natural water samples followed by gas chromatography/mass spectrometry is presented in this report. This method was developed for dimethenamid; flufenacet; fluometuron and its degradation products, demethylfluometuron (DMFM), 3-(trifluromethyl)phenylurea (TFMPU), 3-(trifluromethyl)-aniline (TFMA); molinate; norflurazon and its degradation product, demethylnorflurazon; pendamethalin; the degradation product of prometryn, deisopropylprometryn; propanil; and trifluralin. The eight herbicides are used primarily in the southern United States where cotton, rice, and soybeans are produced. The exceptions are dimethenamid and flufenacet, which are used on corn in the Midwest. Water samples received by the U.S. Geological Survey's Organic Geochemistry Research Group in Lawrence, Kansas, are filtered to remove suspended particulate matter and then passed through disposable solid-phase extraction columns containing octadecyl-bonded porous silica (C-18) to extract the compounds. The herbicides and their degradation products are removed from the column by ethyl acetate elution. The eluate is evaporated under nitrogen, and components then are separated, identified, and quantified by injecting an aliquot of the concentrated extract into a high-resolution, fused-silica capillary column of a gas chromatograph/mass spectrometer under selected-ion mode. Method detection limits ranged from 0.02 to 0.05 ?g/L for all compounds with the exception of TFMPU, which has a method detection limit of 0.32 ?g/L. The mean absolute recovery is 107 percent. This method for the determination of herbicides and their degradation products is valuable for acquiring information about water quality and compound fate and transport in water.

  3. Simultaneous extraction and determination of albendazole and triclabendazole by a novel syringe to syringe dispersive liquid phase microextraction-solidified floating organic drop combined with high performance liquid chromatography.

    Science.gov (United States)

    Asadi, Mohammad; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad

    2016-08-17

    A syringe to syringe dispersive liquid phase microextraction-solidified floating organic drop was introduced and used for the simultaneous extraction of trace amounts of albendazole and triclabendazole from different matrices. The extracted analytes were determined by high performance liquid chromatography along with fluorescence detection. The analytical parameters affecting the microextraction efficiency including the nature and volume of the extraction solvent, sample volume, sample pH, ionic strength and the cycles of extraction were optimized. The calibration curves were linear in the range of 0.1-30.0 μg L(-1) and 0.2-30.0 μg L(-1) with determination coefficients of 0.9999 and 0.9998 for albendazole and triclabendazole respectively. The detection limits defined as three folds of the signal to noise ratio were found to be 0.02 μg L(-1) for albendazole and 0.06 μg L(-1) for triclabendazole. The inter-day and intra-day precision (RSD%) for both analytes at three concentration levels (0.5, 2.0 and 10.0 μg L(-1)) were in the range of 6.3-10.1% and 5.0-7.5% respectively. The developed method was successfully applied to determine albendazole and triclabendazole in water, cow milk, honey, and urine samples. Copyright © 2016. Published by Elsevier B.V.

  4. 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.

  5. Solid-phase extraction versus matrix solid-phase dispersion: Application to white grapes.

    Science.gov (United States)

    Dopico-García, M S; Valentão, P; Jagodziñska, A; Klepczyñska, J; Guerra, L; Andrade, P B; Seabra, R M

    2007-11-15

    The use of matrix solid-phase dispersion (MSPD) was tested to, separately, extract phenolic compounds and organic acids from white grapes. This method was compared with a more conventional analytical method previously developed that combines solid liquid extraction (SL) to simultaneously extract phenolic compounds and organic acids followed by a solid-phase extraction (SPE) to separate the two types of compounds. Although the results were qualitatively similar for both techniques, the levels of extracted compounds were in general quite lower on using MSPD, especially for organic acids. Therefore, SL-SPE method was preferred to analyse white "Vinho Verde" grapes. Twenty samples of 10 different varieties (Alvarinho, Avesso, Asal-Branco, Batoca, Douradinha, Esganoso de Castelo Paiva, Loureiro, Pedernã, Rabigato and Trajadura) from four different locations in Minho (Portugal) were analysed in order to study the effects of variety and origin on the profile of the above mentioned compounds. Principal component analysis (PCA) was applied separately to establish the main sources of variability present in the data sets for phenolic compounds, organic acids and for the global data. PCA of phenolic compounds accounted for the highest variability (77.9%) with two PCs, enabling characterization of the varieties of samples according to their higher content in flavonol derivatives or epicatechin. Additionally, a strong effect of sample origin was observed. Stepwise linear discriminant analysis (SLDA) was used for differentiation of grapes according to the origin and variety, resulting in a correct classification of 100 and 70%, respectively.

  6. Development of a comprehensive screening method for more than 300 organic chemicals in water samples using a combination of solid-phase extraction and liquid chromatography-time-of-flight-mass spectrometry.

    Science.gov (United States)

    Chau, Hong Thi Cam; Kadokami, Kiwao; Ifuku, Tomomi; Yoshida, Yusuke

    2017-12-01

    A comprehensive screening method for 311 organic compounds with a wide range of physicochemical properties (log Pow -2.2-8.53) in water samples was developed by combining solid-phase extraction with liquid chromatography-high-resolution time-of-flight mass spectrometry. Method optimization using 128 pesticides revealed that tandem extraction with styrene-divinylbenzene polymer and activated carbon solid-phase extraction cartridges at pH 7.0 was optimal. The developed screening method was able to extract 190 model compounds with average recovery of 80.8% and average relative standard deviations (RSD) of 13.5% from spiked reagent water at 0.20 μg L -1 , and 87.1% recovery and 10.8% RSD at 0.05 μg L -1 . Spike-recovery testing (0.20 μg L -1 ) using real sewage treatment plant effluents resulted in an average recovery and average RSD of 190 model compounds of 77.4 and 13.1%, respectively. The method was applied to the influent and effluent of five sewage treatment plants in Kitakyushu, Japan, with 29 out of 311 analytes being observed at least once. The results showed that this method can screen for a large number of chemicals with a wide range of physicochemical properties quickly and at low operational cost, something that is difficult to achieve using conventional analytical methods. This method will find utility in target screening of hazardous chemicals with a high risk in environmental waters, and for confirming the safety of water after environmental incidents.

  7. Two-phase ozonation of chlorinated organics

    International Nuclear Information System (INIS)

    Bhattacharyya, D.; Freshour, A.; West, D.

    1995-01-01

    In the last few years the amount of research being conducted in the field of single-phase ozonation has grown extensively. However, traditional aqueous-phase ozonation systems are limited by a lack of selective oxidation potential, low ozone solubility in water, and slow intermediate decomposition rates. Furthermore, ozone may decompose before it can be utilized for pollutant destruction since ozone can be highly unstable in aqueous solutions. Naturally occurring compounds such as NaHCO 3 also affect ozone reactions by inhibiting the formation of OH-free radicals. To compensate for these factors, excess ozone is typically supplied to a reactor. Since ozone generation requires considerable electric power consumption (16 - 24 kWh/kg of O 3 ), attempts to enhance the ozone utilization rate and stability should lead to more efficient application of this process to hazardous waste treatment. To improve the process, ozonation may be more efficiently carried out in a two-phase system consisting of an inert solvent (saturated with O 3 ) contacted with an aqueous phase containing pollutants. The non-aqueous phase must meet the following criteria: (1) non-toxic, (2) very low vapor pressure, (3) high density (for ease of separation), (4) complete insolubility in water, (5) reusability, (6) selective pollutant extractability, (7) high oxidant solubility, and (8) extended O 3 stability. Previously published studies (1) have indicated that a number of fluorinated hydrocarbon compounds fit these criteria. For this project, FC40 (a product of 3M Co.) was chosen due to its low vapor pressure (3 mm Hg) and high specific gravity (1.9). The primary advantages of the FC40 solvent are that it is non-toxic, reusable, has an ozone solubility 10 times that of water, and that 85 % of the ozone remains in the solvent even after 2 hours. This novel two-phase process has been utilized to study the rapid destruction of organic chlorine compounds and organic mixtures

  8. CONVERSION EXTRACTION DESULFURIZATION (CED) PHASE III

    Energy Technology Data Exchange (ETDEWEB)

    James Boltz

    2005-03-01

    This project was undertaken to refine the Conversion Extraction Desulfurization (CED) technology to efficiently and economically remove sulfur from diesel fuel to levels below 15-ppm. CED is considered a generic term covering all desulfurization processes that involve oxidation and extraction. The CED process first extracts a fraction of the sulfur from the diesel, then selectively oxidizes the remaining sulfur compounds, and finally extracts these oxidized materials. The Department of Energy (DOE) awarded Petro Star Inc. a contract to fund Phase III of the CED process development. Phase III consisted of testing a continuous-flow process, optimization of the process steps, design of a pilot plant, and completion of a market study for licensing the process. Petro Star and the Degussa Corporation in coordination with Koch Modular Process Systems (KMPS) tested six key process steps in a 7.6-centimeter (cm) (3.0-inch) inside diameter (ID) column at gas oil feed rates of 7.8 to 93.3 liters per hour (l/h) (2.1 to 24.6 gallons per hour). The team verified the technical feasibility with respect to hydraulics for each unit operation tested and successfully demonstrated pre-extraction and solvent recovery distillation. Test operations conducted at KMPS demonstrated that the oxidation reaction converted a maximum of 97% of the thiophenes. The CED Process Development Team demonstrated that CED technology is capable of reducing the sulfur content of light atmospheric gas oil from 5,000-ppm to less than 15-ppm within the laboratory scale. In continuous flow trials, the CED process consistently produced fuel with approximately 20-ppm of sulfur. The process economics study calculated an estimated process cost of $5.70 per product barrel. The Kline Company performed a marketing study to evaluate the possibility of licensing the CED technology. Kline concluded that only 13 refineries harbored opportunity for the CED process. The Kline study and the research team's discussions

  9. Speciation of As(III) and As(V) in water samples by graphite furnace atomic absorption spectrometry after solid phase extraction combined with dispersive liquid-liquid microextraction based on the solidification of floating organic drop.

    Science.gov (United States)

    Shamsipur, Mojtaba; Fattahi, Nazir; Assadi, Yaghoub; Sadeghi, Marzieh; Sharafi, Kiomars

    2014-12-01

    A solid phase extraction (SPE) coupled with dispersive liquid-liquid microextraction based on the solidification of floating organic drop (DLLME-SFO) method, using diethyldithiphosphate (DDTP) as a proper chelating agent, has been developed as an ultra preconcentration technique for the determination of inorganic arsenic in water samples prior to graphite furnace atomic absorption spectrometry (GFAAS). Variables affecting the performance of both steps were thoroughly investigated. Under optimized conditions, 100mL of As(ΙΙΙ) solution was first concentrated using a solid phase sorbent. The extract was collected in 2.0 mL of acetone and 60.0 µL of 1-undecanol was added into the collecting solvent. The mixture was then injected rapidly into 5.0 mL of pure water for further DLLME-SFO. Total inorganic As(III, V) was extracted similarly after reduction of As(V) to As(III) with potassium iodide and sodium thiosulfate and As(V) concentration was calculated by difference. A mixture of Pd(NO3)2 and Mg(NO3)2 was used as a chemical modifier in GFAAS. The analytical characteristics of the method were determined. The calibration graph was linear in the rage of 10-100 ng L(-1) with detection limit of 2.5 ng L(-1). Repeatability (intra-day) and reproducibility (inter-day) of method based on seven replicate measurements of 80 ng L(-1) of As(ΙΙΙ) were 6.8% and 7.5%, respectively. The method was successfully applied to speciation of As(III), As(V) and determination of the total amount of As in water samples and in a certified reference material (NIST RSM 1643e). Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Metal-organic framework MIL-101(Cr) as a sorbent of porous membrane-protected micro-solid-phase extraction for the analysis of six phthalate esters from drinking water: a combination of experimental and computational study.

    Science.gov (United States)

    Wang, Ting; Wang, Jian; Zhang, Conglu; Yang, Zhao; Dai, Xinpeng; Cheng, Maosheng; Hou, Xiaohong

    2015-08-07

    An attractive metal-organic framework (MOF) MIL-101(Cr) material was synthesized at the nanoscale and applied as a sorbent in the porous membrane-protected micro-solid-phase extraction (μ-SPE) device for the pre-concentration of phthalate esters (PAEs) in drinking water samples for the first time. Parameters influencing the extraction efficiency, such as the selection of sorbent materials, pH adjustment, the effect of salt, magnetic-stirring extraction time, the desorption solvent and the desorption time, were investigated. Under the optimum conditions, the limits of detection from gas chromatography-mass spectrometric analysis for PAEs varied from 0.004 to 0.02 μg L(-1). The linear ranges were from 0.1 to 50 μg L(-1) or from 0.2 to 50 μg L(-1) for the analytes with the relative standard deviations fluctuating from 0.8 to 10.9% (n = 5). The enrichment factors (EFs) for the target PAEs were varied from 143 to 187. MIL-101(Cr) exhibited remarkable advantages compared to activated carbon and MIL-100(Fe). On the other hand, the computational method was first used to predict the adsorption of MIL-101(Cr) towards PAEs. The molecular interactions and the free binding energies between MIL-101(Cr) and PAEs were observed and calculated in terms of the molecular modeling method. MIL-101(Cr) showed high potential in the analysis of PAEs at trace levels in drinking water. The computational result was consistent with the detected enrichment factors. The computational modeling accurately predicted the extraction efficiency of MOF-based material towards the target analytes. Therefore, the combination of experimental and computational study provided a new strategy on the trace contaminant analysis.

  11. Solid-phase extraction of carotenoids.

    Science.gov (United States)

    Shen, Yao; Hu, Yumin; Huang, Ke; Yin, Shi'an; Chen, Bo; Yao, Shouzhuo

    2009-07-24

    In this work, solid-phase extraction (SPE) trapping performance of lutein and beta-carotene, which were used as the model molecules of carotenoids, was investigated. The absorption, elution, and enrichment of carotenoids on SPE cartridges with four different sorbents, i.e. C(30), C(18), diol, and silica, were compared respectively with the help of frontal analysis technique. The high retentions of both lutein and beta-carotene were achieved on the C(18) and C(30) cartridges. The diol and silica cartridges only had good retention for lutein. The optimized SPE method for sample pretreatment for the carotenoids analysis was obtained after the investigation of trapping performance. The method was applied successfully to the analysis of biological sample, i.e. serum and human breast milk. The recovery, accuracy, and precision of SPE method comparing with those of traditional liquid-liquid extraction (LLE) method for the sample pretreatment for the analysis of carotenoids owned a number of advantages such as rapid, no chloroform used, and accurate versus LLE.

  12. Methods of Analysis by the U.S. Geological Survey Organic Geochemistry Research Group--Determination of Triazine and Phenylurea Herbicides and Their Degradation Products in Water Using Solid-Phase Extraction and Liquid Chromatography/Mass Spectrometry

    National Research Council Canada - National Science Library

    Lee, E. A; Strahan, A. P; Thurman, E. M

    2002-01-01

    An analytical method for the determination of 7 triazine and phenylurea herbicides and 12 of their degradation products in natural water samples using solid-phase extraction and liquid chromatography...

  13. Some aspects of synergistic extraction of actinides and lanthanides from mixed aqueous-organic media

    International Nuclear Information System (INIS)

    Shukla, J.P.; Subramanian, M.S.

    1981-01-01

    Various aspects of the synergistic extraction and separation of actinides and lanthanides from mixed aqueous-organic solutions (polar media) have been reviewed. Notable recent developments as well as its current status in solvent extraction systems where the aqueous acidic phase contains an organic solvent which is completely miscible with water, are presented briefly. In general, extraction increases in the presence of an organic component. The less polar the additive, the higher is the tendency to form neutral metal complexes which ultimately brings about an increase in the extraction. In a polar media, synergism has mostly been observed, though antagonism is not uncommon. An attempt has been made to classify the factors that play an important role in polar phase extractions. Also, their influence particularly on the extractability of actinides and lanthanides is discussed. The discussion is limited to the factors affecting the extraction equilibria, effect of dielectric constant of the polar medium, solvation of the extracting agent and to the composition and stability of the metal complex in the organic phase. Hydroxyl (OHsup(-)) bearing organic additives, e.g. alcohols, and solvents not containing the hydroxyl group such as acetone, dimethylsulphoxide, tetrahydrofuran, amides and acetonitrile etc. are the two major classes of organic additives considered in these studies. Generally, synergistic effect in extraction of the ion-association (TBP, TOPO, sulphoxides etc.) or anion exchange (amines etc.) type is relatively more pronounced compared to other extractions. A tabular summary concerning extraction of actinides and lanthanides from polar media is appended for ready reference. (author)

  14. Metal-organic framework MIL-101 as sorbent based on double-pumps controlled on-line solid-phase extraction coupled with high-performance liquid chromatography for the determination of flavonoids in environmental water samples.

    Science.gov (United States)

    Liu, Yue; Hu, Jia; Li, Yan; Li, Xiao-Shuang; Wang, Zhong-Liang

    2016-10-01

    A novel method with high sensitivity for the rapid determination of chrysin, apigenin and luteolin in environment water samples was developed by double-pumps controlled on-line solid-phase extraction (SPE) coupled with high-performance liquid chromatography (HPLC). In the developed technique, metal organic framework MIL-101 was synthesized and applied as a sorbent for SPE. The as-synthesized MIL-101 was characterized by scanning electron microscope, X-ray diffraction spectrometry, thermal gravimetric analysis and micropore physisorption analysis. The MIL-101 behaved as a fast kinetics in the adsorption of chrysin, apigenin and luteolin. On-line SPE of chrysin, apigenin and luteolin was processed by loading a sample solution at a flow rate of 1.0 mL/min for 10 min. The extracted analytes were subsequently eluted into a ZORBAX Bonus-RP analytical column (25 cm long × 4.6 mm i.d.) for HPLC separation under isocratic condition with a mobile phase (MeOH: ACN: 0.02 M H 3 PO 4 = 35:35:30) at a flow rate of 1.0 mL/min. Experimental conditions, including ionic strength, sample pH, sample loading rates, sample loading time and desorption analytes time, were further optimized to obtain efficient preconcentration and high-precision determination of the analytes mentioned above. The method achieved the merits of simplicity, rapidity, sensitivity, wide linear range and high sample throughput. The possible mechanism for the adsorption of flavonoids on MIL-101 was proposed. The developed method has been applied to determine trace chrysin, apigenin and luteolin in a variety of environmental water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. A magnetic-based dispersive micro-solid-phase extraction method using the metal-organic framework HKUST-1 and ultra-high-performance liquid chromatography with fluorescence detection for determining polycyclic aromatic hydrocarbons in waters and fruit tea infusions.

    Science.gov (United States)

    Rocío-Bautista, Priscilla; Pino, Verónica; Ayala, Juan H; Pasán, Jorge; Ruiz-Pérez, Catalina; Afonso, Ana M

    2016-03-04

    A hybrid material composed by the metal-organic framework (MOF) HKUST-1 and Fe3O4 magnetic nanoparticles (MNPs) has been synthetized in a quite simple manner, characterized, and used in a magnetic-assisted dispersive micro-solid-phase extraction (M-d-μSPE) method in combination with ultra-high-performance liquid chromatography (UHPLC) and fluorescence detection (FD). The application was devoted to the determination of 8 heavy polycyclic aromatic hydrocarbons (PAHs) in different aqueous samples, specifically tap water, wastewaters, and fruit tea infusion samples. The overall M-d-μSPE-UHPLC-FD method was optimized and validated. The method is characterized by: its simplicity in both the preparation of the hybrid material (simple mixing) and the magnetic-assisted approach (∼10min extraction time), the use of low sorbent amounts (20mg of HKUST-1 and 5mg of Fe3O4 MNPs), and the low organic solvent consumption in the overall M-d-μSPE-UHPLC-FD method (1.5mL of acetonitrile in the M-d-μSPE method and 2.8mL of acetonitrile in the UHPLC-FD run). The resulting method has high sensitivity, with LODs down to 0.8ngL(-1); adequate intermediate precision, with relative standard deviation values (RSD) always lower than 6.3% (being the range 5.9-9.0% in tap water for a spiked level of 45ngL(-1), 6.1-14% in wastewaters for a spiked level of 45ngL(-1), and 7.2-17% in fruit tea infusion samples for a spiked level of 45ngL(-1)); and adequate relative recoveries, with average values of 82% in tap water, and 94% and 75% in wastewater and fruit tea infusion samples, respectively, if using the proper matrix-matched calibration. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Recovery of Picloram and 2,4-Dichlorophenoxyacetic Acid from Aqueous Samples by Reversed-Phase Solid-Phase Extraction

    Science.gov (United States)

    Martha J.M. Wells; Jerry L. Michael

    1987-01-01

    Extensive preparation of samples before chromatographic analysis is usually the most time-consuming process in the determination of many organic compounds in environmental matrices. In the past, removal of some organic from aqueous solution was commonly done by liquid/liquid extraction. However, the introduction of stable, covalently bonded reversed-phase sorbents now...

  17. Solid phase extraction method for determination of mitragynine in ...

    African Journals Online (AJOL)

    All rights reserved. ... 1Department of Pharmacology, 2Department of Applied Science, 3Police Forensic Science Center 10, Yala 95000, 4Natural ... Purpose: To develop a solid phase extraction (SPE) method that utilizes reverse-phase high.

  18. 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.

  19. IN SITU SOLID-PHASE EXTRACTION AND ANALYSIS OF ...

    Science.gov (United States)

    Fragrance materials, such as synthetic musks in aqueous samples, are normally analyzed by GC/MS in the selected ion monitoring (SIM) mode to provide maximum sensitivity after liquid-liquid extraction of 1-L samples. A 1-L sample, however, usually provides too little analyte for full-scan data acquisition.We have developed an on-site extraction method for extracting synthetic musks from 60 L of wastewater effluent. Such a large sample volume permits high-quality, full-scan mass spectra to be obtained for various synthetic musk compounds. Quantification of these compounds was conveniently achieved from the full-scan data directly, without preparing SIM descriptors for each compound to acquire SIM data. The research focused on in the subtasks is the development and application of state-of the-art technologies to meet the needs of the public, Office of Water, and ORD in the area of Water Quality. Located In the subtasks are the various research projects being performed in support of this Task and more in-depth coverage of each project. Briefly, each project's objective is stated below.Subtask 1: To integrate state-of-the-art technologies (polar organic chemical integrative samplers, advanced solid-phase extraction methodologies with liquid chromatography/electrospray/mass spectrometry) and apply them to studying the sources and fate of a select list of PPCPs. Application and improvement of analytical methodologies that can detect non-volatile, polar, water-s

  20. Influence of radiolytic degradation products from organic phase

    International Nuclear Information System (INIS)

    Azevedo, H.L.P. de.

    1980-01-01

    The influence of primary and secondary degradation products from TBP - dodecane on zirconium extraction is studied. The presence of radiolytical degradation at organic phase, in systems of initial concentration of HNO 3 1 and 4M, and absorbed γ radiation doses from 0,5 to 4,5 Wh/l, lead to an increase of zirconium extraction, being the HDBP the main product of degradation responsable by this effect. The influence of secondary degradation products is significative in systems of HNO 3 1M initial concentration. The formation of precipitator in extractions of Zr in HNO 3 1M with irradiated TBP-dodecane was observed. (M.C.K.) [pt

  1. 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)

  2. Zirconium-based highly porous metal-organic framework (MOF-545) as an efficient adsorbent for vortex assisted-solid phase extraction of lead from cereal, beverage and water samples.

    Science.gov (United States)

    Tokalıoğlu, Şerife; Yavuz, Emre; Demir, Selçuk; Patat, Şaban

    2017-12-15

    In this study, zirconium-based highly porous metal-organic framework, MOF-545, was synthesized and characterized. The surface area of MOF-545 was found to be 2192m 2 /g. This adsorbent was used for the first time as an adsorbent for the vortex assisted-solid phase extraction of Pb(II) from cereal, beverage and water samples. Lead in solutions was determined by FAAS. The optimal experimental conditions were as follows: the amount of MOF-545, 10mg; pH of sample, 7; adsorption and elution time, 15min; and elution solvent, 2mL of 1molL -1 HCl. Under the optimal conditions of the method, the limit of detection, preconcentration factor and precision as RSD% were found to be 1.78μgL -1 , 125 and 2.6%, respectively. The adsorption capacity of the adsorbent for lead was found to be 73mgg -1 . The method was successfully verified by analyzing two certified reference materials (BCR-482 Lichen and SPS-WW1 Batch 114) and spiked chickpea, bean, wheat, lentil, cherry juice, mineral water, well water and wastewater samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. A method for the direct injection and analysis of small volume human blood spots and plasma extracts containing high concentrations of organic solvents using revered-phase 2D UPLC/MS.

    Science.gov (United States)

    Rainville, Paul D; Simeone, Jennifer L; Root, Dan S; Mallet, Claude R; Wilson, Ian D; Plumb, Robert S

    2015-03-21

    The emergence of micro sampling techniques holds great potential to improve pharmacokinetic data quality, reduce animal usage, and save costs in safety assessment studies. The analysis of these samples presents new challenges for bioanalytical scientists, both in terms of sample processing and analytical sensitivity. The use of two dimensional LC/MS with, at-column-dilution for the direct analysis of highly organic extracts prepared from biological fluids such as dried blood spots and plasma is demonstrated. This technique negated the need to dry down and reconstitute, or dilute samples with water/aqueous buffer solutions, prior to injection onto a reversed-phase LC system. A mixture of model drugs, including bromhexine, triprolidine, enrofloxacin, and procaine were used to test the feasibility of the method. Finally an LC/MS assay for the probe pharmaceutical rosuvastatin was developed from dried blood spots and protein-precipitated plasma. The assays showed acceptable recovery, accuracy and precision according to US FDA guidelines. The resulting analytical method showed an increase in assay sensitivity of up to forty fold as compared to conventional methods by maximizing the amount loaded onto the system and the MS response for the probe pharmaceutical rosuvastatin from small volume samples.

  4. A fast, simple and green method for the extraction of carbamate pesticides from rice by microwave assisted steam extraction coupled with solid phase extraction.

    Science.gov (United States)

    Song, Weitao; Zhang, Yiqun; Li, Guijie; Chen, Haiyan; Wang, Hui; Zhao, Qi; He, Dong; Zhao, Chun; Ding, Lan

    2014-01-15

    This paper presented a fast, simple and green sample pretreatment method for the extraction of 8 carbamate pesticides in rice. The carbamate pesticides were extracted by microwave assisted water steam extraction method, and the extract obtained was immediately applied on a C18 solid phase extraction cartridge for clean-up and concentration. The eluate containing target compounds was finally analysed by high performance liquid chromatography with mass spectrometry. The parameters affecting extraction efficiency were investigated and optimised. The limits of detection ranging from 1.1 to 4.2ngg(-1) were obtained. The recoveries of 8 carbamate pesticides ranged from 66% to 117% at three spiked levels, and the inter- and intra-day relative standard deviation values were less than 9.1%. Compared with traditional methods, the proposed method cost less extraction time and organic solvent. Copyright © 2013 Elsevier Ltd. All rights reserved.

  5. Modified resins for solid-phase extraction

    Science.gov (United States)

    Fritz, James S.; Sun, Jeffrey J.

    1991-12-10

    A process of treating aqueous solutions to remove organic solute contaminants by contacting an aqueous solution containing polar organic solute contaminants with a functionalized polystyrene-divinyl benzene adsorbent resin, with the functionalization of said resin being accomplished by organic hydrophilic groups such as hydroxymethyl, acetyl and cyanomethyl.

  6. Uranium extraction from colofanite via organic solvents

    International Nuclear Information System (INIS)

    Ribeiro, Valeria Aparecida Leitao

    2007-01-01

    This work describes the use of pure or combined extractants dissolved in organic solvents for quantitative uranium recovery from colofanite, a fluoroapatite ore, from Itataia, Santa Quiteria, Ceara, Brazil. This ore contains the highest brazilian uranium reserve. The metal is associated to phosphate species. The ore is digested with sulfuric acid (wet process), producing phosphoric acid, which is used for manufacturing of fertilizers and animal food. >From the acid leaching, some systems for uranium recovery were tested. Among them, PC88A (2-ethyl-hexyl phosphonic acid, mono-2-ethyl-hexyl ester) 40% vol. and DEHPA (di(2-ethyl-hexyl)phosphoric acid) 40% vol. in kerosene presented the highest values for the distribution coefficient (D) for uranium. When synergistic systems were employed, the best results were obtained for DEHPA 40%vol. + PC88A 40%vol. and DEHPA 40% vol. + TOPO (trioctylphosphine oxide) 5% vol. in kerosene. 15% wt/v sodium carbonate was the best medium for uranium stripping and separation from iron, the main interfering element. Uranium was precipitated as sodium diuranate by adding sodium hydroxide (5,0 mol L -1 ). Thorium in the raffinate was extracted by TOPO (0,1% vol.) in cyclohexane. The radioactivity level of the final aqueous waste is similar to natural background, according to CNEN-NE 6.05 Norm. After neutralization, the solid can be co-processed, according to the Directory 264 from the National Brazilian Environmental Council (CONAMA), whereas the treated effluent can be discarded according to the Directory 357 from CONAMA. (author)

  7. solid phase extraction method for selective determination

    African Journals Online (AJOL)

    FATOKI

    determination of phthalate ester plasticizers in rivers and marine water samples. Of the ... samples that receive effluent from industries that use phthalate esters. ... Keywords Phthalates, Plasticizers, Solid Phase Gas Chromatography.

  8. Determination of 8 Synthetic Food Dyes by Solid Phase Extraction ...

    African Journals Online (AJOL)

    Keywords: Synthetic colors, Food, Fruit flavored drinks, Solid phase extraction, RP-HPLC. Tropical Journal of ..... food dyes by thin-layer chromatography-fast atom bombardment ... food dyes in soft drinks containing natural pigments by.

  9. A novel metal-organic framework composite MIL-101(Cr)@GO as an efficient sorbent in dispersive micro-solid phase extraction coupling with UHPLC-MS/MS for the determination of sulfonamides in milk samples.

    Science.gov (United States)

    Jia, Xiuna; Zhao, Pan; Ye, Xiu; Zhang, Lianjun; Wang, Ting; Chen, Qinyu; Hou, Xiaohong

    2017-07-01

    As a novel material, metal-organic framework/graphite oxide (MIL-101(Cr)@GO) has great potential for the pretreatment of trace analytes. In the present study, MIL-101(Cr)@GO was synthesized using a solvothermal synthesis method at the nanoscale and was applied as sorbent in the dispersive micro-solid phase extraction (DMSPE) for the enrichment of the trace sulfonamides (SAs) from milk samples for the first time. Several experimental parameters including kinds of sorbents, the effect of pH, the amount of MIL-101(Cr)@GO, ionic strength, adsorption time, desorption solvent and desorption time were investigated. Under the optimal conditions, the linear ranges were from 0.1 to 10μg/L, 0.2-20μg/L or 0.5-50μg/L for the analytes with regression coefficients (r) from 0.9942 to 0.9999. The limits of detection were between 0.012 and 0.145μg/L. The recoveries ranged from 79.83% to 103.8% with relative standard deviations (RSDs)MIL-101(Cr)@GO exhibited remarkable advantages compared to MIL-101(Cr), MIL-100(Fe), activated carbon and other sorbent materials used in pretreatment methods. A simple, rapid, sensitive, inexpensive and less solvent consuming method of DMSPE-ultra-high performance liquid chromatography-tandem mass spectrometry (DMSPE-UHPLC-MS/MS) was successfully applied to the pre-concentration and determination of twelve SAs in milk samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. 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 ...

  11. Phase 1 remediation of jet fuel contaminated soil and groundwater at JFK International Airport using dual phase extraction and bioventing

    International Nuclear Information System (INIS)

    Roth, R.; Bianco, P. Rizzo, M.

    1995-01-01

    Soil and groundwater contaminated with jet fuel at Terminal One of the JFK International Airport in New York have been remediated using dual phase extraction (DPE) and bioventing. Two areas were remediated using 51 DPE wells and 20 air sparging/air injection wells. The total area remediated by the DPE wells is estimated to be 4.8 acres. Groundwater was extracted to recover nonaqueous phase and aqueous phase jet fuel from the shallow aquifer and treated above ground by the following processes; oil/water separation, iron-oxidation, flocculation, sedimentation, filtration, air stripping and liquid-phase granular activated carbon (LPGAC) adsorption. The extracted vapors were treated by vapor-phase granular activated carbon (VPGAC) adsorption in one area, and catalytic oxidation and VPGAC adsorption in another area. After 6 months of remediation, approximately 5,490 lbs. of volatile organic compounds (VOCs) were removed by soil vapor extraction (SVE), 109,650 lbs. of petroleum hydrocarbons were removed from the extracted groundwater, and 60,550 lbs. of petroleum hydrocarbons were biologically oxidized by subsurface microorganisms. Of these three mechanisms, the rate of petroleum hydrocarbon removal was the highest for biological oxidation in one area and by groundwater extraction in another area

  12. Analysis of polar organic contaminants in surface water of the northern Adriatic Sea by solid-phase extraction followed by ultrahigh-pressure liquid chromatography-QTRAP® MS using a hybrid triple-quadrupole linear ion trap instrument.

    Science.gov (United States)

    Loos, Robert; Tavazzi, Simona; Paracchini, Bruno; Canuti, Elisabetta; Weissteiner, Christof

    2013-07-01

    Water-soluble polar organic contaminants are discharged by rivers, cities, and ships into the oceans. Little is known on the fate, pollution effects, and thresholds of toxic chemical mixtures in the marine environment. A new trace analytical method was developed for the multi-compound analysis of polar organic chemical contaminants in marine waters. The method is based on automated solid-phase extraction (SPE) of one-liter water samples followed by ultrahigh-pressure liquid chromatography triple-quadrupole linear ion-trap mass spectrometry (UHPLC-QTRAP(®) MS). Marine water samples from the open Adriatic Sea taken 16 km offshore from Venice (Italy) were analyzed. Method limits of quantification (LOQs) in the low picogram per liter (pg/l) concentration range were achieved. Among the 67 target chemicals analyzed, 45 substances could be detected above the LOQ. The chemicals detected at the highest concentrations were caffeine (up to 367 ng/l), nitrophenol (36 ng/l), 2,4-dinitrophenol (34 ng/l), 5-methyl-1H-benzotriazole (18.5 ng/l), sucralose (11 ng/l), 1H-benzotriazole (9.2 ng/l), terbuthylazine (9 ng/l), alachlor (7.7 ng/l), atrazine-desisopropyl (6.6 ng/l), diethyltoluamide (DEET) (5.0 ng/l), terbuthylazine-desethyl (4.3 ng/l), metolachlor (2.8 ng/l), perfluorooctanoic acid (PFOA) (2.5 ng/l), perfluoropentanoic acid (PFPeA) (2.3 ng/l), linuron (2.3 ng/l), perfluorohexanoic acid (PFHxA) (2.2 ng/l), diuron (2.0 ng/l), perfluorohexane sulfonate (PFHxS) (1.6 ng/l), simazine (1.6 ng/l), atrazine (1.5 ng/l), and perfluorooctane sulfonate (PFOS) (1.3 ng/l). Higher concentrations were detected during summer due to increased levels of tourist activity during this period.

  13. C18, C8, and perfluoro reversed phases on diamond for solid-phase extraction.

    Science.gov (United States)

    Saini, Gaurav; Wiest, Landon A; Herbert, David; Biggs, Katherine N; Dadson, Andrew; Vail, Michael A; Linford, Matthew R

    2009-04-17

    In spite of advances in solid-phase extraction (SPE) technology there are certain disadvantages to current SPE silica-based, column packings. The pH range over which extraction can occur is limited and each column is generally only used once. New diamond-based reversed SPE phases (C(18), C(8), and perfluorinated) were developed in our laboratories. Studies were done which show that these phases do not have the same limitations as traditional silica-based stationary phases. The synthesis and properties of these diamond-based phases are presented, and the stability, percent recovery, and column capacity are given for the C(18) phase.

  14. Dual focal-spot imaging for phase extraction in phase-contrast radiography

    International Nuclear Information System (INIS)

    Donnelly, Edwin F.; Price, Ronald R.; Pickens, David R.

    2003-01-01

    The purpose of this study was to evaluate dual focal spot imaging as a method for extracting the phase component from a phase-contrast radiography image. All measurements were performed using a microfocus tungsten-target x-ray tube with an adjustable focal-spot size (0.01 mm to 0.045 mm). For each object, high-resolution digital radiographs were obtained with two different focal spot sizes to produce matched image pairs in which all other geometric variables as well as total exposure and tube kVp were held constant. For each image pair, a phase extraction was performed using pixel-wise division. The phase-extracted image resulted in an image similar to the standard image processing tool commonly referred to as 'unsharp masking' but with the additional edge-enhancement produced by phase-contrast effects. The phase-extracted image illustrates the differences between the two images whose imaging parameters differ only in focal spot size. The resulting image shows effects from both phase contrast as well as geometric unsharpness. In weakly attenuating materials the phase-contrast effect predominates, while in strongly attenuating materials the phase effects are so small that they are not detectable. The phase-extracted image in the strongly attenuating object reflects differences in geometric unsharpness. The degree of phase extraction depends strongly on the size of the smallest focal spot used. This technique of dual-focal spot phase-contrast radiography provides a simple technique for phase-component (edge) extraction in phase-contrast radiography. In strongly attenuating materials the phase-component is overwhelmed by differences in geometric unsharpness. In these cases the technique provides a form of unsharp masking which also accentuates the edges. Thus, the two effects are complimentary and may be useful in the detection of small objects

  15. Organic light emitting diode with light extracting electrode

    Energy Technology Data Exchange (ETDEWEB)

    Bhandari, Abhinav; Buhay, Harry

    2017-04-18

    An organic light emitting diode (10) includes a substrate (20), a first electrode (12), an emissive active stack (14), and a second electrode (18). At least one of the first and second electrodes (12, 18) is a light extracting electrode (26) having a metallic layer (28). The metallic layer (28) includes light scattering features (29) on and/or in the metallic layer (28). The light extracting features (29) increase light extraction from the organic light emitting diode (10).

  16. Solid phase extraction and metabolic profiling of exudates from living copepods

    DEFF Research Database (Denmark)

    Selander, Erik; Heuschele, Jan; Nylund, Göran M.

    2016-01-01

    describe the development of a closed loop solid phase extraction setup that allows for extraction of exuded metabolites from live copepods. We captured exudates from male and female Temora longicornis and analyzed the content with high resolution LC-MS. Chemometric methods revealed 87 compounds...... that solid phase extraction in combination with metabolic profiling of exudates is a useful tool to develop our understanding of the chemical interplay between pelagic organisms....... Copepodamide G, known to induce defensive responses in phytoplankton, was among the ten compounds of highest relative abundance in both male and female extracts. The presence of copepodamide G shows that the method can be used to capture and analyze chemical signals from living source organisms. We conclude...

  17. 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

  18. Extending the analytical window for water-soluble organic matter in sediments by aqueous Soxhlet extraction

    Science.gov (United States)

    Schmidt, Frauke; Koch, Boris P.; Witt, Matthias; Hinrichs, Kai-Uwe

    2014-09-01

    Dissolved organic matter (DOM) in marine sediments is a complex mixture of thousands of individual constituents that participate in biogeochemical reactions and serve as substrates for benthic microbes. Knowledge of the molecular composition of DOM is a prerequisite for a comprehensive understanding of the biogeochemical processes in sediments. In this study, interstitial water DOM was extracted with Rhizon samplers from a sediment core from the Black Sea and compared to the corresponding water-extractable organic matter fraction (Soxhlet extraction, which mobilizes labile particulate organic matter and DOM. After solid phase extraction (SPE) of DOM, samples were analyzed for the molecular composition by Fourier Transform Ion-Cyclotron Resonance Mass Spectrometry (FT-ICR MS) with electrospray ionization in negative ion mode. The average SPE extraction yield of the dissolved organic carbon (DOC) in interstitial water was 63%, whereas less than 30% of the DOC in Soxhlet-extracted organic matter was recovered. Nevertheless, Soxhlet extraction yielded up to 4.35% of the total sedimentary organic carbon, which is more than 30-times the organic carbon content of the interstitial water. While interstitial water DOM consisted primarily of carbon-, hydrogen- and oxygen-bearing compounds, Soxhlet extracts yielded more complex FT-ICR mass spectra with more peaks and higher abundances of nitrogen- and sulfur-bearing compounds. The molecular composition of both sample types was affected by the geochemical conditions in the sediment; elevated concentrations of HS- promoted the early diagenetic sulfurization of organic matter. The Soxhlet extracts from shallow sediment contained specific three- and four-nitrogen-bearing molecular formulas that were also detected in bacterial cell extracts and presumably represent proteinaceous molecules. These compounds decreased with increasing sediment depth while one- and two-nitrogen-bearing molecules increased, resulting in a higher

  19. 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)

  20. The application of three-phase liquid-liquid extraction to the analysis of bismuth and tellurium in sulphide concentrates

    International Nuclear Information System (INIS)

    Nicholas, D.J.

    1976-01-01

    An extraction system consisting of one aqueous and two organic phases is described. Diantipyrylmethane (DAM) is used as the extractant for bismuth and tellurium, which are extracted into the smaller of the two organic phases from nitric acid and perchloric acid respectively. The extraction efficiency is in the range of 90 to 95 per cent, compensation for incomplete extraction being made by the technique of standard addition. Copper, lead, and zinc are not extracted in either procedure. When the solutions contain high concentrations of iron, thioglycolic acid is used as a masking agent for iron in the extraction of bismuth. Atomic-absorption spectrophotometry is used for the analysis of the third phase after it has been diluted with methanol. The precision for bismuth and tellurium is in the range of 3 to 4 per cent. The accuracy, as ascertained from comparative analyses of sulphide concentrates, is good

  1. The metal-organic framework HKUST-1 as efficient sorbent in a vortex-assisted dispersive micro solid-phase extraction of parabens from environmental waters, cosmetic creams, and human urine.

    Science.gov (United States)

    Rocío-Bautista, Priscilla; Martínez-Benito, Carla; Pino, Verónica; Pasán, Jorge; Ayala, Juan H; Ruiz-Pérez, Catalina; Afonso, Ana M

    2015-07-01

    Three metal-organic frameworks (MOFs), specifically HKUST-1, MOF-5, and MIL-53(Al), have been synthetized, characterized, studied and compared in a vortex-assisted dispersive micro-solid-phase extraction (VA-D-µ-SPE) procedure in combination with high-performance liquid chromatography (HPLC) with diode-array detection (DAD) for determining seven parabens in environmental waters (tap water, swimming pool water, and water coming from a spa pool), human urine (from two volunteers), and cosmetic creams (two commercial brands). Experimental parameters, such as nature and amount of MOF, sample volume, nature of elution solvent and its amount, vortex and centrifugation time, among others, were properly optimized. HKUST-1 was the most adequate MOF to work with. Detection limits for the overall method down to 0.1 μgL(-1) for butylparaben (BPB) and benzylparaben (BzPB) were obtained, with determination coefficients (R(2)) higher than 0.9966 for a range of 0.5-147 μgL(-1) (depending on the paraben), average relative recoveries (RR, in %) of 80.3% at the low spiked level (7 μgL(-1)), and relative standard deviation (RSD) values below 10% also at the low spiked level. The strength of the affinity between HKUST-1 and parabens was evaluated, and it ranged from 33.5% for isopropylparaben (iPPB) to 77.0% for isobutylparaben (iBPB). When analyzing complex environmental waters, RR values of 78%, inter-day precision values (as RSD) lower than 15%, and intra-day precision values lower than 7.8% were obtained, despite the observed matrix effect. When analyzing cosmetic creams, parabens were detected, with contents ranging from 0.14 ± 0.01 μgg(-1) for EPB in the healing cream analyzed to 1.12 ± 0.07 mgg(-1) for MPB in the mask cream analyzed, with precision values (RSD) lower than 12% and RR values from 63.7% for propylparaben (PPB) to 121% for iPPB. When analyzing human urine, no parabens were detected but the method could be performed with RSD values lower than 19%. These

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

    Science.gov (United States)

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

    2012-01-21

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

  3. Organic solvents in electromembrane extraction: recent insights

    DEFF Research Database (Denmark)

    Huang, Chuixiu; Gjelstad, Astrid; Pedersen-Bjergaard, Stig

    2016-01-01

    the introduction. Under the influence of an electrical field, EME is based on electrokinetic migration of the analytes through a supported liquid membrane (SLM), which is an organic solvent immobilized in the pores of the polymeric membrane, and into the acceptor solution. Up to date, close to 150 research...... articles with focus on EME have been published. The current review summarizes the performance of EME with different organic solvents and discusses several criteria for efficient solvents in EME. In addition, the authors highlight their personal perspective about the most promising organic solvents for EME...... and have indicated that more fundamental work is required to investigate and discover new organic solvents for EME....

  4. Fast and simple screening for the simultaneous analysis of seven metabolites derived from five volatile organic compounds in human urine using on-line solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Chiang, Wen-Chieh; Chen, Chao-Yu; Lee, Ting-Chen; Lee, Hui-Ling; Lin, Yu-Wen

    2015-01-01

    Recently, the International Agency for Research on cancer classified outdoor air pollution and particulate matter from outdoor air pollution as carcinogenic to humans (IARC Group 1), based on sufficient evidence of carcinogenicity in humans and experimental animals and strong mechanistic evidence. In particular, a wide variety of volatile organic compounds (VOCs) are volatized or released into the atmosphere and can become ubiquitous, as they originate from many different natural and anthropogenic sources, such as paints, pesticides, vehicle exhausts, cooking fumes, and tobacco smoke. Humans may be exposed to VOCs through inhalation, ingestion, or dermal contact, which may increase the risk of leukemia, birth defects, neurocognitive impairment, and cancer. Therefore, the focus of this study was the development of a simple, effective and rapid sample preparation method for the simultaneous determination of seven metabolites (6 mercaptic acids+t,t-muconic acid) derived from five VOCs (acrylamide, 1,3-butadiene, acrylonitrile, benzene, and xylene) in human urine by using automated on-line solid-phase extraction (SPE) coupled with liquid chromatography-electrospray tandem mass spectrometry (LC-MS/MS). An aliquot of each diluted urinary sample was directly injected into an autosampler through a trap column to reduce contamination, and then the retained target compounds were eluted by back-flush mode into an analytical column for separation. Negative electrospray ionization tandem mass spectrometry was utilized for quantification. The coefficients of correlation (r(2)) for the calibration curves were greater than 0.995. Reproducibility was assessed by the precision and accuracy of intra-day and inter-day precision, which showed results for coefficient of variation (CV) that were low 0.9 to 6.6% and 3.7 to 8.5%, respectively, and results for recovery that ranged from 90.8 to 108.9% and 92.1 to 107.7%, respectively. The limits of detection (LOD) and limits of

  5. Extraction and Ozonation of organic pollutants in drinking waters

    International Nuclear Information System (INIS)

    Kenawi, I.M.; Barsoum, B.N.; Abdelhaflz, M.M.

    2006-01-01

    The continuous liquid-liquid, CLLE, and solid-phase, SPE. extraction techniques were used to study a problem of international relevance. The work was incident on the evaluation of the efficiency and optimisation of extruding techniques, CLLE. SPE and CLLEt-SPE, towards chlorinated pesticides and phenolic compounds from the Giza treatment plant station (Egypt), where the degree of pollution of such substances in drinking waters must be reduced. The total recoveries, rs, using SPE ranged between I).74 -0.87, whereas, the values were much less using the other two methods (0.158 - 0.1961; indicating the preferability of the SF'E technique. Analytical results were obtained through the various chromatographic techniques, liquid or gas. with adequately chosen detectors. A simple mathematical algorithm has been empirically developed allowing the assessment and comparison of the efficiencies of the three extracting procedures. Further treatment with ozone resulted in the oxidation and elimination of organic pollutants, with consequent improvement of water quality (total pesticide content 0.332-0.19μgL -1 ). A useful ozone treatment unit, capable of dealing with the emanation of contaminants in tap water, was built

  6. Poly(Dimethylsiloxane)-Poly(Vinyl Alcohol) Coated Solid Phase Micro extraction Fiber for Chloropyrifos Analysis

    International Nuclear Information System (INIS)

    Wan Aini Wan Ibrahim; Nor Fairul Zukry Ahmad Rasdy; Norfazilah Muhamad

    2016-01-01

    Traditional liquid - liquid extraction of pesticides consumes large volumes of organic solvent which are hazardous to the operator and is not environment friendly. Solid phase micro extraction (SPME) is a solvent less extraction method which is safer to the operator and is environmental friendly. A sol-gel hybrid fibre coating material, poly(dimethylsiloxane)-poly(vinyl alcohol) (PDMS-PVA) was synthesized and used in head space solid phase micro extraction (HS-SPME) of chloropyrifos. The thickness of the synthesised PDMS-PVA fiber coating was 13.5 μm and it is thermally stable up to 400 degree Celsius. The PDMS-PVA sol-gel hybrid fiber was also stable to two organic solvents tested; acetonitrile and dichloromethane (1 hour dipping) and showed no significant changes in extraction performance for chloropyrifos. Extracted chloropyrifos was analysed using gas chromatography electron capture detector (GC-ECD). Optimum SPME parameters affecting the PDMS-PVA HS-SPME performance namely extraction time (15 min), extraction temperature (50 degree Celsius), desorption time (5 min), desorption temperature (260 degree Celsius) and stirring rate (120 rpm) were used for extraction. It was found that HSSPME using PDMS-PVA sol-gel fiber gave significantly better extraction performance of chloropyrifos compared to commercial 100 μm PDMS fiber. The PDMS-PVA fiber showed excellent operational performances such as temperature stability (up to 380 degree Celsius), coating lifetime (up to 170 times use) and organic solvent stability. The PDMS-PVA-HS-SPME method showed excellent recovery for chloropyrifos from tomatoes (98.0 %, 5.9 % RSD) at 0.01 μg/ g spiked level (5 times lower than maximum residue limit set by European Union). (author)

  7. Effect of Morinda Morindiodes Extracts on Organs of Mice Infected ...

    African Journals Online (AJOL)

    Effect of Morinda Morindiodes Extracts on Organs of Mice Infected with ... The histological evaluation of the effect of Morinda(M.) morindiodes plant part(s) extracts in the treatment ... Control animals were given water for the same period of time.

  8. Determination of total and extractable hydrogen peroxide in organic and aqueous solutions of uranyl nitrate

    International Nuclear Information System (INIS)

    Goodall, Ph.

    1999-01-01

    The development of a spectrophotometric method for the determination of hydrogen peroxide in uranyl nitrate solutions is reported. The method involves the measurement of the absorbance at 520 mm of a vanadyl peroxide species. This species was formed by the addition of a reagent consisting of vanadium (V) (50 mmol x dm -3 ) in dilute sulphuric acid (2 mol x dm -3 H 2 SO 4 ). This reagent, after dilution, was also used as an extractant for organic phase samples. The method is simple and robust and tolerant of nitric acid and U(VI). Specificity and accuracy were improved by the application of solid phase extraction techniques to remove entrained organic solvents and Pu(VI). Reverse phase solid phase extraction was used to clean-up aqueous samples or extracts which were contaminated with entrained solvent. A solid phase extraction system based upon an extraction chromatography system was used to remove Pu(IV). Detection limits of 26 μmol x dm -3 (0.88 μg x cm -3 ) or 7 μmol x dm -3 (0.24 μg x cm -3 ) for, respectively, a 1 and 4 cm path length cell were obtained. Precisions of RSD = 1.4% and 19.5% were obtained at the extremes of the calibration curve (5 mmol x dm -3 and 50 μmol x dm -3 H 2 O 2 , 1 cm cell). The introduction of the extraction and clean-up stages had a negligible effect upon the precision of the determination. The stability of an organic phase sample was tested and no loss of analyte could be discerned over a period of at least 5 days. (author)

  9. Phase extraction equilibria in systems rare earth (3) nitrates-ammonium nitrate-water-trialkylmethylammonium nitrate

    International Nuclear Information System (INIS)

    Pyartman, A.K.; Kopyrin, A.A.; Puzikov, E.A.

    1995-01-01

    The distribution of rare earth metals (3) between aqueous and organic phases in the systems rare earth metal (3) (praseodymium-lutetium (3), yttrium (3)) nitrate-ammonium nitrate-water-trialkylmethylammonium (kerosene diluent nitrate has been studied. It is shown that in organic phase di- and trisolvates of metals (3) with tralkylmethylammonium nitrate are formed. The influence of concentration of rare earth metal (3) nitrate and ammonium nitrate on the values of extraction concentrational constants has been ascertained: they decrease with increase in the ordinal number of lanthanide (3). 11 refs., 4 figs. 1 tab

  10. Methods of Analysis by the U.S. Geological Survey Organic Geochemistry Research Group?Determination of acetamide herbicides and their degradation products in water using online solid-phase extraction and liquid chromatography/mass spectrometry

    Science.gov (United States)

    Lee, E.A.; Strahan, A.P.

    2003-01-01

    An analytical method for the determination of 6 acetamide herbicides (acetochlor, alachlor, dimethenamid, flufenacet, metolachlor, and propachlor) and 16 of their degradation products in natural water samples using solid-phase extraction and liquid chromatography/mass spectrometry is described in this report. Special consideration was given during the development of the method to prevent the formation of degradation products during the analysis. Filtered water samples were analyzed using octadecylsilane as the solid-phase extraction media on online automated equipment followed by liquid chromatography/mass spectrometry. The method uses only 10 milliliters of sample per injection. Three different water-sample matrices, a reagent-water, a ground-water, and a surface-water sample spiked at 0.10 and 1.0 microgram per liter, were analyzed to determine method performance. Method detection limits ranged from 0.004 to 0.051 microgram per liter for the parent acetamide herbicides and their degradation products. Mean recoveries for the acetamide compounds in the ground- and surface-water samples ranged from 62.3 to 117.4 percent. The secondary amide of acetochlor/metolachlor ethanesulfonic acid (ESA) was recovered at an average rate of 43.5 percent. The mean recoveries for propachlor and propachlor oxanilic acid (OXA) were next lowest, ranging from 62.3 to 95.5 percent. Mean recoveries from reagent-water samples ranged from 90.3 to 118.3 percent for all compounds. Overall the mean of the mean recoveries of all compounds in the three matrices spiked at 0.10 and 1.0 microgram per liter ranged from 89.9 to 100.7 percent, including the secondary amide of acetochlor/metolachlor ESA and the propachlor compounds. The acetamide herbicides and their degradation products are reported in concentrations ranging from 0.05 to 2.0 micrograms per liter. The upper concentration limit is 2.0 micrograms per liter for all compounds without dilution. With the exception of the secondary amide of

  11. Methods of analysis by the U.S. Geological Survey Organic Geochemistry Research Group; determination of glyphosate, aminomethylphosphonic acid, and glufonsinate in water using online solid-phase extraction and high-performance liquid chromat

    Science.gov (United States)

    Lee, E.A.; Strahan, A.P.; Thurman, E.M.

    2001-01-01

    An analytical method for the determination of glyphosate, its principal degradation compound, aminomethylphosphonic acid (AMPA), and glufosinate in water with varying matrices has been developed. Four different sample matrices fortified at 0.2 and 2.0 ?g/L (micrograms per liter) were analyzed using precolumn derivatization with 9-fluorenylmethylchloroformate (FMOC). After derivatization, cleanup and concentration were accomplished using automated online solid-phase extraction followed by elution with the mobile phase allowing for direct injection into a liquid chromatograph/mass spectrometer (LC/MS). Analytical conditions for MS detection were optimized, and quantitation was carried out using the following representative ions: 390 and 168 for glyphosate; 332, 110, and 136 for AMPA; and 402, 180, and 206 for glufosinate. Matrix effects were minimized by utilizing standard addition for quantification and an isotope-labeled glyphosate (2-13C,15N) as the internal standard. Method detection limits (MDLs) were 0.084 ?g/L for glyphosate, 0.078 ?g/L for AMPA, and 0.057 ?g/L for glufosinate. The method reporting limits (MRLs) were set at 0.1 ?g/L for all three compounds. The mean recovery values ranged from 88.0 to 128.7 percent, and relative standard deviation values ranged from 5.6 to 32.6 percent.

  12. Organics in water contamination analyzer, phase 1

    Science.gov (United States)

    1986-01-01

    The requirements which would result in identifying the components of an automatic analytical system for the analysis of specific organic compounds in the space station potable water supply are defined. The gas chromatographic system for such an analysis is limited to commercially available off-the-shelf hardware and includes the sample inlet, an ionization detector, capillary columns as well as computerized compound identification. The sampling system will be a special variation of the purge and trap Tenax mode using six-port valves and a 500 microliter water sample. Capillary columns used for the separating of contaminants will be bonded phase fused silica with a silicone stationary phase. Two detectors can be used: photoionization and far ultraviolet, since they are sensitive and compatible with capillary columns. A computer system evaluation and program with the principle of compound identification based on the retention index is presented.

  13. Hypercrosslinked particles for the extraction of sweeteners using dispersive solid-phase extraction from environmental samples.

    Science.gov (United States)

    Lakade, Sameer S; Zhou, Qing; Li, Aimin; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa M

    2018-04-01

    This work presents a new extraction material, namely, Q-100, based on hypercrosslinked magnetic particles, which was tested in dispersive solid-phase extraction for a group of sweeteners from environmental samples. The hypercrosslinked Q-100 magnetic particles had the advantage of suitable pore size distribution and high surface area, and showed good retention behavior toward sweeteners. Different dispersive solid-phase extraction parameters such as amount of magnetic particles or extraction time were optimized. Under optimum conditions, Q-100 showed suitable apparent recovery, ranging in the case of river water sample from 21 to 88% for all the sweeteners, except for alitame (12%). The validated method based on dispersive solid-phase extraction using Q-100 followed by liquid chromatography with tandem mass spectrometry provided good linearity and limits of quantification between 0.01 and 0.1 μg/L. The method was applied to analyze samples from river water and effluent wastewater, and four sweeteners (acesulfame, saccharin, cyclamate, and sucralose) were found in both types of sample. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. The effect of organic water-miscible solvents on the extraction of uranium by TOA

    International Nuclear Information System (INIS)

    Shi Xiukun; Shen Xinghai; Pen Qixiu; Gao Hongchen

    1989-01-01

    The effect of organic water-miscible solvents, such as methanol, ethanol, acetone, dioxane, glycol, dimethylsulfoxide (DMSO), dimethylformamide (DMF), tetrahydrofurance (THF) in aqueous phase on the extraction of uranyl sulphate by tri-n-octylamine (TOA) has been investigated. All data obtained showed that the addition of alcohols, ketones etc. into aqueous phase brings about an increase of distribution ratio of uranium, whereas the addition of DMSO, DMF etc. brings about a decrease of distribution ratio of uranium. In the present study, the regularity and mechanism of extraction with TOA are further studied and discussed from the measurements of some physical properties, such as dielectric constant, interface tension etc

  15. ON-SITE SOLID-PHASE EXTRACTION AND LABORATORY ...

    Science.gov (United States)

    Fragrance materials such as synthetic musks in aqueous samples, are normally determined by gas chromatography/mass spectrometry in the selected ion monitoring (SIM) mode to provide maximum sensitivity after liquid-liquid extraction of I -L samples. Full-scan mass spectra are required to verify that a target analyte has been found by comparison with the mass spectra of fragrance compounds in the NIST mass spectral library. A I -L sample usually provides insufficient analyte for full scan data acquisition. This paper describes an on-site extraction method developed at the U.S. Environmental Protection Agency (USEPA)- Las Vegas Nevada - for synthetic musks from 60 L of wastewater effluent. Such a large sample volume permits high-quality, full-scan mass spectra to be obtained for a wide array of synthetic musks. Quantification of these compounds was achieved from the full-scan data directly, without the need to acquire SIM data. The detection limits obtained with this method are an order of magnitude lower than those obtained from liquid-liquid and other solid phase extraction methods. This method is highly reproducible, and recoveries ranged from 80 to 97% in spiked sewage treatment plant effluent. The high rate of sorbent-sample mass transfer eliminated the need for a methanolic activation step, which reduced extraction time, labor, and solvent use, More samples could be extracted in the field at lower cost. After swnple extraction, the light- weight cartridges ar

  16. Platform construction and extraction mechanism study of magnetic mixed hemimicelles solid-phase extraction

    Science.gov (United States)

    Xiao, Deli; Zhang, Chan; He, Jia; Zeng, Rong; Chen, Rong; He, Hua

    2016-12-01

    Simple, accurate and high-throughput pretreatment method would facilitate large-scale studies of trace analysis in complex samples. Magnetic mixed hemimicelles solid-phase extraction has the power to become a key pretreatment method in biological, environmental and clinical research. However, lacking of experimental predictability and unsharpness of extraction mechanism limit the development of this promising method. Herein, this work tries to establish theoretical-based experimental designs for extraction of trace analytes from complex samples using magnetic mixed hemimicelles solid-phase extraction. We selected three categories and six sub-types of compounds for systematic comparative study of extraction mechanism, and comprehensively illustrated the roles of different force (hydrophobic interaction, π-π stacking interactions, hydrogen-bonding interaction, electrostatic interaction) for the first time. What’s more, the application guidelines for supporting materials, surfactants and sample matrix were also summarized. The extraction mechanism and platform established in the study render its future promising for foreseeable and efficient pretreatment under theoretical based experimental design for trace analytes from environmental, biological and clinical samples.

  17. Solvent extraction of thorium(IV) with dibutyldithiophosphoric acid in various organic solvents

    International Nuclear Information System (INIS)

    Curtui, M.; Haiduc, I.

    1994-01-01

    The extraction of thorium(IV) from perchlorate solutions with di-n-butyldithiophosphoric acid (HBudtp) in various organic solvents occurs through an ion exchange mechanism. The extracted species in the organic phase is an eight-coordinate complex Th(Budtp) 4 . The higher values of the distribution ratio obtained in HBudtp-benzene-water system than in HBudtp-n-butanol-water system are explained by higher solubility of the complex species in nonpolar solvents. The position of the extraction curves in the pH-range lower than 0.7 reduces the complexation of thorium(IV) with Budtp - in the aqueous phase and also the hydrolysis process. (author) 8 refs.; 4 figs.; 1 tab

  18. Method of analysis and quality-assurance practices for determination of pesticides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry at the U.S. Geological Survey California District Organic Chemistry Laboratory, 1996-99

    Science.gov (United States)

    Crepeau, Kathryn L.; Baker, Lucian M.; Kuivila, Kathryn

    2000-01-01

    A method of analysis and quality-assurance practices were developed to study the fate and transport of pesticides in the San Francisco Bay-Estuary by the U.S. Geological Survey. Water samples were filtered to remove suspended-particulate matter and pumped through C-8 solid-phase extraction cartridges to extract the pesticides. The cartridges were dried with carbon dioxide and the pesticides were eluted with three cartridge volumes of hexane:diethyl ether (1:1) solution. The eluants were analyzed using capillary-column gas chromatography/mass spectrometry in full-scan mode. Method detection limits for pesticides ranged from 0.002 to 0.025 microgram per liter for 1-liter samples. Recoveries ranged from 44 to 140 percent for 25 pesticides in samples of organic-free reagent water and Sacramento-San Joaquin Delta and Suisun Bay water fortified at 0.05 and 0.50 microgram per liter. The estimated holding time for pesticides after extraction on C-8 solid-phase extraction cartridges ranged from 10 to 257 days.

  19. Attractive interactions between reverse aggregates and phase separation in concentrated malonamide extractant solutions

    International Nuclear Information System (INIS)

    Erlinger, C.; Belloni, L.; Zemb, T.; Madic, C.

    1999-01-01

    Using small angle X-ray scattering, conductivity, and phase behavior determination, the authors show that concentrated solutions of malonamide extractants, dimethyldibutyltetradecylmalonamide (DMDBTDMA), are organized in reverse oligomeric aggregates which have many features in common with reverse micelles. The aggregation numbers of these reverse globular aggregates as well as their interaction potential are determined from absolute scattering curves. An attractive interaction is responsible for the demixing of the oil phase when in equilibrium with excess oil. Prediction of conductivity as well as the formation conditions for the third phase is possible using standard liquid theory applied to the extractant aggregates. The interactions, modeled with the sticky sphere model proposed by Baster, are shown to be due to steric interactions resulting from the hydrophobic tails of the extractant molecule and van der Waals forces between the highly polarizable water core of the reverse micelles. The attractive interaction in the oil phase, equilibrated with water, is determined as a function of temperature, extractant molecule concentration, and proton and neodynium(III) cation concentration. It is shown that van der Waals interactions, with an effective Hamaker constant of 3kT, quantitatively explain the behavior of DMDBTDMA in n-dodecane in terms of scattering as well as phase stability limits

  20. Remediation in clay using two-phase vacuum extraction

    International Nuclear Information System (INIS)

    Lindhult, E.C.; Tarsavage, J.M.; Foukaris, K.A.

    1995-01-01

    Soil and groundwater contamination in a tight clay usually requires costly and/or time consuming remediation, due to the inherently low hydraulic conductivity of the soil. However, Dames and Moore is successfully using an innovative, cost-effective two-phase vacuum extraction (VE) technology at a former gasoline service station. Dramatic decreases in BTEX concentrations in onsite and downgradient monitoring wells are apparent

  1. Chromatography, solid-phase extraction, and capillary electrochromatography with MIPs.

    Science.gov (United States)

    Tóth, Blanka; Horvai, George

    2012-01-01

    Most analytical applications of molecularly imprinted polymers are based on their selective adsorption properties towards the template or its analogs. In chromatography, solid phase extraction and electrochromatography this adsorption is a dynamic process. The dynamic process combined with the nonlinear adsorption isotherm of the polymers and other factors results in complications which have limited the success of imprinted polymers. This chapter explains these problems and shows many examples of successful applications overcoming or avoiding the problems.

  2. Methods of analysis by the U.S. Geological Survey Organic Geochemistry Research Group : determination of triazine and phenylurea herbicides and their degradation products in water using solid-phase extraction and liquid chromatography/mass spectrometry

    Science.gov (United States)

    Lee, Edward Alan; Strahan, Alex P.; Thurman, Earl Michael

    2002-01-01

    An analytical method for the determination of 7 triazine and phenylurea herbicides and 12 of their degradation products in natural water samples using solid-phase extraction and liquid chromatography/mass spectrometry is presented in this report. Special consideration was given during the development of the method to prevent the formation of degradation products during the analysis. Filtered water samples were analyzed using 0.5 gram graphitized carbon as the solid-phase extraction media followed by liquid chromatography/mass spectrometry. Three different water-sample matrices?ground-water, surface-water, and reagent-water samples?spiked at 0.2 and 2.0 micrograms per liter were analyzed. Method detection limits ranged from 0.013 to 0.168 microgram per liter for the parent triazine herbicides and the triazine degradation products. Method detection limits ranged from 0.042 to 0.141 microgram per liter for the parent phenylurea herbicides and their degradation products. Mean recoveries for the triazine compounds in the ground- and surface-water samples generally ranged from 72.6 to 117.5 percent, but deethyl-cyanazine amide was recovered at 140.5 percent. Mean recoveries from the ground- and surface-water samples for the phenylurea compounds spiked at the 2.0-micrograms-per-liter level ranged from 82.1 to 114.4 percent. The mean recoveries for the phenylureas spiked at 0.2-microgram per liter were less consistent, ranging from 87.0 to 136.0 percent. Mean recoveries from reagent-water samples ranged from 87.0 to 109.5 percent for all compounds. The triazine compounds and their degradation products are reported in concentrations ranging from 0.05 to 2.0 micrograms per liter, with the exception of deethylcyanazine and deethylcyanazine amide which are reported at 0.20 to 2.0 micrograms per liter. The phenylurea compounds and their degradation products are reported in concentrations ranging from 0.20 to 2.0 micrograms per liter. The upper concentration limit was 2

  3. Determination of persistent organic pollutants in solid environmental samples using accelerated solvent extraction and supercritical fluid extraction. Exhaustive extraction and sorption/desorption studies of PCBs

    Energy Technology Data Exchange (ETDEWEB)

    Bjoerklund, E.

    1998-10-01

    Human activity is constantly causing environmental problems due to production and release of numerous chemicals. A group of compounds of special concern is persistent organic pollutants (POP). These toxic, lipophilic chemicals have a high chemical and biological stability, and tend to accumulate in the lipid phase of living organisms. A major sink for POPs are sediments, and consequently these are important for the distribution of POPs in the aquatic environment. Traditionally, determination of POPs relay on exhaustive extraction using liquid extraction techniques (e.g. Soxhlet extraction developed in the late 19th century) followed by gas chromatographic analysis. Since liquid-solid extraction normally requires large volumes of organic solvents in combination with long extraction times and extract clean-up, there has been an increasing demand for improved technology. This should result in reduced organic solvent consumption and sample preparation time, at the same time improving the environment and cutting costs for POP monitoring. In this thesis two modern techniques with capability of fulfilling at least one of these goals have been investigated: (1) Supercritical Fluid Extraction (SFE), and (2) Accelerated Solvent Extraction (ASE). Polychlorinated biphenyls (PCBs) were chosen as model compounds in all experiments performed on environmental matrices, since they cover a relatively large range of physiochemical parameters. Important parameters influencing the overall extraction efficiency in ASE and SFE, are discussed and illustrated for a large number of sediments. It was demonstrated that, by careful consideration of the experimental parameters, both techniques are capable of replacing old methods such as Soxhlet extraction. ASE is somewhat faster than SFE, but the extracts generated in SFE are much cleaner and can be analyzed without sample clean-up. Consequently the overall sample preparation time may be substantially lower using SFE. However, ASE is important

  4. [Corrected Title: Solid-Phase Extraction of Polar Compounds from Water] Automated Electrostatics Environmental Chamber

    Science.gov (United States)

    Sauer, Richard; Rutz, Jeffrey; Schultz, John

    2005-01-01

    A solid-phase extraction (SPE) process has been developed for removing alcohols, carboxylic acids, aldehydes, ketones, amines, and other polar organic compounds from water. This process can be either a subprocess of a water-reclamation process or a means of extracting organic compounds from water samples for gas-chromatographic analysis. This SPE process is an attractive alternative to an Environmental Protection Administration liquid-liquid extraction process that generates some pollution and does not work in a microgravitational environment. In this SPE process, one forces a water sample through a resin bed by use of positive pressure on the upstream side and/or suction on the downstream side, thereby causing organic compounds from the water to be adsorbed onto the resin. If gas-chromatographic analysis is to be done, the resin is dried by use of a suitable gas, then the adsorbed compounds are extracted from the resin by use of a solvent. Unlike the liquid-liquid process, the SPE process works in both microgravity and Earth gravity. In comparison with the liquid-liquid process, the SPE process is more efficient, extracts a wider range of organic compounds, generates less pollution, and costs less.

  5. Impact of solvent extraction organics on bioleaching by Acidithiobacillus ferrooxidans

    Science.gov (United States)

    Yu, Hualong; Liu, Xiaorong; Shen, Junhui; Chi, Daojie

    2017-03-01

    Solvent extraction organics (SX organics) entrained and dissoluted in the raffinate during copper SX operation, can impact bioleaching in case of raffinate recycling. The influence of SX organics on bioleaching process by Acidithiobacillus ferrooxidans (At. ferrooxidans) has been investigated. The results showed that, cells of At. ferrooxidans grew slower with contaminated low-grade chalcopyrite ores in shaken flasks bioleaching, the copper bioleaching efficiency reached 15%, lower than that of 24% for uncontaminated minerals. Obviously, the SX organics could adsorb on mineral surface and hinder its contact with bacterials, finanlly lead to the low bioleaching efficiency.

  6. New Approaches in Soil Organic Matter Fluorescence; A Solid Phase Fluorescence Approach

    Science.gov (United States)

    Bowman, M. M.; Sanclements, M.; McKnight, D. M.

    2017-12-01

    Fluorescence spectroscopy is a well-established technique to investigate the composition of organic matter in aquatic systems and is increasingly applied to soil organic matter (SOM). Current methods require that SOM be extracted into a liquid prior to analysis by fluorescence spectroscopy. Soil extractions introduce an additional layer of complexity as the composition of the organic matter dissolved into solution varies based upon the selected extractant. Water is one of the most commonly used extractant, but only extracts the water-soluble fraction of the SOM with the insoluble soil organic matter fluorescence remaining in the soil matrix. We propose the use of solid phase fluorescence on whole soils as a potential tool to look at the composition of organic matter without the extraction bias and gain a more complete understand of the potential for fluorescence as a tool in terrestrial studies. To date, the limited applications of solid phase fluorescence have ranged from food and agriculture to pharmaceutical with no clearly defined methods and limitations available. We are aware of no other studies that use solid phase fluorescence and thus no clear methods to look at SOM across a diverse set of soil types and ecosystems. With this new approach to fluorescence spectroscopy there are new challenges, such as blank correction, inner filter effect corrections, and sample preparation. This work outlines a novel method for analyzing soil organic matter using solid phase fluorescence across a wide range of soils collected from the National Ecological Observatory Network (NEON) eco-domains. This method has shown that organic matter content in soils must be diluted to 2% to reduce backscattering and oversaturation of the detector in forested soils. In mineral horizons (A) there is observed quenching of the humic-like organic matter, which is likely a result of organo-mineral complexation. Finally, we present preliminary comparisons between solid and liquid phase

  7. Evaluation of a novel metal-organic framework as an adsorbent for the extraction of multiclass pesticides from coconut palm (Cocos nucifera L.): An analytical approach using matrix solid-phase dispersion and liquid chromatography.

    Science.gov (United States)

    de Jesus, Jemmyson Romário; Wanderley, Kaline Amaral; Alves Júnior, Severino; Navickiene, Sandro

    2017-08-01

    We report the synthesis, characterization, and application of [Zn(1,4-benzenedicarboxylate)(H 2 O) 2 ] n , Zn(1,4-benzenedicarboxylate) 0.99 (NH 2 -1,4-benzenedicarboxylate) 0.01 (H 2 O) 2 ] n , [Zn(1,4-benzenedicarboxylate) 0.95 (NH 2 -1,4-benzenedicarboxylate) 0.05 (H 2 O) 2 ] n , and [Zn(1,4-benzenedicarboxylate) 0.9 (NH 2 -1,4-benzenedicarboxylate) 0.1 (H 2 O) 2 ] n as sorbents for the extraction of multiclass pesticides from coconut palm. Liquid chromatography with ultraviolet diode array detection was used as the analysis technique, and the experiments were performed at one fortification level (0.1 μg/g). The recoveries were 47-67, 51-70, 58-72, and 64-76% for [Zn(1,4-benzenedicarboxylate)(H 2 O) 2 ] n , Zn(1,4-benzenedicarboxylate) 0.99 (NH 2 -1,4-benzenedicarboxylate) 0.01 (H 2 O) 2 ] n , [Zn(1,4-benzenedicarboxylate) 0.95 (NH 2 -1,4-benzenedicarboxylate) 0.05 (H 2 O) 2 ] n , and [Zn(1,4-benzenelate) 0.95 (NH 2 -1,4-benzenedicarboxylate) 0.05 (H 2 O) 2 ] n , and [Zn(1,4-benzenedicarboxylate) 0.9 (NH 2 -1,4-benzenedicarboxylate) 0.1 (H 2 O) 2 ] n , respectively, with relative standard deviation ranging from 1 to 7% (n = 3). Detection and quantification limits were 0.01-0.05 and 0.05-0.2 μg/g, respectively, for the different pesticides studied. The method developed was linear over the range tested (0.01-10.0 μg/g) with r 2  > 0.9991. A direct comparison of [Zn(1,4-benzenedicarboxylate) 0.9 (NH 2 -1,4-benzenedicarboxylate) 0.1 (H 2 O) 2 ] n with the commercially available neutral alumina showed that [Zn(1,4-benzenedicarboxylate) 0.9 (NH 2 -1,4-benzenedicarboxylate) 0.1 (H 2 O) 2 ] n was a similar extracting phase for the pesticides investigated. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Aqueous Two-Phase Extraction of Polyphenols Using a Microchannel System – Process Optimization and Intensification

    Directory of Open Access Journals (Sweden)

    Ivana Rukavina

    2011-01-01

    Full Text Available Polyphenols are one of the most numerous and widespread groups of compounds in the plant world. Nowadays, organic solvents such as methanol, ethanol, acetone, dimethylformamide, ethyl acetate and diethylether are mainly used for the extraction of polyphenols. These solvents require special process conditions and special care in the disposal of the used solvents. In this paper, the extraction of polyphenols from the model solution was performed using the aqueous two-phase system which contains 80.90 % water and represents low burden on the environment. The aqueous solution of gallic acid (GA was used as a model solution of polyphenols. The extraction was performed in the aqueous two-phase system containing PEG6000/H2O/(NH42SO4 in a macroextractor (V=10 mL and microextractor (V=14 ƒμL. The influence of the process parameters, the concentration of gallic acid, pH and composition of the aqueous two-phase system was investigated in order to maximize the partition coefficient. The method of multifactor experimental planning was used to optimize the extraction process and the results were statistically analysed using the evolutionary operation method (EVOP. Optimal operating conditions of the extraction process were pH=6.50, γGA=4.50 g/L, the mass fraction of polyethylene glycol (PEG wPEG=0.1037 g/g and the mass fraction of ammonium sulphate (AMS wAMS=0.0925 g/g. Under these conditions the maximal partition coefficient of K=5.54 and the extraction efficiency of E=89.11 % were achieved and successfully applied for total phenol extraction from white wine in the macro- and microextractor. Approximately the same partition coefficients and extraction efficiency were achieved in the microextractor within a 60-fold shorter residence time.

  9. Experimental and molecular docking investigation on metal-organic framework MIL-101(Cr) as a sorbent for vortex assisted dispersive micro-solid-phase extraction of trace 5-nitroimidazole residues in environmental water samples prior to UPLC-MS/MS analysis.

    Science.gov (United States)

    Lu, Nan; Wang, Ting; Zhao, Pan; Zhang, Lianjun; Lun, Xiaowen; Zhang, Xueli; Hou, Xiaohong

    2016-11-01

    In the presented work, metal-organic framework (MOF) material MIL-101(Cr) (MIL, Matérial Institute Lavoisier) was used as a sorbent for vortex assisted dispersive micro-solid-phase extraction (VA-D-μ-SPE) of trace amount of metronidazole (MNZ), ronidazole (RNZ), secnidazole (SNZ), dimetridazole (DMZ), tinidazole (TNZ), and ornidazole (ONZ) in different environmental water samples. Ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) was used to quantify the target analytes. The extraction conditions, including type of sorbents, amount of MIL-101(Cr), solution pH, extraction method, extraction time, effect of salt, and elution conditions were investigated. Upon the optimal conditions, the developed method showed an excellent extraction performance with the average recovery ranging from 75.2 to 98.8 %. Good sensitivity levels were achieved with the detection limits of 0.03∼0.06 μg/L and the quantitation limits of 0.09∼0.20 μg/L. The linear ranges were varied from 0.1 to 20 for SNZ and ONZ and from 0.2 to 40 μg/L for MNZ, RNZ, DMZ, and TNZ (r 2  > 0.992), and repeatability of the method was satisfactory with the relative standard deviations (RSD) extraction and determination of 5-nitroimidazoles (5-NDZs) in 12 real water samples, showing the positive findings of MNZ and TNZ ranging from 0.3 to 1.0 μg/L. Furthermore, molecular docking was applied to explain the molecular interactions and free binding energies between MIL-101(Cr) and 5-NDZs, providing a deep insight into the adsorption mechanism. The proposed method exhibited the advantages of simplicity, rapidly, less solvent consumption, ease of operation, higher sensitivity, and lower matrix effect. Graphical abstract Schematic diagram of the extraction process and molecular docking investigation.

  10. Antifeedant Activty Of Different Organic Solvent Crude Extracts Of ...

    African Journals Online (AJOL)

    The antifeedant activity of different organic solvents (acetone, carbon tetrachloride, chloroform, diethyl ether and ethyl alcohol) crude extracts of latex of Euphorbia hirta (family Euphobiaceae) against Limicolaria aurora was investigated, and compared with a control, using pawpaw, (Carica papaya) as bait, at a concentration ...

  11. Hot atom chemistry of monovalent atoms in organic condensed phases

    International Nuclear Information System (INIS)

    Stoecklin, G.

    1975-01-01

    The advantages and disadvantages of hot atom studies in condensed organic phases are considered, and recent advances in condensed phase organic hot atom chemistry of recoil tritium and halogen atoms are discussed. Details are presented of the present status and understanding of liquid phase hot atom chemistry and also that of organic solids. The consequences of the Auger effect in condensed organic systems are also considered. (author)

  12. Determination of silver in soils, sediments, and rocks by organic-chelate extraction and atomic absorption spectrophotometry

    Science.gov (United States)

    Chao, T.T.; Ball, J.W.; Nakagawa, H.M.

    1971-01-01

    A useful method for the determination of silver in soil, sediment, and rock samples in geochemical exploration has been developed. The sample is digested with concentrated nitric acid, and the silver extracted with triisooctyl thiophosphate (TOTP) in methyl isobutyl ketone (MIBK) after dilution of the acid digest to approximately 6 M. The extraction of silver into the organic extractant is quantitative and not affected by the nitric acid concentration from 4 M to 8 M, or by different volumes of TOTP-MIBK. The extracted silver is stable and remains in the organic phase up to several days. The silver concentration is determined by atomic absorption spectrophotometry. ?? 1971.

  13. Phase Grouping Line Extraction Algorithm Using Overlapped Partition

    Directory of Open Access Journals (Sweden)

    WANG Jingxue

    2015-07-01

    Full Text Available Aiming at solving the problem of fracture at the discontinuities area and the challenges of line fitting in each partition, an innovative line extraction algorithm is proposed based on phase grouping using overlapped partition. The proposed algorithm adopted dual partition steps, which will generate overlapped eight partitions. Between the two steps, the middle axis in the first step coincides with the border lines in the other step. Firstly, the connected edge points that share the same phase gradients are merged into the line candidates, and fitted into line segments. Then to remedy the break lines at the border areas, the break segments in the second partition steps are refitted. The proposed algorithm is robust and does not need any parameter tuning. Experiments with various datasets have confirmed that the method is not only capable of handling the linear features, but also powerful enough in handling the curve features.

  14. 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.

  15. Solid phase extraction for the speciation and preconcentration of inorganic selenium in water samples: a review.

    Science.gov (United States)

    Herrero Latorre, C; Barciela García, J; García Martín, S; Peña Crecente, R M

    2013-12-04

    Selenium is an essential element for the normal cellular function of living organisms. However, selenium is toxic at concentrations of only three to five times higher than the essential concentration. The inorganic forms (mainly selenite and selenate) present in environmental water generally exhibit higher toxicity (up to 40 times) than organic forms. Therefore, the determination of low levels of different inorganic selenium species in water is an analytical challenge. Solid-phase extraction has been used as a separation and/or preconcentration technique prior to the determination of selenium species due to the need for accurate measurements for Se species in water at extremely low levels. The present paper provides a critical review of the published methods for inorganic selenium speciation in water samples using solid phase extraction as a preconcentration procedure. On the basis of more than 75 references, the different speciation strategies used for this task have been highlighted and classified. The solid-phase extraction sorbents and the performance and analytical characteristics of the developed methods for Se speciation are also discussed. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Optimization of Solid Phase Micro-Extraction (SPME for Monitoring Occupational Exposure to Ethyl Benzene

    Directory of Open Access Journals (Sweden)

    H. Heidari

    2009-08-01

    Full Text Available AbstractBackground and Objectives: Analytical methods for volatile organic compounds (VOCs in different samples need extraction of compounds, by applying hazardous solvents. Solid phase micro-extraction (SPME is a solvent-free equilibrium extraction method, in which proper calibration can allow quantitative determinations of VOCs at a very good sensitivity without the use of any organic solvent. VOCs are generally present in urine only at trace levels, therefore, a sensitive procedure is needed for their trace determinations. Throughout this study, headspace solid phase micro-extraction (HS-SPME was followed by GC-FID for ethyl benzene in spiked urine was optimized.Methods: In this study, the parameters influencing SPME and gas chromatography of ethyl benzene, including extraction time, temperature, desorption temperature, desorption time, salt addition, sample pH, sample volume and sample agitation were investigated. Results: Extraction procedure was performed at 30°C for 6 min, using 0.2 gml-1 of NaCl in the sample solution. The sample volume and sample pH were optimized at 5 ml and 7 (neutral pH, respectively. Desorption of the ethyl benzene was carried out for 60 sec. at 250°C. The method was also validated with three different spiked urine samples and illustrated an appropriate reproducibility over six consecutive days as well as six within-day experiments. During this investigation, parameters of accuracy, linearity, and detection limits of the procedure were also evaluated.Conclusion: The developed method of HS- SPME-GC-FID proved to be a simple, convenient, and practical procedure, and was successfully used for measuring of ethyl benzene in spiked urine.

  17. A novel hybrid metal-organic framework-polymeric monolith for solid-phase microextraction.

    Science.gov (United States)

    Lin, Chen-Lan; Lirio, Stephen; Chen, Ya-Ting; Lin, Chia-Her; Huang, Hsi-Ya

    2014-03-17

    This study describes the fabrication of a novel hybrid metal-organic framework- organic polymer (MOF-polymer) for use as a stationary phase in fritless solid-phase microextraction (SPME) for validating analytical methods. The MOF-polymer was prepared by using ethylene dimethacrylate (EDMA), butyl methacrylate (BMA), and an imidazolium-based ionic liquid as porogenic solvent followed by microwave-assisted polymerization with the addition of 25 % MOF. This novel hybrid MOF-polymer was used to extract penicillin (penicillin G, penicillin V, oxacillin, cloxacillin, nafcillin, dicloxacillin) under different conditions. Quantitative analysis of the extracted penicillin samples using the MOF-organic polymer for SPME was conducted by using capillary electrochromatography (CEC) coupled with UV analysis. The penicillin recovery was 63-96.2 % with high reproducibility, sensitivity, and reusability. The extraction time with the proposed fabricated SPME was only 34 min. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Automated solid-phase extraction of phenolic acids using layered double hydroxide-alumina-polymer disks.

    Science.gov (United States)

    Ghani, Milad; Palomino Cabello, Carlos; Saraji, Mohammad; Manuel Estela, Jose; Cerdà, Víctor; Turnes Palomino, Gemma; Maya, Fernando

    2018-01-26

    The application of layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks for solid-phase extraction is reported for the first time. Al 2 O 3 is embedded in a polymer matrix followed by an in situ metal-exchange process to obtain a layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disk with excellent flow-through properties. The extraction performance of the prepared disks is evaluated as a proof of concept for the automated extraction using sequential injection analysis of organic acids (p-hydroxybenzoic acid, 3,4-dihydroxybenzoic acid, gallic acid) following an anion-exchange mechanism. After the solid-phase extraction, phenolic acids were quantified by reversed-phase high-performance liquid chromatography with diode-array detection using a core-shell silica-C18 stationary phase and isocratic elution (acetonitrile/0.5% acetic acid in pure water, 5:95, v/v). High sensitivity and reproducibility were obtained with limits of detection in the range of 0.12-0.25 μg/L (sample volume, 4 mL), and relative standard deviations between 2.9 and 3.4% (10 μg/L, n = 6). Enrichment factors of 34-39 were obtained. Layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks had an average lifetime of 50 extractions. Analyte recoveries ranged from 93 to 96% for grape juice and nonalcoholic beer samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. A combination of computational-experimental study on metal-organic frameworks MIL-53(Al) as sorbent for simultaneous determination of estrogens and glucocorticoids in water and urine samples by dispersive micro-solid-phase extraction coupled to UPLC-MS/MS.

    Science.gov (United States)

    Gao, Guihua; Li, Sijia; Li, Shuo; Wang, Yudan; Zhao, Pan; Zhang, Xiangyu; Hou, Xiaohong

    2018-04-01

    In this work, computational and experimental methods were used to study the adsorption of estrogens and glucocorticoids on metal-organic frameworks (MOFs). Computer-aided molecular simulation was applied to predict the adsorption of eight analytes on four MOFs (MIL-101(Cr), MIL-100(Fe), MIL-53(Al), and UiO-66(Zr)) by examining molecular interactions and calculating free binding energies. Subsequently, the four water-stable MOFs were synthesized and evaluated as adsorbents for the target hormones in aqueous solution. As the MOF exhibiting the highest adsorption capacity in both computations and experiments, MIL-53(Al) was chosen as a sorbent to develop a dispersive micro-solid-phase extraction procedure coupled to ultra-performance liquid chromatography tandem mass spectrometry for simultaneous determination of the target analytes in water and human urine samples. Experimental parameters affecting the extraction recoveries, including pH, ionic strength, MIL-53(Al) amount, extraction time, desorption time, and desorption solvent, were optimized. The optimized method provided a linear range of 0.005025-368.6μg/L with good correlation coefficients (0.9982 ≤ r 2 ≤ 0.9992), and limits of detection (S/N = 3) and quantification (S/N = 10) of 0.0015-1.0μg/L and 0.005-1.8μg/L, respectively. The analyte recoveries were in the range of 80.6-98.4% in water samples and 88.4-93.2% in urine samples. Furthermore, MIL-53(Al) showed good stability over 10 extraction cycles (RSD extraction efficiencies for MOFs and targets, providing new directions for the development and utilization of MOFs. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Evaluate the Influence of Eupatorium adenophorum Extract with Mice Organ

    Science.gov (United States)

    Nong, Xiang; Yang, Can; Yang, Yaojun; Liang, Zi; Hu, Qiang; Zhang, Ting

    2018-01-01

    In order to study the influence of extract from Eupatorium adenophorum in mice organs, this experiment will be the basis of further study that make Eupatorium adenophorum become Phyto contraceptive, this experiment take the feeding respectively way after the completion of the 1D, 5D, 10d, 15d of Eupatorium adenophorum mice by intragastrical administration of levonorgestrel group and blank control group. After the same operation in different periods of small rat heart and kidney the uterus, testis, and other organs were observed. The results showed that after extraction of E. adenophorum changes in female mice uterus shape was perfused significantly, showed swelling larger. Data analysis of each viscera coefficient was found E. adenophorum had No obvious effect on the heart, kidneys and testicles of mice. but there are obvious differences date between the treatment group and the blank group. (5d: F=10. 800 P=0. 043 cases) from tissue sections we can see female mice uterus cell morphology changes significantly, there was a similar appearance change in the uterus of the female mice with the estradiol For a male mouse testis of E.adenophorum gavage had No obvious effect. And it is found that the heart, the treated mice kidney, testis, ovary and other organs were observed in each period of time the organization had No obvious change; only female mice uterus tissue sections of individual cells became larger, and the organization of the gap larger. This research shows that E.adenophorum extract has the potential to develop botanical contraceptives, we will conduct in-depth study.

  1. Subcritical-Water Extraction of Organics from Solid Matrices

    Science.gov (United States)

    Amashukeli, Xenia; Grunthaner, Frank; Patrick, Steven; Kirby, James; Bickler, Donald; Willis, Peter; Pelletier, Christine; Bryson, Charles

    2009-01-01

    An apparatus for extracting organic compounds from soils, sands, and other solid matrix materials utilizes water at subcritical temperature and pressure as a solvent. The apparatus, called subcritical water extractor (SCWE), is a prototype of subsystems of future instrumentation systems to be used in searching for organic compounds as signs of past or present life on Mars. An aqueous solution generated by an apparatus like this one can be analyzed by any of a variety of established chromatographic or spectroscopic means to detect the dissolved organic compound( s). The apparatus can be used on Earth: indeed, in proof-of-concept experiments, SCWE was used to extract amino acids from soils of the Atacama Desert (Chile), which was chosen because the dryness and other relevant soil conditions there approximate those on Mars. The design of the apparatus is based partly on the fact that the relative permittivity (also known as the dielectric constant) of liquid water varies with temperature and pressure. At a temperature of 30 C and a pressure of 0.1 MPa, the relative permittivity of water is 79.6, due to the strong dipole-dipole electrostatic interactions between individual molecular dipoles. As the temperature increases, increasing thermal energy causes increasing disorientation of molecular dipoles, with a consequent decrease in relative permittivity. For example, water at a temperature of 325 C and pressure of 20 MPa has a relative permittivity of 17.5, which is similar to the relative permittivities of such nonpolar organic solvents as 1-butanol (17.8). In the operation of this apparatus, the temperature and pressure of water are adjusted so that the water can be used in place of commonly used organic solvents to extract compounds that have dissimilar physical and chemical properties.

  2. Fifty years of solid-phase extraction in water analysis--historical development and overview.

    Science.gov (United States)

    Liska, I

    2000-07-14

    The use of an appropriate sample handling technique is a must in an analysis of organic micropollutants in water. The efforts to use a solid phase for the recovery of analytes from a water matrix prior to their detection have a long history. Since the first experimental trials using activated carbon filters that were performed 50 years ago, solid-phase extraction (SPE) has become an established sample preparation technique. The initial experimental applications of SPE resulted in widespread use of this technique in current water analysis and also to adoption of SPE into standardized analytical methods. During the decades of its evolution, chromatographers became aware of the advantages of SPE and, despite many innovations that appeared in the last decade, new SPE developments are still expected in the future. A brief overview of 50 years of the history of the use of SPE in organic trace analysis of water is given in presented paper.

  3. Phase extraction based on iterative algorithm using five-frame crossed fringes in phase measuring deflectometry

    Science.gov (United States)

    Jin, Chengying; Li, Dahai; Kewei, E.; Li, Mengyang; Chen, Pengyu; Wang, Ruiyang; Xiong, Zhao

    2018-06-01

    In phase measuring deflectometry, two orthogonal sinusoidal fringe patterns are separately projected on the test surface and the distorted fringes reflected by the surface are recorded, each with a sequential phase shift. Then the two components of the local surface gradients are obtained by triangulation. It usually involves some complicated and time-consuming procedures (fringe projection in the orthogonal directions). In addition, the digital light devices (e.g. LCD screen and CCD camera) are not error free. There are quantization errors for each pixel of both LCD and CCD. Therefore, to avoid the complex process and improve the reliability of the phase distribution, a phase extraction algorithm with five-frame crossed fringes is presented in this paper. It is based on a least-squares iterative process. Using the proposed algorithm, phase distributions and phase shift amounts in two orthogonal directions can be simultaneously and successfully determined through an iterative procedure. Both a numerical simulation and a preliminary experiment are conducted to verify the validity and performance of this algorithm. Experimental results obtained by our method are shown, and comparisons between our experimental results and those obtained by the traditional 16-step phase-shifting algorithm and between our experimental results and those measured by the Fizeau interferometer are made.

  4. Elucidation of the structure of organic solutions in solvent extraction by combining molecular dynamics and X-ray scattering

    International Nuclear Information System (INIS)

    Ferru, G.; Gomes Rodrigues, D.; Berthon, L.; Guilbaud, P.; Diat, O.; Bauduin, P.

    2014-01-01

    Knowledge of the supramolecular structure of the organic phase containing amphiphilic ligand molecules is mandatory for full comprehension of ionic separation during solvent extraction. Existing structural models are based on simple geometric aggregates, but no consensus exists on the interaction potentials. Herein, we show that molecular dynamics crossed with scattering techniques offers key insight into the complex fluid involving weak interactions without any long range ordering. Two systems containing mono- or diamide extractants in heptane and contacted with an aqueous phase were selected as examples to demonstrate the advantages of coupling the two approaches for furthering fundamental studies on solvent extraction. (authors)

  5. Organic Contaminants Associated with the Extraction of Unconventional Gas. Risk Analysis in the Initial Phases of the Project; Contaminantes Orgánicos Asociados a la Extracción de Gas no Convencional. Análisis de Riesgos en las Fases Iniciales del Proyecto

    Energy Technology Data Exchange (ETDEWEB)

    Xu, L.; Hurtado, A.; Recreo, F.; Eguilior, S.

    2015-07-01

    The latest technological advances in hydraulic fracturing and horizontal drilling are promoting a commercial scale extraction of unconventional fossil fuels in several regions of the world. Although there is still no commercial scale extraction in the Member States of the EU, potential stocks in some of them, as in the case of Spain, stimulate the need to carry out precautionary previous studies. These, based on the experience in the USA, will allow to define the characteristics that a priori should include a project of unconventional gas extraction, so that their safety is maximized by minimizing the likelihood of adverse effects on the environment. In unconventional gas production a fracturing fluid, typically water, with different types of additives is injected into the reservoir at very high pressure in order to create fractures to increase the porosity and permeability of the rock. In this scenario the flowback and produced water (water brought to the surface during the extraction of gas or oil) is usually a mixture of fluids injected and brines present in the repository. The quality of the flowback and produced water is variable. Its salinity varies from similar to drinking water to several times more saline than seawater. Furthermore, different compounds other than salt can be present in various amounts in the flowback and produced water: oil and other organic compounds, solids in suspension, bacteria, naturally occurring radioactive elements (NORM), and any of the elements injected with the hydraulic fracturing fluid. Due to the high variability of contaminants in the flowback and produced water as well as potentially large volumes involved, composition of flowback and produced water and the analysis of the risks associated with them is an important aspect to consider from the initial phases of project development of unconventional gas extraction. This report covers the risk analysis of an unconventional gas extraction project, the initial assessment of the

  6. Estimation of visibility of phase contrast with extraction voltages for field emission gun electron microscopes

    Energy Technology Data Exchange (ETDEWEB)

    Meng, Xing, E-mail: xmeng101@gmail.com

    2017-02-15

    Estimation was made for visibility of phase contrast with varying extraction voltages. The resulting decay rates of visibility show that images with low image contrast from cryo EM will be seriously impacted with high extraction voltages. - Highlights: • Cryo EM • Phase contrast • Extraction votage.

  7. Determination of phenols in landfill leachate-contaminated groundwaters by solid-phase extraction

    DEFF Research Database (Denmark)

    Ask Reitzel, Lotte; Ledin, Anna

    2002-01-01

    A solid-phase extraction method for phenols in landfill leachates was developed and optimized in order to solve the expected and observed problems associated with an anaerobic matrix containing high concentrations of salts and organic matter. Isolute ENV1 cartridges exhibited the best retention...... be identified in leachates from three Danish landfills, ranging in concentration from 0.01 to 29 mg/ L, which is at the lower end of the concentration range usually found for phenols in landfill leachates (sub-mg/L to mg/L).  2002 Elsevier Science B.V. All rights reserved....

  8. Third phase formation in the extraction of Th(NO{sub 3}){sub 4} by Tri-sec-butyl phosphate. A comparison with Tri-n-butyl phosphate

    Energy Technology Data Exchange (ETDEWEB)

    Chandrasekar, Aditi; Suresh, A.; Sivaraman, N. [Indira Gandhi Centre for Atomic Research, Kalpakkam (India). Chemistry Group

    2017-06-01

    Earlier studies carried out in our laboratory indicated that Tri-sec-butyl phosphate (TsBP) is a potential extractant for U/Th separation. Also, the third phase formation tendency of TsBP is lower compared to its isomers, Tri-n-butyl-phosphate (TBP) and Tri-iso-butyl phosphate (TiBP). In this context, the extraction and third phase formation behaviour of 1.1 M solutions of TiBP and TsBP in n-dodecane in the extraction of Th(IV) from 1 M HNO{sub 3} at 303 K over a wide range of Th concentrations were investigated in the present study and the results are compared with the literature data on TBP system. Concentrations of Th(IV) and HNO{sub 3} loaded in the organic phase before third phase formation (biphasic region) as well as in third phase and diluent-rich phase after third phase formation (triphasic region) were measured as a function of equilibrium aqueous phase Th(IV) concentration. The density of loaded organic phase was also measured at various Th(IV) concentrations. The extraction profiles in the biphasic region indicated that extraction of Th(IV) by TBP is higher than that of TiBP which in turn is higher than that of TsBP. Extractant concentration in the diluent-rich phase and third phase was measured for the triphasic region.

  9. Third phase formation in the extraction of Th(NO_3)_4 by Tri-sec-butyl phosphate. A comparison with Tri-n-butyl phosphate

    International Nuclear Information System (INIS)

    Chandrasekar, Aditi; Suresh, A.; Sivaraman, N.

    2017-01-01

    Earlier studies carried out in our laboratory indicated that Tri-sec-butyl phosphate (TsBP) is a potential extractant for U/Th separation. Also, the third phase formation tendency of TsBP is lower compared to its isomers, Tri-n-butyl-phosphate (TBP) and Tri-iso-butyl phosphate (TiBP). In this context, the extraction and third phase formation behaviour of 1.1 M solutions of TiBP and TsBP in n-dodecane in the extraction of Th(IV) from 1 M HNO_3 at 303 K over a wide range of Th concentrations were investigated in the present study and the results are compared with the literature data on TBP system. Concentrations of Th(IV) and HNO_3 loaded in the organic phase before third phase formation (biphasic region) as well as in third phase and diluent-rich phase after third phase formation (triphasic region) were measured as a function of equilibrium aqueous phase Th(IV) concentration. The density of loaded organic phase was also measured at various Th(IV) concentrations. The extraction profiles in the biphasic region indicated that extraction of Th(IV) by TBP is higher than that of TiBP which in turn is higher than that of TsBP. Extractant concentration in the diluent-rich phase and third phase was measured for the triphasic region.

  10. Reversed phase column extraction studies to recovery of uranium using a modified perlite

    International Nuclear Information System (INIS)

    Akcay, H.

    2006-01-01

    Reversed phase column (RPC) extraction chromatography is an useful technique and has been carried out successfully to the separation of various metals and organic compounds. Its application has received considerable attention because it combines the selectivity of LLE with the advantage of chromatography. The efficiency of the separation by RPC depends on both the chemical and physical properties of the solid support and the stationary phase. This work describes the preparation of an improved adsorbent from natural perlite and its properties to uptake of uranyl ion. Perlite is a volcanic glassy rock produced in commercially workable quantities from mines of Aegean region of Turkey and contains 70-75% CO 2 .The CO 2 was converted to soluble silicates with NaOH modification then its acidification to form hydrogen which turned into xerogels upon drying. Fundamental parameters (particle size, specific surface area, pore size and volume, surface hydroxyl group density) were determined for modified perlite and it was silanized then loaded with 20% (w/w) TBP before being used as reversed phase column chromatography solid support. Finally the sorption of UO 2 + 2 from aqueous solutions by the modified perlite was investigated using Batch techniques. The use of TBP-loaded perlite as a reversed phase column (RPC) extraction chromatography support seems to be useful to uptake of UO 2 + 2 from aqueous solutions and to separate from various cations

  11. Dissolved organic carbon enhances the mass transfer of hydrophobic organic compounds from Nonaqueous Phase Liquids (NAPLs) into the aqueous phase

    NARCIS (Netherlands)

    Smith, K.E.C.; Thullner, M.; Wick, L.Y.; Harms, H.

    2011-01-01

    The hypothesis that dissolved organic carbon (DOC) enhances the mass transfer of hydrophobic organic compounds from nonaqueous phase liquids (NAPLs) into the aqueous phase above that attributable to dissolved molecular diffusion alone was tested. In controlled experiments, mass transfer rates of

  12. 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...

  13. Solvent extraction of hafnium(IV) by dinonylnaphthalene sulfonic acid from mixed aqueous-organic media

    International Nuclear Information System (INIS)

    Hala, J.; Piperkovova, H.

    1979-01-01

    The extraction of hafnium(IV) by heptane and toluene solutions of dinonylnaphthalene sulfonic acid (HD) from mixed aqueous-organic solutions has been studied. Alcohols, ketones, carboxylic acids, cyclic ethers, dimethylsulfoxide and dimethylformamide were used as the organic component of the mixed phase. Methanol, ethanol, formic acid and dioxane increased the extractability of Hf(IV) whereas other solvents showed only an antagonistic effect. The results were discussed from the point of view of the changes in micellar structure of HD, and compared with the uptake of Hf(IV) by resinous cation exchangers. The solubilization by HD of alcohols, carboxylic acids and dimethylsulfoxide was demonstrated by using the corresponding 14 C and 35 S labelled compounds. (author)

  14. Amino-modified diamond as a durable stationary phase for solid-phase extraction.

    Science.gov (United States)

    Saini, Gaurav; Yang, Li; Lee, Milton L; Dadson, Andrew; Vail, Michael A; Linford, Matthew R

    2008-08-15

    We report the formation of a highly stable amino stationary phase on diamond and demonstrate its use in solid-phase extraction (SPE). This process consists of spontaneous and self-limiting adsorption of polyallylamine (PAAm) from aqueous solution onto oxidized diamond. Thermal curing under reduced pressure or chemical cross-linking with a diepoxide was shown to fix the polymer to the particles. The resulting adsorbents are stable under even extreme pH conditions (from at least pH 0-14) and significantly more stable than a commercially available amino SPE adsorbent. Coated diamond particles were characterized by X-ray photoelectron spectroscopy (XPS) and diffuse reflectance Fourier transform-infrared spectroscopy (DRIFT). Model silicon surfaces were characterized by spectroscopic ellipsometry and wetting. Solid-phase extraction was demonstrated using cholesterol, hexadecanedioic acid, and palmitoyloleoylphosphatidylcholine as analytes, and these results were compared to those obtained with commercially available materials. Breakthrough curves indicate that, as expected, porous diamond particles have higher analyte capacity than nonporous solid particles.

  15. Dysprosium separation from aqueous phase by non-dispersive solvent extraction employing hollow fibre membrane module

    International Nuclear Information System (INIS)

    Yadav, Kartikey K.; Singh, D.K.; Kain, V.

    2017-01-01

    Rare earth elements (REEs) consist of fourteen lanthanides and three elements which are Sc, Y and La resulting in total 17 REEs. In the last decade, these rare earths elements which have unique physical and chemical properties have been highly in demand for their application in almost all walks of life. Various methods such as ion exchange, precipitation and solvent extraction have been used to recover these elements from aqueous solutions. These traditional methods have some inherent disadvantages like handling of hazardous organic chemicals, ineffectiveness to recover a very low concentration of contaminated source etc. In this regard, an important method i.e. liquid membrane offers separation scheme; which combines the characteristics, of solvent extraction and solid membrane separation, to overcome the disadvantages of conventional techniques. Various experiments were carried out to evaluate the effect of feed acidity, metal ion concentration, carrier concentration, feed composition, flow rates and phase ratio on the transport of rare earths metal ions across the membrane

  16. Speciation analysis of mercury by dispersive solid-phase extraction coupled with capillary electrophoresis.

    Science.gov (United States)

    Li, Jinhua; Liu, Junying; Lu, Wenhui; Gao, Fangfang; Wang, Liyan; Ma, Jiping; Liu, Huitao; Liao, Chunyang; Chen, Lingxin

    2018-04-23

    A pretreatment method of dispersive solid-phase extraction (DSPE) along with back-extraction followed by CE-UV detector was developed for the determination of mercury species in water samples. Sulfhydryl-functionalized SiO 2 microspheres (SiO 2 -SH) were synthesized and used as DSPE adsorbents for selective extraction and enrichment of three organic mercury species namely ethylmercury (EtHg), methylmercury (MeHg), and phenylmercury (PhHg), along with L-cysteine (L-cys) containing hydrochloric acid as back-extraction solvent. Several main extraction parameters were systematically investigated including sample pH, amount of adsorbent, extraction and back-extraction time, volume of eluent, and concentration of hydrochloric acid. Under optimal conditions, good linearity was achieved with correlation coefficients over 0.9990, in the range of 4-200 μg/L for EtHg, and 2-200 μg/L for MeHg and PhHg. The LODs were obtained of 1.07, 0.34, and 0.24 μg/L for EtHg, MeHg, and PhHg, respectively, as well as the LOQs were 3.57, 1.13, and 0.79 μg/L, respectively, with enrichment factors ranging from 109 to 184. Recoveries were attained with tap and lake water samples in a range of 62.3-107.2%, with relative standard deviations of 3.5-10.1%. The results proved that the method of SiO 2 -SH based DSPE coupled with CE-UV was a simple, rapid, cost-effective, and eco-friendly alternative for the determination of mercury species in water samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Extraction of UO22+ by two highly sterically hindered (X1) (X2) PO(OH) extractants from an aqueous chloride phase

    International Nuclear Information System (INIS)

    Mason, G.W.; Lewey, S.M.; Gilles, D.M.; Peppard, D.F.

    1978-01-01

    The comparative extraction behaviour of tracer-level UO 2 2+ into benzene solutions of two highly sterically hindered extractants, di(2,6-di-iso-propylphenyl) phosphoric acid, HD(2,6-i-PPHI)P and di-tertiary-butyl phosphinic acid, H[Dt-BP], vs an aqueous 1.0 F (NaCl + HCl) phase was studied. The extraction of UO 2 2+ in both systems is directly second-power dependent upon extractant concentration and inversely second-power dependent upon hydrogen ion concentration, the stoichiometry of extraction being UOsub(2A) 2+ + 2(HY)sub(2O) = UO 2 (HY 2 )sub(2O) + 2Hsub(A) + . The expression for the distribution ratio, K is K = Ksub(s)F 2 /[H + ] 2 the general expression for the extraction of any metallic species being K - Ksub(s)Fsup(a)/[H + ]sup(b) where Ksub(s) is a constant characteristic of the system, F the concentration in formality units of extractant in the organic phase, [H + ] the concentration of hydrogen ion in the aqueous phase, and a and b the respective extractant and hydrogen-ion dependencies. Both extractants have a high degree of steric hindrance. The HD(2,6-i-PPHI)P is the more highly acidic, the pKsub(A) value, in 75% ethanol, being 3.2. The pKsub(A), previously reported, for H[Dt-BP] is 6.26. The Ksub(s) for UO 2 2+ in the system HY in benzene diluent vs an aqueous 1.0 F (NaCl + HCl) phase is 2 x 10 4 for H[Dt-BP] and 3 x 10 -1 for HD(2,6-i-PPHI)P; the ratio of the Ksub(s) values nearly 7 x 10 3 , favours the less acidic extractant. For comparative purposes, the Ksub(s) values for UO 2 2+ and for Am 3+ and Eu 3+ in other (X 1 )(X 2 )PO(OH), in benzene diluent, vs 1.0 F (NaCl + HCl) systems are presented. The variations are discussed in terms of the pKsub(A) of the extractant and the steric hindrance within the extractant. (author)

  18. Metal-organic aerogel as a coating for solid-phase microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Saraji, Mohammad, E-mail: saraji@cc.iut.ac.ir; Shahvar, Ali

    2017-06-22

    An iron-based metal-organic aerogel was synthesized using metal-organic framework nanoparticles and applied as a fiber coating for solid-phase microextraction (SPME). Chemical, thermal and morphological characteristics of the material were investigated. Headspace SPME followed by gas chromatography-electron capture detection was used for the determination of chlorobenzenes in the environmental samples. The key experimental factors affecting the extraction efficiency of the analytes, such as ionic strength, extraction and desorption temperature, and extraction time were investigated and optimized. The applicability of the coating for the extraction of chlorobenzenes from the environmental samples including river and tap water, sludge, and coastal soil was evaluated. The detection limits were in the range of 0.1–60 ng L{sup −1}. The relative standard deviations were between 2.0 and 5.0%. The extraction recovery of the analytes was in the range of 88–100%. Compared to the commercial PDMS fiber, the present fiber showed better extraction efficiency. - Highlights: • Metal-organic aerogel was synthesized and used as a novel fiber coating for SPME. • The new coating material showed high surface area and good thermal stability. • GC-ECD was used for determination of chlorobenzenes in environmental samples. • The method showed fast extraction and better efficiency than PDMS commercial fiber.

  19. Manifold Learning with Self-Organizing Mapping for Feature Extraction of Nonlinear Faults in Rotating Machinery

    Directory of Open Access Journals (Sweden)

    Lin Liang

    2015-01-01

    Full Text Available A new method for extracting the low-dimensional feature automatically with self-organization mapping manifold is proposed for the detection of rotating mechanical nonlinear faults (such as rubbing, pedestal looseness. Under the phase space reconstructed by single vibration signal, the self-organization mapping (SOM with expectation maximization iteration algorithm is used to divide the local neighborhoods adaptively without manual intervention. After that, the local tangent space alignment algorithm is adopted to compress the high-dimensional phase space into low-dimensional feature space. The proposed method takes advantages of the manifold learning in low-dimensional feature extraction and adaptive neighborhood construction of SOM and can extract intrinsic fault features of interest in two dimensional projection space. To evaluate the performance of the proposed method, the Lorenz system was simulated and rotation machinery with nonlinear faults was obtained for test purposes. Compared with the holospectrum approaches, the results reveal that the proposed method is superior in identifying faults and effective for rotating machinery condition monitoring.

  20. Prediction of extraction ability during metal complexing with organic phosphorus extractants

    International Nuclear Information System (INIS)

    Rozen, A.M.; Krupnov, B.V.

    1995-01-01

    Quantum-chemical calculations of thermodynamic parameters of complexing of neutral organic phosphorus compounds (phosphates, phosphine oxides and diphosphine dioxides with different substituents) with seven acceptors of different strength have been made. It is shown that in a wide range of the complexes strength change the entropy contribution of the Gibbs energy of complexing depends but slightly both on the ligand basicity and on the acceptor nature. It is ascertained that this reaction series is isoentropic for any Lewis acid. Practicability of the previously used correlation between extractability and complexing enthalpy has been proved. 17 refs., 1 fig., 1 tab

  1. Modeling the effect of temperature on thorium and nitric acid extraction and the formation of third phase for modification of the SEPHIS: Thorex computer program

    Energy Technology Data Exchange (ETDEWEB)

    Watson, S.B.; Rainey, R.H.

    1979-05-01

    Mathematical models have been developed for use with the SEPHIS - Thorex code which correct for the effect of temperature on thorium and nitric acid extraction and which provide a signal to indicate the formation of a second organic phase. Experimental programs have provided data which have been analyzed and indicate that increasing temperature decreases the distribution coefficient of thorium. Also increasing the temperature increases the concentration of thorium in the organic phase at which the third phase is formed. 14 figures, 3 tables.

  2. Comparison of solvent extraction and solid-phase extraction for the determination of polychlorinated biphenyls in transformer oil.

    Science.gov (United States)

    Mahindrakar, A N; Chandra, S; Shinde, L P

    2014-01-01

    Solid-phase extraction (SPE) of nine polychlorinated biphenyls (PCBs) from transformer oil samples was evaluated using octadecyl (CI8)-bonded porous silica. The efficiency of SPE of these PCBs was compared with those obtained by solvent extraction with DMSO and hexane. Average recoveries exceeding 95% for these PCBs were obtained via the SPE method using small cartridges containing 100mg of 40 pm CI8-bonded porous silica. The average recovery by solvent extraction with DMSO and hexane exceeded 83%. It was concluded that the recoveries and precision for the solvent extraction of PCBs were poorer than those for the SPE. Copyright © 2013 Elsevier Ltd. All rights reserved.

  3. Application of microwave irradiation to organic liquid phase reactions

    International Nuclear Information System (INIS)

    Huang Kun; Liu Hua; Ji Xuelin

    1994-01-01

    Microwave irradiation has been used in organic liquid phase reactions to significantly reduce the reaction time and improve the yield. The proposed mechanism, the development of techniques and reactions, such as Diels-Alder, ene, rearrangement reactions etc., are discussed

  4. Transvaginal organ extraction: potential for broad clinical application.

    Science.gov (United States)

    Jacobsen, Garth R; Barajas-Gamboa, Juan S; Coker, Alisa M; Cheverie, Joslin; Macias, C Aitor; Sandler, Bryan J; Talamini, Mark A; Horgan, Santiago

    2014-02-01

    Natural orifice transluminal endoscopic surgery procedures have evolved over the past few years. A transvaginal approach is a promising alternative for intraperitoneal procedures. Our objective was to evaluate the safety and feasibility of transvaginal organ extraction. This institutional review board-approved protocol involved retrospective review of an ongoing prospective study. Female subjects who presented to our hospital for elective cholecystectomy, appendectomy, or sleeve gastrectomy were offered participation in the study. Eligible patients met the following criteria: age between 18 and 75, diagnosis of gallbladder disease, acute appendicitis, or morbid obesity who desired surgical treatment. A hybrid transvaginal natural orifice approach was used in this series. Thirty-four women underwent transvaginal organ extraction between September 2007 and January 2012. The mean age was 40 ± 12.1 years (range 23-63 years). The mean body mass index was 27 ± 6.4 kg/m(2) (range 16-43 kg/m(2)). All patients had an American Society of Anesthesiologists classification of two or below. The mean operative time for cholecystectomy, appendectomy, and sleeve gastrectomy was 90, 71, and 135 min, respectively. There were no conversions to open operation and no intraoperative complications. The mean hospital stay was 2 days for all cases. Patients were followed for a mean of 24 months (range 1-61 months). There were two pregnancies and two successful vaginal deliveries. Six patients (18 %) had minor complaints of spotting or heavy menses in the immediate postoperative period that resolved with conservative measures. There were no abdominal wall complications. There were no long-term complications and no mortalities. This initial experience suggests that this surgical approach is safe, does not increase length of stay, and has no long-term vaginal complications. Given this attractive profile, a transvaginal approach may prove to be a superior mode of organ extraction

  5. Organic Phase Change Materials And Their Textile Applications: An Overview

    OpenAIRE

    Sarıer, Nihal; Önder, Emel

    2012-01-01

    An organic phase change material (PCM) possesses the ability to absorb and release large quantity of latent heat during a phase change process over a certain temperature range. The use of PCMs in energy storage and thermal insulation has been tested scientifically and industrially in many applications. The broad based research and development studies concentrating on the characteristics of known organic PCMs and new materials as PCM candidates, the storage methods of PCMs, as well as the reso...

  6. Graphene oxide for solid-phase extraction of bioactive phenolic acids.

    Science.gov (United States)

    Hou, Xiudan; Wang, Xusheng; Sun, Yingxin; Wang, Licheng; Guo, Yong

    2017-05-01

    A solid-phase extraction (SPE) method for the efficient analysis of trace phenolic acids (PAs, caffeic acid, ferulic acid, protocatechuic acid, cinnamic acid) in urine was established. In this work, a graphene oxide (GO) coating was grafted onto pure silica to be investigated as SPE material. The prepared GO surface had a layered and wrinkled structure that was rough and well organized, which could provide more open adsorption sites. Owing to its hydrophilicity and polarity, GO showed higher extraction efficiency toward PAs than reduced GO did, in agreement with the theoretical calculation results performed by Gaussian 09 software. The adsorption mechanism of PAs on GO@Sil was also investigated through static state and kinetic state adsorption experiments, which showed a monolayer surface adsorption. Extraction capacity of the as-prepared material was optimized using the response surface methodology. Under the optimized conditions, the as-established method provided wide linearity range (2-50 μg L -1 for protocatechuic acid and 1-50 μg L -1 for caffeic acid, ferulic acid, and cinnamic acid) and low limits of detection (0.25-1 μg L -1 ). Finally, the established method was applied for the analysis of urine from two healthy volunteers. The results indicate that the prepared material is a practical, cost-effective medium for the extraction and determination of phenolic acids in complex matrices. Graphical Abstract A graphene oxide coating was grafted onto pure silica as the SPE material for the extraction of phenolic acids in urines and the extraction mechanism was also mainly investigated.

  7. Application of micro-solid-phase extraction for the on-site extraction of heterocyclic aromatic amines in seawater.

    Science.gov (United States)

    Basheer, Chanbasha

    2018-04-01

    An efficient on-site extraction technique to determine carcinogenic heterocyclic aromatic amines in seawater has been reported. A micro-solid-phase extraction device placed inside a portable battery-operated pump was used for the on-site extraction of seawater samples. Before on-site applications, parameters that influence the extraction efficiency (extraction time, type of sorbent materials, suitable desorption solvent, desorption time, and sample volume) were investigated and optimized in the laboratory. The developed method was then used for the on-site sampling of heterocyclic aromatic amines determination in seawater samples close to distillation plant. Once the on-site extraction completed, the small extraction device with the analytes was brought back to the laboratory for analysis using high-performance liquid chromatography with fluorescence detection. Based on the optimized conditions, the calibration curves were linear over the concentration range of 0.05-20 μg/L with correlation coefficients up to 0.996. The limits of detection were 0.004-0.026 μg/L, and the reproducibility values were between 1.3 and 7.5%. To evaluate the extraction efficiency, a comparison was made with conventional solid-phase extraction and it was applied to various fortified real seawater samples. The average relative recoveries obtained from the spiked seawater samples varied in the range 79.9-95.2%. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Optimization of Solid Phase Micro-Extraction (SPME for Monitoring Occupational Exposure to Ethyl Benzene

    Directory of Open Access Journals (Sweden)

    H Heidari

    2012-05-01

    Full Text Available

    Background and Objectives: Analytical methods for volatile organic compounds (VOCs in different samples need extraction of compounds, by applying hazardous solvents. Solid phase micro-extraction (SPME is a solvent-free equilibrium extraction method, in which proper calibration can allow quantitative determinations of VOCs at a very good sensitivity without the use of any organic solvent. VOCs are generally present in urine only at trace levels, therefore, a sensitive procedure is needed for their trace determinations. Throughout this study, headspace solid phase micro-extraction (HS-SPME was followed by GC-FID for ethyl benzene in spiked urine was optimized.

    Methods: In this study, the parameters influencing SPME and gas chromatography of ethyl benzene, including extraction time, temperature, desorption temperature, desorption time, salt addition, sample pH, sample volume and sample agitation were investigated.

    Results: Extraction procedure was performed at 30°C for 6 min, using 0.2 gml-1 of NaCl in the sample solution. The sample volume and sample pH were optimized at 5 ml and 7 (neutral pH, respectively. Desorption of the ethyl benzene was carried out for 60 sec. at 250°C. The method was also validated with three different spiked urine samples and illustrated an appropriate reproducibility over six consecutive days as well as six within-day experiments. During this investigation, parameters of accuracy, linearity, and detection limits of the procedure were also evaluated.

    Conclusion: The developed method of HS- SPME-GC-FID proved to be a simple, convenient, and practical procedure, and was successfully used for measuring of ethyl benzene in spiked urine.

  9. MOLECULARLY IMPRINTED SOLID PHASE EXTRACTION FOR TRACE ANALYSIS OF DIAZINON IN DRINKING WATER

    Directory of Open Access Journals (Sweden)

    M. Rahiminejad ، S. J. Shahtaheri ، M. R. Ganjali ، A. Rahimi Forushani ، F. Golbabaei

    2009-04-01

    Full Text Available Amongst organophosphate pesticides, the one most widely used and common environmental contaminant is diazinon; thus methods for its trace analysis in environmental samples must be developed. Use of diazinon imprinted polymers such as sorbents in solid phase extraction, is a prominent and novel application area of molecular imprinted polymers. For diazinon extraction, high performance liquid chromatography analysis was demonstrated in this study. During optimization of the molecular imprinted solid phase extraction procedure for efficient solid phase extraction of diazinon, Plackett-Burman design was conducted. Eight experimental factors with critical influence on molecular imprinted solid phase extraction performance were selected, and 12 different experimental runs based on Plackett-Burman design were carried out. The applicability of diazinon imprinted polymers as the sorbent in solid phase extraction, presented obtained good recoveries of diazinon from LC-grade water. An increase in pH caused an increase in the recovery on molecular imprinted solid phase extraction. From these results, the optimal molecular imprinted solid phase extraction procedure was as follows: solid phase extraction packing with 100 mg diazinon imprinted polymers; conditioning with 5 mL of methanol and 6 mL of LC-grade water; sample loading containing diazinon (pH=10; washing with 1 mL of LC-grade water, 1 mL LC- grade water containing 30% acetonitrile and 0.5 mL of acetonitrile, respectively; eluting with 1 mL of methanol containing 2% acetic acid. The percentage recoveries obtained by the optimized molecular imprinted solid phase extraction were more than 90% with drinking water spiked at different trace levels of diazinon. Generally speaking, the molecular imprinted solid phase extraction procedure and subsequent high performance liquid chromatography analysis can be a relatively fast and proper approach for qualitative and quantitative analysis of diazinon in

  10. DNA extraction on bio-chip: history and preeminence over conventional and solid-phase extraction methods.

    Science.gov (United States)

    Ayoib, Adilah; Hashim, Uda; Gopinath, Subash C B; Md Arshad, M K

    2017-11-01

    This review covers a developmental progression on early to modern taxonomy at cellular level following the advent of electron microscopy and the advancement in deoxyribonucleic acid (DNA) extraction for expatiation of biological classification at DNA level. Here, we discuss the fundamental values of conventional chemical methods of DNA extraction using liquid/liquid extraction (LLE) followed by development of solid-phase extraction (SPE) methods, as well as recent advances in microfluidics device-based system for DNA extraction on-chip. We also discuss the importance of DNA extraction as well as the advantages over conventional chemical methods, and how Lab-on-a-Chip (LOC) system plays a crucial role for the future achievements.

  11. Phase associations and potential selective extraction methods for selected high-tech metals from ferromanganese nodules and crusts with siderophores

    International Nuclear Information System (INIS)

    Mohwinkel, Dennis; Kleint, Charlotte; Koschinsky, Andrea

    2014-01-01

    Highlights: • Phase associations of metals in marine Fe–Mn nodules and crusts were determined. • Selective leaching experiments with siderophore desferrioxamine B were conducted. • Siderophores selectively mobilize high-tech metals associated with Fe carrier phases. • Base metal liberation including Fe and Mn is limited. • Siderophores have promising potential for application in ore processing industries. - Abstract: Deep-sea ferromanganese deposits contain a wide range of economically important metals. Ferromanganese crusts and nodules represent an important future resource, since they not only contain base metals such as Mn, Ni, Co, Cu and Zn, but are also enriched in critical or rare high-technology elements such as Li, Mo, Nb, W, the rare earth elements and yttrium (REY). These metals could be extracted from nodules and crusts as a by-product to the base metal production. However, there are no proper separation techniques available that selectively extract certain metals out of the carrier phases. By sequential leaching, we demonstrated that, except for Li, which is present in an easily soluble form, all other high-tech metals enriched in ferromanganese nodules and crusts are largely associated with the Fe-oxyhydroxide phases and only to subordinate extents with Mn-oxide phases. Based on this fact, we conducted selective leaching experiments with the Fe-specific organic ligand desferrioxamine-B, a naturally occurring and ubiquitous siderophore. We showed by leaching of ferromanganese nodules and crusts with desferrioxamine-B that a significant and selective extraction of high-tech metals such as Li, Mo, Zr, Hf and Ta is possible, while other elements like Fe and the base metals Mn, Ni, Cu, Co and Zn are not extracted to large extents. The set of selectively extracted elements can be extended to Nb and W if Mn and carbonate phases are stripped from the bulk nodule or crust prior to the siderophore leach by e.g. a sequential leaching technique. This

  12. Solid phase extraction-electrospray ionization mass spectrometric method for the determination of palladium

    International Nuclear Information System (INIS)

    Pranaw Kumar; Telmore, Vijay M.; Jaison, P.G.; Sarkar, Arnab; Alamelu, D.; Aggarwal, S.K.

    2015-01-01

    Platinum group of element (PGEs) are extensively used as a catalyst and anticancer reagent. Due to the soft nature of PGEs, sulphur based donar ligands are used for the separation of these elements. Studies on the formation of different species are helpful for obtaining the ideas about separation of these elements from the complex matrices. Palladium (Pd) is studied as a representative element which is also formed by nuclear fission of fissile nuclides. In view of the relatively small amount of solvent required for separation, solid phase extraction is preferred over most of the separation methods. Solid phase extraction method using DPX as a stationary phase was previously reported for the separation of Pd in SHLLW using benzoylthiourea as a ligand. However, in case of large volume samples manual extraction by DPX is tedious task. In the present studies, the feasibility of extraction using benzoylthiourea on automated solid phase extraction system was carried out for the extraction of Pd

  13. Advances in organic-inorganic hybrid sorbents for the extraction of organic and inorganic pollutants in different types of food and environmental samples.

    Science.gov (United States)

    Ng, Nyuk-Ting; Kamaruddin, Amirah Farhan; Wan Ibrahim, Wan Aini; Sanagi, Mohd Marsin; Abdul Keyon, Aemi S

    2018-01-01

    The efficiency of the extraction and removal of pollutants from food and the environment has been an important issue in analytical science. By incorporating inorganic species into an organic matrix, a new material known as an organic-inorganic hybrid material is formed. As it possesses high selectivity, permeability, and mechanical and chemical stabilities, organic-inorganic hybrid materials constitute an emerging research field and have become popular to serve as sorbents in various separaton science methods. Here, we review recent significant advances in analytical solid-phase extraction employing organic-inorganic composite/nanocomposite sorbents for the extraction of organic and inorganic pollutants from various types of food and environmental matrices. The physicochemical characteristics, extraction properties, and analytical performances of sorbents are discussed; including morphology and surface characteristics, types of functional groups, interaction mechanism, selectivity and sensitivity, accuracy, and regeneration abilities. Organic-inorganic hybrid sorbents combined with extraction techniques are highly promising for sample preparation of various food and environmental matrixes with analytes at trace levels. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Pfaff equation and Fourier analysis to phase extraction from an interferogram with carrier frequency

    International Nuclear Information System (INIS)

    Lara-Cortez, Francisco; Meneses-Fabian, Cruz; Rodriguez-Zurita, Gustavo

    2011-01-01

    In the phase extraction techniques, one of the steps most used is to calculate the phase unwrapping from the wrapped phase, which is generally obtained via the inverse tangent function. With the idea to avoid this process, in the present manuscript a method based in the solution of the Pfaff equations is proposed. It is shown that the Pfaff equation is formed with the phase gradient and an auxiliary vector. The phase gradient is obtained from an interference patron with carrier frequency by applying the Fourier transform method and the partial derivatives. In the present manuscript, mathematical analysis, numerical simulation, and the phase extraction of some experimental interferograms are shown.

  15. Tritium distribution ratios between the 30 % tributyl phosphate(TBP)-normal dodecane(nDD) organic phase and uranyl nitrate-nitric acid aqueous phase

    International Nuclear Information System (INIS)

    Fujine, Sachio; Uchiyama, Gunzou; Sugikawa, Susumu; Maeda, Mitsuru; Tsujino, Takeshi.

    1989-10-01

    Tritium distribution ratios between the organic and aqueous phases were measured for the system of 30 % tributyl phosphate(TBP)-normal dodecane(nDD)/uranyl nitrate-nitric acid water. It was confirmed that tritium is extracted by TBP into the organic phase in both chemical forms of tritiated water (HTO) and tritiated nitric acid (TNO 3 ). The value of tritium distribution ratio ranged from 0.002 to 0.005 for the conditions of 0-6 mol/L nitric acid, 0.5-800 mCi/L tritium in aqueous phase, and 0-125 g-U/L uranium in organic phase. Isotopic distribution coefficient of tritium between the organic and aqueous phases was observed to be about 0.95. (author)

  16. Sample preparation with solid phase microextraction and exhaustive extraction approaches: Comparison for challenging cases.

    Science.gov (United States)

    Boyacı, Ezel; Rodríguez-Lafuente, Ángel; Gorynski, Krzysztof; Mirnaghi, Fatemeh; Souza-Silva, Érica A; Hein, Dietmar; Pawliszyn, Janusz

    2015-05-11

    In chemical analysis, sample preparation is frequently considered the bottleneck of the entire analytical method. The success of the final method strongly depends on understanding the entire process of analysis of a particular type of analyte in a sample, namely: the physicochemical properties of the analytes (solubility, volatility, polarity etc.), the environmental conditions, and the matrix components of the sample. Various sample preparation strategies have been developed based on exhaustive or non-exhaustive extraction of analytes from matrices. Undoubtedly, amongst all sample preparation approaches, liquid extraction, including liquid-liquid (LLE) and solid phase extraction (SPE), are the most well-known, widely used, and commonly accepted methods by many international organizations and accredited laboratories. Both methods are well documented and there are many well defined procedures, which make them, at first sight, the methods of choice. However, many challenging tasks, such as complex matrix applications, on-site and in vivo applications, and determination of matrix-bound and free concentrations of analytes, are not easily attainable with these classical approaches for sample preparation. In the last two decades, the introduction of solid phase microextraction (SPME) has brought significant progress in the sample preparation area by facilitating on-site and in vivo applications, time weighted average (TWA) and instantaneous concentration determinations. Recently introduced matrix compatible coatings for SPME facilitate direct extraction from complex matrices and fill the gap in direct sampling from challenging matrices. Following introduction of SPME, numerous other microextraction approaches evolved to address limitations of the above mentioned techniques. There is not a single method that can be considered as a universal solution for sample preparation. This review aims to show the main advantages and limitations of the above mentioned sample

  17. Principles and applications of colorimetric solid-phase extraction with negligible depletion

    International Nuclear Information System (INIS)

    Dias, Neil C.; Porter, Marc D.; Fritz, James S.

    2006-01-01

    Colorimetric solid-phase extraction (C-SPE) is an integrated technique in which an analyte is selectively concentrated onto a disk and then quantitated by diffuse reflectance spectroscopy. This paper describes the results of an investigation that applies the concept of negligible depletion (ND) to C-SPE, representing the first application of ND concepts to solid-phase extractions. The approach relies on passing the minimal volume of sample through the disk required to reach an equilibrium in which the concentration of analyte in the sample entering and exiting the disk are equal. At this point, the amount of analyte extracted by the disk is proportional to the sample concentration but is independent of the sample volume passed through the disk. With this new method, called C-SPE/ND, the precise measurement of sample volume is no longer necessary. The work herein details the general principles of this new methodology, and validates its basic tenets in an investigation of the extraction of the organic dye methyl violet. The analytical capabilities of C-SPE/ND are then demonstrated by its application to measurements of iodine. Iodine is a biocide increasingly used as a simple and effective disinfectant for water in locations where municipal water treatment systems are potentially compromised. Thus, the ability to operate C-SPE in an ND mode notably enhances the broad-based utility of this methodology as a reliable and an easy-to-use analysis tool for water quality assessments. Since iodine is also the biocide used on NASAs Space Shuttle, C-SPE/ND has the potential to overcome problems associated with the removal of air bubbles entrapped in a water sample in the microgravity environment encountered in space exploration. Extensions of C-SPE/ND to facile determinations of other water quality parameters with respect to both earth- and space-based needs are briefly discussed

  18. Plutonium association with selected solid phases in soils of Rocky Flats, Colorado, using sequential extraction technique

    International Nuclear Information System (INIS)

    Litaor, M.I.; Ibrahim, S.A.

    1996-01-01

    Plutonium contamination in the soil environs of Rock Flats, CO, has been a potential health risk to the public since the late 1960s. Although the measurement of total activity of Pu-239 + 240 in the soil is important information in appraising this risk, total activity does not provide the information required to characterize the geochemical behavior that affects the transport of Pu from the soil and vadose zone to groundwater. A sequential extraction experiment was conducted to assess the geochemical association of Pu with selected mineralogical and chemical phases of the soil. In the surface horizons, Pu-239 + 240 was primarily associated with the organic C (45-65%), sesquioxides (20-40%), and the residual fraction (10-15%). A small portion of Pu-239+240 was associated with soluble (0.09-0.22%), exchangeable (0.04-0.08%), and carbonates (0.57-7.0%) phases. These results suggest that under the observed pH and oxic conditions, relatively little Pu-239 + 240 is available for geochemically induced transport processes. Uncommon hydrogeochemical conditions were observed during the spring of 1995, which may have facilitated a partial dissolution of sesquioxides followed by desorption of Pu resulting in increased Pu mobility. Systematic errors in the sequential extraction experiment due to postextraction readsorption were evaluated using Np-237 tracer as a surrogate to Pu-239. The results suggested that postextraction readsorption rates were insignificant during the first 30 min after extraction for most chemical and mineralogical phases under study. 50 refs., 2 figs., 5 tabs

  19. 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.

  20. Methods of Analysis by the U.S. Geological Survey Organic Geochemistry Research Group-Determination of Dissolved Isoxaflutole and Its Sequential Degradation Products, Diketonitrile and Benzoic Acid, in Water Using Solid-Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry

    Science.gov (United States)

    Meyer, Michael T.; Lee, Edward A.; Scribner, Elisabeth A.

    2007-01-01

    An analytical method for the determination of isoxaflutole and its sequential degradation products, diketonitrile and a benzoic acid analogue, in filtered water with varying matrices was developed by the U.S. Geological Survey Organic Geochemistry Research Group in Lawrence, Kansas. Four different water-sample matrices fortified at 0.02 and 0.10 ug/L (micrograms per liter) are extracted by vacuum manifold solid-phase extraction and analyzed by liquid chromatography/tandem mass spectrometry using electrospray ionization in negative-ion mode with multiple-reaction monitoring (MRM). Analytical conditions for mass spectrometry detection are optimized, and quantitation is carried out using the following MRM molecular-hydrogen (precursor) ion and product (p) ion transition pairs: 357.9 (precursor), 78.9 (p), and 277.6 (p) for isoxaflutole and diketonitrile, and 267.0 (precursor), 159.0 (p), and 223.1 (p) for benzoic acid. 2,4-dichlorophenoxyacetic acid-d3 is used as the internal standard, and alachlor ethanesulfonic acid-d5 is used as the surrogate standard. Compound detection limits and reporting levels are calculated using U.S. Environmental Protection Agency procedures. The mean solid-phase extraction recovery values ranged from 104 to 108 percent with relative standard deviation percentages ranging from 4.0 to 10.6 percent. The combined mean percentage concentration normalized to the theoretical spiked concentration of four water matrices analyzed eight times at 0.02 and 0.10 ug/L (seven times for the reagent-water matrix at 0.02 ug/L) ranged from approximately 75 to 101 percent with relative standard deviation percentages ranging from approximately 3 to 26 percent for isoxaflutole, diketonitrile, and benzoic acid. The method detection limit (MDL) for isoxaflutole and diketonitrile is 0.003 ug/L and 0.004 ug/L for benzoic acid. Method reporting levels (MRLs) are 0.011, 0.010, and 0.012 ug/L for isoxaflutole, diketonitrile, and benzoic acid, respectively. On the basis

  1. Instrument for Solvent Extraction and Analysis (ISEE) of Organics from Regolith Simulant Using Supercritical Fluid Extraction and Chromatography

    Science.gov (United States)

    Franco, Carolina; Hintze, Paul E.

    2017-01-01

    ISEE is an instrument with the potential to perform extractions from regolith found on the surface of asteroids and planets, followed by characterization and quantitation of the extracts using supercritical fluid extraction (SFE) and chromatography (SFC). SFE is a developed technique proven to extract a wide range of organic compounds. SFC is similar to High Performance Liquid Chromatography (HPLC) but has the advantage of performing chiral separations without needing to derivatize the chiral compounds. CO2 will be the solvent for both stages as it is readily available in the Mars atmosphere. ISEE will capture CO2 from the environment, and use it for SFE and SFC. If successful, this would allow ISEE to perform analysis of organic compounds without using consumables. This paper will present results on a preliminary, proof-of-principle effort to use SFE and SFC to extract and analyze lunar regolith simulant spiked with organic compounds representing a range of organics that ISEE would expect to characterize. An optimization of variables for the extraction of the organics from the spiked regolith was successfully developed, using 138 bar pressure and 40 C temperature. The extraction flow rate was optimized at 2% SLPM with 30% methanol modifier. The extractions were successful with a value of 77.3+/- 0.9% of organics extracted. However, the recovery of organics after the extraction was very low with only 48.5+/-14.2%. Moreover, three columns were selected to analyze multiple samples at a time; two of them are Viridis HSS C18 SB and Torus DIOL, and the third column, specific for chiral separations, has not yet been selected yet.

  2. Chelating agents as stationary phase in extraction chromatography, ch. 11

    International Nuclear Information System (INIS)

    Sebesta, F.

    1975-01-01

    Chelating agents have been used largely in extraction chromatography for separations related to activation analysis, for concentration of metals from dilute solutions, and for preparation of radiochemically pure or carrier-free radionuclides. This review deals with the theory of extraction by chelating agents, the experimental technique, and the chelating agents and systems used (β-diketones, oximes, hydroxamic acid, dithizone and diethyldithiocarbamic acid)

  3. 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

  4. Determination of amphetamine-type stimulants (ATSs) and synthetic cathinones in urine using solid phase micro-extraction fibre tips and gas chromatography-mass spectrometry

    OpenAIRE

    Alsenedi, Khalid A.; Morrison, Calum

    2018-01-01

    In recent years, an increasing number of stimulant drugs and new psychoactive substances (NPSs) have caused concern in scientific communities and therefore innovative methods to extract compounds from complex biological samples are required. This work is aimed at developing and validating a clean, convenient and straightforward extraction procedure with microliter amounts of organic solvent using Solid Phase Micro-Extraction tips (SPME tips) and analysis using Gas Chromatography-Mass Spectrom...

  5. Microporous Carbon Spheres Solid Phase Membrane Tip Extraction for the Analysis of Nitrosamines in Water Samples

    International Nuclear Information System (INIS)

    Mohammed Salisu Musa; Wan Aini Wan Ibrahim

    2015-01-01

    A simple solid phase membrane tip extraction (SPMTE) utilizing microporous carbon spheres (MCS) was developed for the analysis of nitrosamines in aqueous samples. The method termed MCS-SPMTE was optimized for various important extraction parameters namely conditioning organic solvent, extraction time, effects of salt addition and pH change, desorption time, desorption solvent and sample volume. Under the optimized conditions, the method indicated good linearity in the range of 10-100 μg/ L with coefficients of determination, r 2 ≥0.9984. The method also demonstrated good reproducibility with % RSDs values ranging from 2.2 - 8.9 (n = 3). Limit of detection (LOD) and limit of quantification (LOQ) for the method ranged from 3.2 - 4.8 μg/ L and 10.9 - 15.9 μg/L respectively. Recoveries for both tap-water and lake water samples spiked at 10 μg/L were in the range of 83.2 - 107.5 %. (author)

  6. Lunar In-Situ Volatile Extraction, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — A method of extracting volatile resources from the Lunar regolith is proposed to reduce the launch mass and cost of bringing such resources from the Earth to enable...

  7. Automated Feature Extraction from Hyperspectral Imagery, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — The proposed activities will result in the development of a novel hyperspectral feature-extraction toolkit that will provide a simple, automated, and accurate...

  8. Plasma Extraction of Oxygen from Martian Atmosphere, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Plasma techniques are proposed for the extraction of oxygen from the abundant carbon dioxide contained in the Martian atmosphere (96 % CO2). In this process, CO2 is...

  9. Solid phase extraction of hydroxyaromatic compounds from aquatic environment

    Directory of Open Access Journals (Sweden)

    P. T. Sukhanov

    2012-01-01

    Full Text Available The dependence of extraction parameters of hydroxyaromatic compounds on sort of polyurethane foam, nature and composition of solution deposited on a polymer foam, content of inorganic salt in solution.

  10. Removal of endotoxins from bacteriophage preparations by extraction with organic solvents.

    Directory of Open Access Journals (Sweden)

    Bożena Szermer-Olearnik

    Full Text Available Lipopolysaccharide (LPS, endotoxin, pyrogen constitutes a very troubling contaminant of crude phage lysates produced in Gram-negative bacteria. Toxicity of LPS depends on the strong innate immunity response including the cytokines. Therefore, its removal is important for bacteriophage applications. In this paper, we present a procedure for extractive removal of endotoxin from bacteriophage preparations with water immiscible solvents (1-octanol or 1-butanol. During extraction most of the phage lytic activity is retained in the aqueous phase, while endotoxin accumulates in the organic solvent. The levels of endotoxin (expressed as endotoxin units, EU in the aqueous bacteriophage-containing fraction determined by limulus amebocyte lysate or EndoLISA assay were exceptionally low. While the initial endotoxin levels in the crude phage lysates ranged between 10(3 and 10(5 EU/ml the average level after organic extraction remaining in the aqueous fraction was 5.3 EU/ml. These values when related to phage titers decreased from 10(3-10(5 EU/10(9 PFU (plaque forming units down to an average of 2.8 EU/10(9 PFU. The purification procedure is scalable, efficient and applicable to all the bacteriophages tested: T4, HAP1 (E. coli and F8 (P. aeruginosa.

  11. Soy Sauce Residue Oil Extracted by a Novel Continuous Phase Transition Extraction under Low Temperature and Its Refining Process.

    Science.gov (United States)

    Zhao, Lichao; Zhang, Yong; He, Liping; Dai, Weijie; Lai, Yingyi; Yao, Xueyi; Cao, Yong

    2014-04-09

    On the basis of previous single-factor experiments, extraction parameters of soy sauce residue (SSR) oil extracted using a self-developed continuous phase transition extraction method at low temperature was optimized using the response surface methodology. The established optimal conditions for maximum oil yield were n-butane solvent, 0.5 MPa extraction pressure, 45 °C temperature, 62 min extraction time, and 45 mesh raw material granularity. Under these conditions, the actual yield was 28.43% ± 0.17%, which is relatively close to the predicted yield. Meanwhile, isoflavone was extracted from defatted SSR using the same method, but the parameters and solvent used were altered. The new solvent was 95% (v/v) ethanol, and extraction was performed under 1.0 MPa at 60 °C for 90 min. The extracted isoflavones, with 0.18% ± 0.012% yield, mainly comprised daidzein and genistein, two kinds of aglycones. The novel continuous phase transition extraction under low temperature could provide favorable conditions for the extraction of nonpolar or strongly polar substances. The oil physicochemical properties and fatty acids compositions were analyzed. Results showed that the main drawback of the crude oil was the excess of acid value (AV, 63.9 ± 0.1 mg KOH/g) and peroxide value (POV, 9.05 ± 0.3 mmol/kg), compared with that of normal soybean oil. However, through molecular distillation, AV and POV dropped to 1.78 ± 0.12 mg KOH/g and 5.9 ± 0.08 mmol/kg, respectively. This refined oil may be used as feedstuff oil.

  12. In vitro antimicrobial potential of organic solvent extracts of novel ...

    African Journals Online (AJOL)

    SAM

    methanol and water extracts of selected promising actinomycetes strains were studied towards Gram- positive ... Glucose and all other chemicals were obtained from Himedia. (India). ..... acetate, benzene, n-butanol and ethanol to extract the.

  13. Carbon coated magnetic nanoparticles as a novel magnetic solid phase extraction adsorbent for simultaneous extraction of methamphetamine and ephedrine from urine samples.

    Science.gov (United States)

    Taghvimi, Arezou; Hamishehkar, Hamed

    2017-01-15

    This paper develops a highly selective, specific and efficient method for simultaneous determination of ephedrine and methamphetamine by a new carbon coated magnetic nanoparticles (C/MNPs) as a magnetic solid phase extraction (MSPE) adsorbent in biological urine medium. The characterization of synthesized magnetic nano adsorbent was completely carried out by various characterization techniques like Fourier transform infrared (FT-IR) spectroscopy, powder x-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). Nine important parameters influencing extraction efficiency including amount of adsorbent, amounts of sample volume, pH, type and amount of extraction organic solvent, time of extraction and desorption, agitation rate and ionic strength of extraction medium, were studied and optimized. Under optimized extraction conditions, a good linearity was observed in the concentration range of 100-2000ng/mL for ephedrine and 100-2500ng/mL for methamphetamine. Analysis of positive urine samples was carried out by proposed method with the recovery of 98.71 and 97.87% for ephedrine and methamphetamine, respectively. The results indicated that carbon coated magnetic nanoparticles could be applied in clinical and forensic laboratories for simultaneous determination of abused drugs in urine media. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Supercritical fluid extraction of uranium from tissue paper matrix using organic extractants

    International Nuclear Information System (INIS)

    Kanekar, A.S.; Bhattacharyya, A.; Pathak, P.N.; Mohapatra, P.K.; Manchanda, V.K.

    2009-01-01

    Direct extraction of dried uranyl nitrate from tissue paper matrix was carried out using supercritical carbon dioxide modified with methanol solutions of extractants such as tri-n-butyl phosphate (TBP) and di-n-hexyl octanamide (DHOA)). The effects of temperature, pressure, extractant and nitric acid concentration on the extraction of uranyl ion were investigated. (author)

  15. Organic light emitting diode with light extracting layer

    Science.gov (United States)

    Lu, Songwei

    2016-06-14

    A light extraction substrate includes a glass substrate having a first surface and a second surface. A light extraction layer is formed on at least one of the surfaces. The light extraction layer is a coating, such as a silicon-containing coating, incorporating nanoparticles.

  16. Two-dimensional solid-phase extraction strategy for the selective enrichment of aminoglycosides in milk.

    Science.gov (United States)

    Shen, Aijin; Wei, Jie; Yan, Jingyu; Jin, Gaowa; Ding, Junjie; Yang, Bingcheng; Guo, Zhimou; Zhang, Feifang; Liang, Xinmiao

    2017-03-01

    An orthogonal two-dimensional solid-phase extraction strategy was established for the selective enrichment of three aminoglycosides including spectinomycin, streptomycin, and dihydrostreptomycin in milk. A reversed-phase liquid chromatography material (C 18 ) and a weak cation-exchange material (TGA) were integrated in a single solid-phase extraction cartridge. The feasibility of two-dimensional clean-up procedure that experienced two-step adsorption, two-step rinsing, and two-step elution was systematically investigated. Based on the orthogonality of reversed-phase and weak cation-exchange procedures, the two-dimensional solid-phase extraction strategy could minimize the interference from the hydrophobic matrix existing in traditional reversed-phase solid-phase extraction. In addition, high ionic strength in the extracts could be effectively removed before the second dimension of weak cation-exchange solid-phase extraction. Combined with liquid chromatography and tandem mass spectrometry, the optimized procedure was validated according to the European Union Commission directive 2002/657/EC. A good performance was achieved in terms of linearity, recovery, precision, decision limit, and detection capability in milk. Finally, the optimized two-dimensional clean-up procedure incorporated with liquid chromatography and tandem mass spectrometry was successfully applied to the rapid monitoring of aminoglycoside residues in milk. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Huaier Aqueous Extract Induces Hepatocellular Carcinoma Cells Arrest in S Phase via JNK Signaling Pathway

    Directory of Open Access Journals (Sweden)

    Chengshuo Zhang

    2015-01-01

    Full Text Available Huaier aqueous extract, the main active constituent of Huaier proteoglycan, has antihepatocarcinoma activity in experimental and clinical settings. However, the potential and associated antihepatoma mechanisms of Huaier extract are not yet fully understood. Therefore, in this study, we aimed to elucidate the inhibitory proliferation effect of Huaier extract on apoptosis and cycle of HepG2 and Bel-7402 cells. Our data demonstrated that incubation with Huaier extract resulted in a marked decrease in cell viability dose-dependently. Flow cytometric analysis showed that a 48 h treatment of Huaier extract caused cell apoptosis. Typical apoptotic nucleus alterations were observed with fluorescence microscope after Hoechst staining. Immunoblot analysis further demonstrated that Huaier extract activated caspase 3 and PARP. Additionally, Huaier extract inhibited the activity of p-ERK, p-p38, and p-JNK in terms of MAPK. Furthermore, Huaier extract induced HCC cells arrest in S phase and decreased the cycle related protein expression of β-catenin and cyclin D1. Studies with JNK specific inhibitor, SP600125, showed that Huaier extract induced S phase arrest and decreased β-catenin and cyclin D1 expression via JNK signaling pathway. In conclusion, we verify that Huaier extract causes cell apoptosis and induces hepatocellular carcinoma cells arrest in S phase via JNK pathway, which advances our understanding on the molecular mechanisms of Huaier extract in hepatocarcinoma management.

  18. Optimization of cloud point extraction and solid phase extraction methods for speciation of arsenic in natural water using multivariate technique.

    Science.gov (United States)

    Baig, Jameel A; Kazi, Tasneem G; Shah, Abdul Q; Arain, Mohammad B; Afridi, Hassan I; Kandhro, Ghulam A; Khan, Sumaira

    2009-09-28

    The simple and rapid pre-concentration techniques viz. cloud point extraction (CPE) and solid phase extraction (SPE) were applied for the determination of As(3+) and total inorganic arsenic (iAs) in surface and ground water samples. The As(3+) was formed complex with ammonium pyrrolidinedithiocarbamate (APDC) and extracted by surfactant-rich phases in the non-ionic surfactant Triton X-114, after centrifugation the surfactant-rich phase was diluted with 0.1 mol L(-1) HNO(3) in methanol. While total iAs in water samples was adsorbed on titanium dioxide (TiO(2)); after centrifugation, the solid phase was prepared to be slurry for determination. The extracted As species were determined by electrothermal atomic absorption spectrometry. The multivariate strategy was applied to estimate the optimum values of experimental factors for the recovery of As(3+) and total iAs by CPE and SPE. The standard addition method was used to validate the optimized methods. The obtained result showed sufficient recoveries for As(3+) and iAs (>98.0%). The concentration factor in both cases was found to be 40.

  19. Six-phase soil heating accelerates VOC extraction from clay soil

    International Nuclear Information System (INIS)

    Gauglitz, P.A.; Roberts, J.S.; Bergsman, T.M.; Caley, S.M.; Heath, W.O.; Miller, M.C.; Moss, R.W.; Schalla, R.; Jarosch, T.R.; Eddy-Dilek, C.A.

    1994-08-01

    Six-Phase Soil Heating (SPSH) was demonstrated as a viable technology for heating low permeability soils containing volatile organic contaminants. Testing was performed as part of the Volatile Organic Compounds in Non-Arid Soils Integrated Demonstration (VOC Non-Arid ID) at the Savannah River Site. The soil at the integrated demonstration site is contaminated with perchloroethylene (PCE) and trichloroethylene (TCE); the highest soil contamination occurs in clay-rich zones that are ineffectively treated by conventional soil vapor extraction due to the very low permeability of the clay. The SPSH demonstration sought to heat the clay zone and enhance the performance of conventional soil vapor extraction. Thermocouples at thirty locations quantified the areal and vertical heating within the treated zone. Soil samples were collected before and after heating to quantify the efficacy of heat-enhanced vapor extraction of PCE and TCE from the clay soil. Samples were taken (essentially every foot) from six wells prior to heating and adjacent to these wells after heating. Results show that contaminant removal from the clay zone was 99.7% (median) within the electrode array. Outside the array where the soil was heated, but to only 50 degrees C, the removal efficiency was 93%, showing that heating accelerated the removal of VOCs from the clay soil. The accelerated remediation resulted from effective heating of the contaminated clay zone by SPSH. The temperature of the clay zone increased to 100 degrees C after 8 days of heating and was maintained near 100 degrees C for 17 days. Electrical heating removed 19,000 gal of water from the soil as steam, with peak removal rate of 1,500 gpd of condensed steam

  20. Phase shift extraction and wavefront retrieval from interferograms with background and contrast fluctuations

    International Nuclear Information System (INIS)

    Liu, Qian; Wang, Yang; He, Jianguo; Ji, Fang

    2015-01-01

    The fluctuations of background and contrast cause measurement errors in the phase-shifting technique. To extract the phase shifts from interferograms with background and contrast fluctuations, an iterative algorithm is represented. The phase shifts and wavefront phase are calculated in two individual steps with the least-squares method. The fluctuation factors are determined when the phase shifts are calculated, and the fluctuations are compensated when the wavefront phase is calculated. The advantage of the algorithm lies in its ability to extract phase shifts from interferograms with background and contrast fluctuations converging stably and rapidly. Simulations and experiments verify the effectiveness and reliability of the proposed algorithm. The convergence accuracy and speed are demonstrated by the simulation results. The experiment results show its ability for suppressing phase retrieval errors. (paper)

  1. Importance of the hexagonal lipid phase in biological membrane organization

    OpenAIRE

    Jouhet, Juliette

    2013-01-01

    Domains are present in every natural membrane. They are characterized by a distinctive protein and/or lipid composition. Their size is highly variable from the nano- to the micrometer scale. The domains confer specific properties to the membrane leading to original structure and function. The determinants leading to domain organization are therefore important but remain obscure. This review presents how the ability of lipids to organize into hexagonal II or lamellar phases can promote particu...

  2. EXTRACT

    DEFF Research Database (Denmark)

    Pafilis, Evangelos; Buttigieg, Pier Luigi; Ferrell, Barbra

    2016-01-01

    The microbial and molecular ecology research communities have made substantial progress on developing standards for annotating samples with environment metadata. However, sample manual annotation is a highly labor intensive process and requires familiarity with the terminologies used. We have the...... and text-mining-assisted curation revealed that EXTRACT speeds up annotation by 15-25% and helps curators to detect terms that would otherwise have been missed.Database URL: https://extract.hcmr.gr/......., organism, tissue and disease terms. The evaluators in the BioCreative V Interactive Annotation Task found the system to be intuitive, useful, well documented and sufficiently accurate to be helpful in spotting relevant text passages and extracting organism and environment terms. Comparison of fully manual...

  3. Solid-phase extraction procedures in systematic toxicological analysis

    NARCIS (Netherlands)

    Franke, J.P.; de Zeeuw, R.A

    1998-01-01

    In systematic toxicological analysis (STA) the substance(s) present is (are) not known at the start of the analysis. in such an undirected search the extraction procedure cannot be directed to a given substance but must be a general procedure where a compromise must be reached in that the substances

  4. after solid phase extraction on modified sawdust s

    African Journals Online (AJOL)

    Preferred Customer

    extraction (SPE) techniques are widely used for the determination of trace metal ions in aqueous samples, because ... adsorption resin [16] and modified activated carbon [17]. ... washed with distilled water, and dried in oven at 40 ºC for 24 h.

  5. Solvent extraction of organic acids from stillage for its re-use in ethanol production process.

    Science.gov (United States)

    Castro, G A; Caicedo, L A; Alméciga-Díaz, C J; Sanchez, O F

    2010-06-01

    Stillage re-use in the fermentation stage in ethanol production is a technique used for the reduction of water and fermentation nutrients consumption. However, the inhibitory effect on yeast growth of the by-products and feed components that remains in stillage increases with re-use and reduces the number of possible recycles. Several methods such as ultrafiltration, electrodialysis and advanced oxidation processes have been used in stillage treatment prior its re-use in the fermentation stage. Nevertheless, few studies evaluating the effect of solvent extraction as a stillage treatment option have been performed. In this work, the inhibitory effect of serial stillage recycling over ethanol and biomass production was determined, using acetic acid as a monitoring compound during the fermentation and solvent extraction process. Raw palm oil methyl ester showed the highest acetic acid extraction from the aqueous phase, presenting a distribution coefficient of 3.10 for a 1:1 aqueous phase mixture:solvent ratio. Re-using stillage without treatment allowed up to three recycles with an ethanol production of 53.7 +/- 2.0 g L(-1), which was reduced 25% in the fifth recycle. Alternatively, treated stillage allowed up to five recycles with an ethanol final concentration of 54.7 +/- 1.3 g L(- 1). These results show that reduction of acetic acid concentration by an extraction process with raw palm oil methyl ester before re-using stillage improves the number of recycles without a major effect on ethanol production. The proposed process generates a palm oil methyl ester that contains organic acids, among other by-products, that could be used for product recovery and as an alternative fuel.

  6. Improved detection limits for phthalates by selective solid-phase micro-extraction

    KAUST Repository

    Zia, Asif I.; Afsarimanesh, Nasrin; Xie, Li; Nag, Anindya; Al-Bahadly, I. H.; Yu, P. L.; Kosel, Jü rgen

    2016-01-01

    Presented research reports on an improved method and enhanced limits of detection for phthalates; a hazardous additive used in the production of plastics by solid-phase micro-extraction (SPME) polymer in comparison to molecularly imprinted solid

  7. Utilizing ion-pairing hydrophilic interaction chromatography solid phase extraction for efficient glycopeptide enrichment in glycoproteomics

    DEFF Research Database (Denmark)

    Mysling, Simon; Palmisano, Giuseppe; Højrup, Peter

    2010-01-01

    Glycopeptide enrichment is a prerequisite to enable structural characterization of protein glycosylation in glycoproteomics. Here we present an improved method for glycopeptide enrichment based on zwitter-ionic hydrophilic interaction chromatography solid phase extraction (ZIC-HILIC SPE...

  8. Development and validation of a magnetic solid-phase extraction with high-performance liquid chromatography method for the simultaneous determination of amphetamine and methadone in urine.

    Science.gov (United States)

    Taghvimi, Arezou; Hamishehkar, Hamed; Ebrahimi, Mahmoud

    2016-06-01

    The simultaneous determination of amphetamine and methadone was carried out by magnetic graphene oxide nanoparticles, a magnetic solid-phase extraction adsorbent, as a new sample treatment technique. The main factors (the amounts of sample volume, amount of adsorbent, type and amount of extraction organic solvent, time of extraction and desorption, pH, the ionic strength of extraction medium, and agitation rate) influencing the extraction efficiency were investigated and optimized. Under the optimized conditions, good linearity was observed in the range of 100-1500 ng/mL for amphetamine and 100-1000 ng/mL for methadone. The method was evaluated for determination of AM and methadone in positive urine samples, satisfactory results were obtained, therefore magnetic solid-phase extraction can be applied as a novel method for the determination of drugs of abuse in forensic laboratories. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Experimental design for extraction and quantification of phenolic compounds and organic acids in white "Vinho Verde" grapes.

    Science.gov (United States)

    Dopico-García, M S; Valentão, P; Guerra, L; Andrade, P B; Seabra, R M

    2007-01-30

    An experimental design was applied for the optimization of extraction and clean-up processes of phenolic compounds and organic acids from white "Vinho Verde" grapes. The developed analytical method consisted in two steps: first a solid-liquid extraction of both phenolic compounds and organic acids and then a clean-up step using solid-phase extraction (SPE). Afterwards, phenolic compounds and organic acids were determined by high-performance liquid chromatography (HPLC) coupled to a diode array detector (DAD) and HPLC-UV, respectively. Plackett-Burman design was carried out to select the significant experimental parameters affecting both the extraction and the clean-up steps. The identified and quantified phenolic compounds were: quercetin-3-O-glucoside, quercetin-3-O-rutinoside, kaempferol-3-O-rutinoside, isorhamnetin-3-O-glucoside, quercetin, kaempferol and epicatechin. The determined organic acids were oxalic, citric, tartaric, malic, shikimic and fumaric acids. The obtained results showed that the most important variables were the temperature (40 degrees C) and the solvent (acid water at pH 2 with 5% methanol) for the extraction step and the type of sorbent (C18 non end-capped) for the clean-up step.

  10. Solid-phase extraction of berries’ anthocyanins and evaluation of their antioxidative properties

    Czech Academy of Sciences Publication Activity Database

    Denev, P.; Číž, Milan; Ambrožová, Gabriela; Lojek, Antonín; Yanakieva, I.; Kratchanova, M.

    2010-01-01

    Roč. 123, č. 4 (2010), s. 1055-1061 ISSN 0308-8146 R&D Projects: GA MŠk(CZ) OC08058 Institutional research plan: CEZ:AV0Z50040507; CEZ:AV0Z50040702 Keywords : anthocyanins * solid-phase extraction * berry extracts Subject RIV: BO - Biophysics Impact factor: 3.458, year: 2010

  11. 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.

  12. Polyaniline-coated cigarette filters as a solid-phase extraction sorbent for the extraction and enrichment of polycyclic aromatic hydrocarbon in water samples.

    Science.gov (United States)

    Bunkoed, Opas; Rueankaew, Thanaschaphorn; Nurerk, Piyaluk; Kanatharana, Proespichaya

    2016-06-01

    Polyaniline coated cigarette filters were successfully synthesized and used as a solid-phase extraction sorbent for the extraction and preconcentration of polycyclic aromatic hydrocarbons in water samples. The polyaniline helped to enhance the adsorption ability of polycyclic aromatic hydrocarbons on the sorbent through π-π interactions. The high porosity and large surface area of the cigarette filters helped to reduce backpressure and can be operated with high sample flow rate without loss of extraction efficiency. The developed sorbent was characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. The parameters that affected the extraction efficiencies, i.e. polymerization time, type of desorption solvent and its volume, sample flow rate, sample volume, sample pH, ionic strength, and organic modifier were investigated. Under the optimal conditions, the method was linear over the range of 0.5-10 μg/L and a detection limit of 0.5 ng/L. This simple, rapid, and cost-effective method was successfully applied to the preconcentration of polycyclic aromatic hydrocarbons from water samples. The developed method provided a high enrichment factor with good extraction efficiency (85-98%) and a relative standard deviation <10%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. 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.

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

    Science.gov (United States)

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

    2007-11-09

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

  15. Effects of degradation on third phase formation in the extraction of Th(NO3)4 by trialkyl phosphates

    International Nuclear Information System (INIS)

    Benadict Rakesh, K.; Suresh, A.; Vasudeva Rao, P.R.

    2014-01-01

    It is well known that solvents undergo chemical and radiolytic degradation during processing and in general the degradation products affect organic-aqueous phase separation, extraction and stripping behaviour, density, viscosity etc. In the present study, an attempt has been made to understand the effects of irradiation (100 MRad with 60 Co- γ-source) on third phase formation in the extraction of Th(IV) from nitric acid media by 1.1 M solutions of tri-n-butyl phosphate (TBP) and tri-iso-amyl phosphate (TiAP) in n-dodecane (n-DD). Two types of irradiated solvents, namely Type 1 solvents containing only primary degradation products (formed by the degradation of TBP molecules) and Type 2 solvents containing primary as well as secondary degradation products (surfactant type molecules formed by the reaction between the degradation products of extractant and diluent) were prepared by dissolving required amount of irradiated extractant in unirradiated n-DD and irradiating 1.1 M solutions of extractant in n-DD, respectively. These solvents with and without washing with 5 M NaOH solution have been investigated for third phase formation. The variations of limiting organic concentration (LOC) for third phase formation as a function of equilibrium aqueous phase acidity are shown. LOC values for third phase formation by unirradiated solvents reported in our earlier work are also shown. These figures depict that LOC values for Type 1 solvents are lower than the corresponding unirradiated solvents and can be attributed to the decrease in the extractant concentration by degradation. Estimation of extractant in Type 1 solvents by nitric acid equilibration method after the removal of primary degradation products by washing with 5 M NaOH solution revealed that extractant concentrations have been reduced to 1.03 M and 1.05 M for TBP and TiAP, respectively. Estimation of extractant in Type 2 solvents revealed 1.07 M extractant concentration in TBP and TiAP solvents. However, data

  16. Solid phase extraction method for determination of mitragynine in ...

    African Journals Online (AJOL)

    phase high performance liquid chromatography (RP-HPLC) to determine mitragynine (MG) in rat and human urine, and to investigate the influence of caffeine (CF) on urinary excretion of MG in rats. Methods: A two-dimensional wash-elute ...

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

    International Nuclear Information System (INIS)

    Siti Munirah Abd Wahib; Mohd Marsin Sanagi

    2016-01-01

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

  18. Novel approach to microwave-assisted extraction and micro-solid-phase extraction from soil using graphite fibers as sorbent.

    Science.gov (United States)

    Xu, Li; Lee, Hian Kee

    2008-05-30

    A single-step extraction-cleanup procedure involving microwave-assisted extraction (MAE) and micro-solid-phase extraction (micro-SPE) has been developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) from soil samples. Micro-SPE is a relatively new extraction procedure that makes use of a sorbent enclosed within a sealed polypropylene membrane envelope. In the present work, for the first time, graphite fiber was used as a sorbent material for extraction. MAE-micro-SPE was used to cleanup sediment samples and to extract and preconcentrate five PAHs in sediment samples prepared as slurries with addition of water. The best extraction conditions comprised of microwave heating at 50 degrees C for a duration of 20 min, and an elution (desorption) time of 5 min using acetonitrile with sonication. Using gas chromatography (GC)-flame ionization detection (FID), the limits of detection (LODs) of the PAHs ranged between 2.2 and 3.6 ng/g. With GC-mass spectrometry (MS), LODs were between 0.0017 and 0.0057 ng/g. The linear ranges were between 0.1 and 50 or 100 microg/g for GC-FID analysis, and 1 and 500 or 1000 ng/g for GC-MS analysis. Granular activated carbon was also used for the micro-SPE device but was found to be not as efficient in the PAH extraction. The MAE-micro-SPE method was successfully used for the extraction of PAHs in river and marine sediments, demonstrating its applicability to real environmental solid matrixes.

  19. Extraction of interesting organic compounds from olive oil waste

    Directory of Open Access Journals (Sweden)

    Jiménez, Ana

    2006-03-01

    Full Text Available In the olive fruits there is a large amount of bioactive compounds and substances of high interest. Many of them are known by owing health beneficial properties that contribute to protective effect of the virgin olive oil. During olive oil processing, most of them remain in the olive oil wastes. Although, olive-mill wastewater (OMWW or “alpechin”, olive oil cake (OOC, and the new by-product, known as “alperujo” in Spain and generated by the two-phase extraction process, represent a major disposal and potentially severe pollution problem for the industry, they are also promising source of substances of high value. This review summarises the last knowledge on the utilisation of residual products, with more than 90 references including articles and patents, which are promising with regard to future application. All these investigations have been classified into two options, the recovery of valuable natural constituents and the bioconversion into useful products.Existe una gran cantidad de compuestos bioactivos y de alto interés presentes en la aceituna. Muchos de ellos se conocen por las cualidades beneficiosas que aportan al aceite de oliva virgen. La mayoría permanecen en mayor cantidad en el subproducto de la extracción del aceite. Aunque, el alpechín, el orujo y el nuevo subproducto de extracción del aceite en dos fases, alperujo, representan un problema potencial de vertido y contaminación, también son una prometedora fuente de compuestos de alto valor. Esta revisión resume lo último que se conoce sobre la utilización de estos residuos en el campo anteriormente mencionado, con más de 90 referencias que incluyen artículos y patentes. Todas estas investigaciones han sido clasificadas en cuanto a la recuperación de constituyentes naturalmente presentes o en cuanto a la bioconversión de los residuos en sustancias de interés.

  20. Surfactant assisted pulsed two-phase electromembrane extraction followed by GC analysis for quantification of basic drugs in biological samples.

    Science.gov (United States)

    Zahedi, Pegah; Davarani, Saied Saeed Hosseiny; Moazami, Hamid Reza; Nojavan, Saeed

    2016-01-05

    In this work, a simple and efficient surfactant assisted pulsed two-phase electromembrane extraction (SA-PEME) procedure combined with gas chromatography (GC) has been developed for the determination of alfentanil, sufentanil and methadone in various samples. It has been found that the addition of anionic surfactant causes the accumulation of the cationic analytes at the SLM/solution interface resulting in an easier transfer of the analytes into the organic phase. The method was accomplished with 1-octanol as the acceptor phase and supported liquid membrane (SLM) by means of an 80 V pulsed electrical driving force and the extraction time of 20 min. The model analytes were extracted from 3.0 mL sample solution (pH 4.0) containing 0.02% w/v surfactant (sodium dodecyl sulfate). The duty cycle of 92% and frequency of 0.357 Hz gave the best performance. Extraction recoveries in the range of 70.5-95.2% and satisfactory repeatability (7.6samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Preparation of alumina-coated magnetite nanoparticle for extraction of trimethoprim from environmental water samples based on mixed hemimicelles solid-phase extraction.

    Science.gov (United States)

    Sun, Lei; Zhang, Chuanzhou; Chen, Ligang; Liu, Jun; Jin, Haiyan; Xu, Haoyan; Ding, Lan

    2009-04-13

    In this study, a new type of alumina-coated magnetite nanoparticles (Fe(3)O(4)/Al(2)O(3) NPs) modified by the surfactant sodium dodecyl sulfate (SDS) has been successfully synthesized and applied for extraction of trimethoprim (TMP) from environmental water samples based on mixed hemimicelles solid-phase extraction (MHSPE). The coating of alumina on Fe(3)O(4) NPs not only avoids the dissolving of Fe(3)O(4) NPs in acidic solution, but also extends their application without sacrificing their unique magnetization characteristics. Due to the high surface area of these new sorbents and the excellent adsorption capacity after surface modification by SDS, satisfactory concentration factor and extraction recoveries can be produced with only 0.1g Fe(3)O(4)/Al(2)O(3) NPs. Main factors affecting the adsolubilization of TMP such as the amount of SDS, pH value, standing time, desorption solvent and maximal extraction volume were optimized. Under the selected conditions, TMP could be quantitatively extracted. The recoveries of TMP by analyzing the four spiked water samples were between 67 and 86%, and the relative standard deviation (RSD) ranged from 2 to 6%. Detection and quantification limits of the proposed method were 0.09 and 0.24 microg L(-1), respectively. Concentration factor of 1000 was achieved using this method to extract 500 mL of different environmental water samples. Compared with conventional SPE methods, the advantages of this new Fe(3)O(4)/Al(2)O(3) NPs MHSPE method still include easy preparation and regeneration of sorbents, short times of sample pretreatment, high extraction yields, and high breakthrough volumes. It shows great analytical potential in preconcentration of organic compounds from large volume water samples.

  2. EXTRACTION CHARACTERISTICS OF THE CATION OF ALKYLDIMETHYLBENZYLAMMONIUM CHLORIDE AT THE PHASE BOUNDARY WATER-MEMBRANE SOLVENT

    Directory of Open Access Journals (Sweden)

    O. V. Luganska

    2015-06-01

    Full Text Available The extraction coefficients of the cation of alkyldimethylbenzylammonium chloride at the phase boundary water-tricresylphosphate, water-dioctylphthalate, water-dibutylphtalate have been determined by the potentiometric titration of the aqueous phase with a silver electrode. The correctness of the obtained results has been proved by the titrimetric method with visual fixation of the equivalence point using methylene blue indicator.

  3. Analysis of volatiles in silver carp by headspace solid phase micro-extraction coupled with GC-MS

    International Nuclear Information System (INIS)

    Yang Yuping; Xiong Guangquan; Cheng Wei; Liao Tao; Lin Ruotai; Geng Shengrong; Li Xin; Li Xiaoding; Wu Wenjin

    2010-01-01

    In this paper, a method for the determination of volatiles using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) was presented. The extraction conditions were optimized with reference to these volatiles as hexanal, heptanal, benzaldehyde, 1-Octen-3-ol, octanal, nonanal, decenal, 2,4-heptadienal and 2,4-decadienal. The extraction of fish muscle followed by incubation on a StableFlex divinyl benzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber during 50 in at 60 obtained the most effective extraction of the analytes. The methods by HS-SPME and GC-MS were effective in detecting volatiles in the gills, scales, viscera and fish muscles. The types of volatiles in the gill were more than other organs and the number of odors compounds was 63, and the number of volatiles in scales, viscera and fish muscles was 48, 44 and 42 respectively. (authors)

  4. A green deep eutectic solvent-based aqueous two-phase system for protein extracting

    International Nuclear Information System (INIS)

    Xu, Kaijia; Wang, Yuzhi; Huang, Yanhua; Li, Na; Wen, Qian

    2015-01-01

    Highlights: • A strategy for the protein purification with a deep eutectic solvent(DES)-based aqueous two-phase system. • Choline chloride-glycerin DES was selected as the extraction solvent. • Bovine serum albumin and trypsin were used as the analytes. • Aggregation phenomenon was detected in the mechanism research. - Abstract: As a new type of green solvent, deep eutectic solvent (DES) has been applied for the extraction of proteins with an aqueous two-phase system (ATPS) in this work. Four kinds of choline chloride (ChCl)-based DESs were synthesized to extract bovine serum albumin (BSA), and ChCl-glycerol was selected as the suitable extraction solvent. Single factor experiments have been done to investigate the effects of the extraction process, including the amount of DES, the concentration of salt, the mass of protein, the shaking time, the temperature and PH value. Experimental results show 98.16% of the BSA could be extracted into the DES-rich phase in a single-step extraction under the optimized conditions. A high extraction efficiency of 94.36% was achieved, while the conditions were applied to the extraction of trypsin (Try). Precision, repeatability and stability experiments were studied and the relative standard deviations (RSD) of the extraction efficiency were 0.4246% (n = 3), 1.6057% (n = 3) and 1.6132% (n = 3), respectively. Conformation of BSA was not changed during the extraction process according to the investigation of UV–vis spectra, FT-IR spectra and CD spectra of BSA. The conductivity, dynamic light scattering (DLS) and transmission electron microscopy (TEM) were used to explore the mechanism of the extraction. It turned out that the formation of DES–protein aggregates play a significant role in the separation process. All the results suggest that ChCl-based DES-ATPS are supposed to have the potential to provide new possibilities in the separation of proteins

  5. Determination of colloidal and dissolved silver in water samples using colorimetric solid-phase extraction.

    Science.gov (United States)

    Hill, April A; Lipert, Robert J; Porter, Marc D

    2010-03-15

    The increase in bacterial resistance to antibiotics has led to resurgence in the use of silver as a biocidal agent in applications ranging from washing machine additives to the drinking water treatment system on the International Space Station (ISS). However, growing concerns about the possible toxicity of colloidal silver to bacteria, aquatic organisms and humans have led to recently issued regulations by the US EPA and FDA regarding the usage of silver. As part of an ongoing project, we have developed a rapid, simple method for determining total silver, both ionic (silver(I)) and colloidal, in 0.1-1mg/L aqueous samples, which spans the ISS potable water target of 0.3-0.5mg/L (total silver) and meets the US EPA limit of 0.1mg/L in drinking water. The method is based on colorimetric solid-phase extraction (C-SPE) and involves the extraction of silver(I) from water samples by passage through a solid-phase membrane impregnated with the colorimetric reagent DMABR (5-[4-(dimethylamino)benzylidene]rhodanine). Silver(I) exhaustively reacts with impregnated DMABR to form a colored compound, which is quantified using a handheld diffuse reflectance spectrophotometer. Total silver is determined by first passing the sample through a cartridge containing Oxone, which exhaustively oxidizes colloidal silver to dissolved silver(I). The method, which takes less than 2 min to complete and requires only approximately 1 mL of sample, has been validated through a series of tests, including a comparison with the ICP-MS analysis of a water sample from ISS that contained both silver(I) and colloidal silver. Potential earth-bound applications are also briefly discussed. Copyright (c) 2009 Elsevier B.V. All rights reserved.

  6. [Determination of patulin in fruits and jam by solid phase extraction-ultra performance liquid chromatography].

    Science.gov (United States)

    Lü, Weichao; Shen, Shuchang; Wang, Chao

    2017-11-08

    With magnesium silicate, silica gel, diatomite and calcium sulfate as raw materials, a new solid phase extraction column was prepared through a series of processes of grinding to ethanol homogenate, drying and packing into polypropylene tube. The sample was hydrolyzed by pectinase, extracted by acetonitrile and purified by solid phase extraction. The target compounds were separated on a C18 column (100 mm×2.1 mm, 1.8 μm), using 0.8% (v/v) tetrahydrofuran solution as mobile phase with a flow rate of 0.5 mL/min. The detection wavelength was 276 nm. The effect of pectinase on extraction yield and purification effect of solid-phase extraction column were investigated. The optimum chromatographic conditions were selected. There was a good linear relationship between the peak heights and the mass concentrations of patulin in the range of 0.1 to 10 mg/L with the correlation coefficient ( R 2 ) of 1. The limit of detection for this method was 10.22 μg/kg. The spiked recoveries of samples were 86.58%-94.84% with the relative standard deviations (RSDs) of 1.45%-2.28%. The results indicated that the self-made solid phase extraction column had a good purification efficiency, and the UPLC had a high separation efficiency. The method is simple, accurate and of great significance for the quality and safety control of fruit products.

  7. Tetraphenylimidodiphosphinate as solid phase extractant for preconcentrative separation of thorium from aqueous solution

    International Nuclear Information System (INIS)

    Na Liu; Yanfei Wang; Chuhua He

    2016-01-01

    A simple and reliable method for solid phase extraction of thorium using tetraphenylimidodiphosphinate is presented. The solid phase extraction process was optimized at equilibrium time 3 h, pH = 4.5, initial concentration 30 mg L -1 and extractant dosage 0.01 g with 98.95 % of removal efficiency and 29.68 mg g -1 of adsorption capacity. The interfering ions experiments indicated that it had almost no effect on thorium adsorption. Kinetics data follow the pseudo-first-order model and equilibrium data agreed with the Langmuir isotherm model very well. FT-IR analysis indicated that imino group and phosphoryl acted as the significant roles in the solid phase extraction process. (author)

  8. Molecularly imprinted solid-phase extraction in the analysis of agrochemicals.

    Science.gov (United States)

    Yi, Ling-Xiao; Fang, Rou; Chen, Guan-Hua

    2013-08-01

    The molecular imprinting technique is a highly predeterminative recognition technology. Molecularly imprinted polymers (MIPs) can be applied to the cleanup and preconcentration of analytes as the selective adsorbent of solid-phase extraction (SPE). In recent years, a new type of SPE has formed, molecularly imprinted polymer solid-phase extraction (MISPE), and has been widely applied to the extraction of agrochemicals. In this review, the mechanism of the molecular imprinting technique and the methodology of MIP preparations are explained. The extraction modes of MISPE, including offline and online, are discussed, and the applications of MISPE in the analysis of agrochemicals such as herbicides, fungicides and insecticides are summarized. It is concluded that MISPE is a powerful tool to selectively isolate agrochemicals from real samples with higher extraction and cleanup efficiency than commercial SPE and that it has great potential for broad applications.

  9. A novel method to augment extraction of mangiferin by application of microwave on three phase partitioning.

    Science.gov (United States)

    Kulkarni, Vrushali M; Rathod, Virendra K

    2015-06-01

    This work reports a novel approach where three phase partitioning (TPP) was combined with microwave for extraction of mangiferin from leaves of Mangifera indica . Soxhlet extraction was used as reference method, which yielded 57 mg/g in 5 h. Under optimal conditions such as microwave irradiation time 5 min, ammonium sulphate concentration 40% w/v, power 272 W, solute to solvent ratio 1:20, slurry to t -butanol ratio 1:1, soaking time 5 min and duty cycle 50%, the mangiferin yield obtained was 54 mg/g by microwave assisted three phase partitioning extraction (MTPP). Thus extraction method developed resulted into higher extraction yield in a shorter span, thereby making it an interesting alternative prior to down-stream processing.

  10. A novel method to augment extraction of mangiferin by application of microwave on three phase partitioning

    Directory of Open Access Journals (Sweden)

    Vrushali M. Kulkarni

    2015-06-01

    Full Text Available This work reports a novel approach where three phase partitioning (TPP was combined with microwave for extraction of mangiferin from leaves of Mangifera indica. Soxhlet extraction was used as reference method, which yielded 57 mg/g in 5 h. Under optimal conditions such as microwave irradiation time 5 min, ammonium sulphate concentration 40% w/v, power 272 W, solute to solvent ratio 1:20, slurry to t-butanol ratio 1:1, soaking time 5 min and duty cycle 50%, the mangiferin yield obtained was 54 mg/g by microwave assisted three phase partitioning extraction (MTPP. Thus extraction method developed resulted into higher extraction yield in a shorter span, thereby making it an interesting alternative prior to down-stream processing.

  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. New practical algorithm for modelling analyte recovery in bioanalytical reversed phase and mixed-mode solid phase extraction

    NARCIS (Netherlands)

    Hendriks, G.; Uges, D. R. A.; Franke, J. P.

    2008-01-01

    Solid phase extraction (SPE) is a widely used method for sample cleanup and sample concentration in bioanalytical sample preparation. A few methods to model the retention behaviour on SPE cartridges have been described previously but they are either not applicable to ionised species or are not

  13. Using a new ligand for solid phase extraction of mercury

    Energy Technology Data Exchange (ETDEWEB)

    Soleimani, Majid, E-mail: m-soleimani@hotmail.com [Department of Chemistry, Faculty of Sciences, Imam Khomeini International University (IKIU), Qazvin (Iran, Islamic Republic of); Mahmodi, Mohamad Saleh [Department of Chemistry, Faculty of Sciences, Imam Khomeini International University (IKIU), Qazvin (Iran, Islamic Republic of); Morsali, Ali [Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, Tehran (Iran, Islamic Republic of); Khani, Azam; Afshar, Majid Ghahraman [Department of Chemistry, Faculty of Sciences, Imam Khomeini International University (IKIU), Qazvin (Iran, Islamic Republic of)

    2011-05-15

    The octadecyl silica cartridge as a sorbent and 4-bpdb (1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene) as a ligand is a simple, rapid and reliable method for extracting and preconcentrating of Hg(II) in real samples prior to cold vapor atomic absorption spectrometry. Sample solutions were passed through a column at pH 4.5 then retained mercury ions on the column were eluted with minimal amount of 0.01 M nitric acid with 3 mL min{sup -1} flow rate. The effect of pH, type of buffer, flow rate of sample and eluent, type and volume of the eluent were investigated and optimized. At optimum effective parameters, concentration factor and detection limit were achieved 128 and 1.87 ng L{sup -1}, respectively.

  14. Using a new ligand for solid phase extraction of mercury

    International Nuclear Information System (INIS)

    Soleimani, Majid; Mahmodi, Mohamad Saleh; Morsali, Ali; Khani, Azam; Afshar, Majid Ghahraman

    2011-01-01

    The octadecyl silica cartridge as a sorbent and 4-bpdb (1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene) as a ligand is a simple, rapid and reliable method for extracting and preconcentrating of Hg(II) in real samples prior to cold vapor atomic absorption spectrometry. Sample solutions were passed through a column at pH 4.5 then retained mercury ions on the column were eluted with minimal amount of 0.01 M nitric acid with 3 mL min -1 flow rate. The effect of pH, type of buffer, flow rate of sample and eluent, type and volume of the eluent were investigated and optimized. At optimum effective parameters, concentration factor and detection limit were achieved 128 and 1.87 ng L -1 , respectively.

  15. 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

  16. Organic Extractives from Mentha spp. Honey and the Bee-Stomach: Methyl Syringate, Vomifoliol, Terpenediol I, Hotrienol and Other Compounds

    Directory of Open Access Journals (Sweden)

    Igor Jerković

    2010-04-01

    Full Text Available The GC and GC/MS analyses of the solvent organic extractive from the stomach of the bees, having collected Mentha spp. nectar, revealed the presence of methyl syringate (6.6%, terpendiol I (5.0% and vomifoliol (3.0% that can be attributed to the plant origin. Other major compounds from the bee-stomach were related to the composition of cuticular waxes and less to pheromones. Organic extractivesfrom Mentha spp. honey were obtained by solvent-free headspace solid-phase microextraction (HS-SPME and ultrasonic solvent extraction (USE and analyzed by GC and GC/MS. The major honey headspace compounds were hotrienol (31.1%–38.5%, 2-methoxy-4-methylphenol (0.5–6.0%, cis- and trans-linalool oxides (0.9–2.8%, linalool (1.0–3.1% and neroloxide (0.9–1.9%. Methyl syringate was the most abundant compound (38.3-56.2% in the honey solvent extractives followed by vomifoliol (7.0–26.6%. Comparison of the honey organic extractives with the corresponding bee-stomach extractive indicated that methyl syringate and vomofoliol were transferred to the honey while terpendiol I was partially transformed to hotrienol in ripened honey.

  17. Determination of Inorganic Arsenic in Natural Water by Solid Phase Extraction

    International Nuclear Information System (INIS)

    Nazaratul Ashifa Abdullah Salim; Amares Chatt, A.

    2011-01-01

    Arsenic (As) is generally known for its toxicity. The toxicity and mobility of As in the environment are dependent on the chemical forms or species in which it exists. Arsenic (III) and (V) are the most often determined species in environmental water, soil and sediment, while organic As species are common constituents of biological tissue and fluids. It is well known that inorganic As, such as arsenite (As(III)) and arsenate (As(V)) are more toxic than their organic counterparts. This study is conducted to investigate the separation of each As inorganic species using solid phase extraction (SPE) technique. The technique utilizes SPE column for selective retention of As species, followed by elution and measurement of eluted fractions by inductively coupled plasma mass spectrometry (ICP-MS) for total As. Several type of SPE columns namely strongly anion exchange (SAX), strongly cation exchange (SCX), weakly anion exchange (WAX) and weakly cation exchange (WCX) were tested using three different types of media including deionized water, succinic acid and acetic acid containing inorganic As species. The SPE technique is suitable for on-site separation and preservation of As species from water. (author)

  18. Coalescence of organic solutions in acid and metal extraction by tri-alkylamines

    International Nuclear Information System (INIS)

    Blain, J.

    1970-01-01

    The formation of two layers with tri-alkylammonium salts solutions in low polarity diluents could be explained on the basis of settling of micelles. Light scattering and viscosity measurements reveal that micelles size increases rather sharply before coalescence. The existence of micelles in the solution has been confirmed by ultracentrifuge experiments. The behaviour of these solutions, in general, is similar to that of colloidal soap solutions. The various parameters which promote third phase formation are: anion size in the order of Cl - ∼ Br - 3 4 - ; extraction of excess acid; metal cation size in the order of UO 2 ++ 4+ ∼ Th 4+ ; decreasing in the length of the n-alkyl chain in the alkyl-ammonium salts; decreasing in diluent polarity. The above phenomenon could be explained on the basis of the affinity between alkylammonium salts and organic solvent. The composition of the three phases is independent of the initial amine concentration for a fixed acid and metal concentration. This has been verified experimentally and is in conformity with phase rule. (author) [fr

  19. Importance of the hexagonal lipid phase in biological membrane organization.

    Science.gov (United States)

    Jouhet, Juliette

    2013-01-01

    Domains are present in every natural membrane. They are characterized by a distinctive protein and/or lipid composition. Their size is highly variable from the nano- to the micrometer scale. The domains confer specific properties to the membrane leading to original structure and function. The determinants leading to domain organization are therefore important but remain obscure. This review presents how the ability of lipids to organize into hexagonal II or lamellar phases can promote particular local structures within membranes. Since biological membranes are composed of a mixture of lipids, each with distinctive biophysical properties, lateral and transversal sorting of lipids can promote creation of domains inside the membrane through local modulation of the lipid phase. Lipid biophysical properties have been characterized for long based on in vitro analyses using non-natural lipid molecules; their re-examinations using natural lipids might open interesting perspectives on membrane architecture occurring in vivo in various cellular and physiological contexts.

  20. Thin film solar cells grown by organic vapor phase deposition

    Science.gov (United States)

    Yang, Fan

    Organic solar cells have the potential to provide low-cost photovoltaic devices as a clean and renewable energy resource. In this thesis, we focus on understanding the energy conversion process in organic solar cells, and improving the power conversion efficiencies via controlled growth of organic nanostructures. First, we explain the unique optical and electrical properties of organic materials used for photovoltaics, and the excitonic energy conversion process in donor-acceptor heterojunction solar cells that place several limiting factors of their power conversion efficiency. Then, strategies for improving exciton diffusion and carrier collection are analyzed using dynamical Monte Carlo models for several nanostructure morphologies. Organic vapor phase deposition is used for controlling materials crystallization and film morphology. We improve the exciton diffusion efficiency while maintaining good carrier conduction in a bulk heterojunction solar cell. Further efficiency improvement is obtained in a novel nanocrystalline network structure with a thick absorbing layer, leading to the demonstration of an organic solar cell with 4.6% efficiency. In addition, solar cells using simultaneously active heterojunctions with broad spectral response are presented. We also analyze the efficiency limits of single and multiple junction organic solar cells, and discuss the challenges facing their practical implementations.

  1. Transport of Liquid Phase Organic Solutes in Liquid Crystalline Membranes

    OpenAIRE

    Han, Sangil

    2010-01-01

    Porous cellulose nitrate membranes were impregnated with 8CB and PCH5 LCs (liquid crystals) and separations of solutes dissolved in aqueous phases were performed while monitoring solute concentration via UV-VIS spectrometry. The diffusing organic solutes, which consist of one aromatic ring and various functional groups, were selected to exclude molecular size effects on the diffusion and sorption. We studied the effects on solute transport of solute intra-molecular hydrogen bonding and so...

  2. Extraction and characterisation of aqueous organic acids from natural waters

    International Nuclear Information System (INIS)

    Smith, B.; Moody, P.M.; Higgo, J.J.W.

    1993-01-01

    Humic and fulvic acids were extracted from large volumes of groundwater associated with the Broubster and Needle's Eye natural analogue sites, and the BGS research site at Drigg in Cumbria. Extractions were performed by both batchwise extraction and radial flow chromatography using DEAE-cellulose. Retained humic substances were eluted using NaOH and separated into humic and fulvic components by acidification to pH 1. After separation the humic component was purified by repetitive precipitation and dissolution whilst the fulvic component was purified by absorption chromatography. The resulting humic substances were shown to be of high purity with respect to metallic elements, with less than 1% of available sites being occupied. During elution the association of trace elements with humic substances was monitored and a high degree of association between humic substances, U and the Rare Earth Elements was noted. (author)

  3. Tailoring phase-space in neutron beam extraction

    Energy Technology Data Exchange (ETDEWEB)

    Weichselbaumer, S. [Heinz Maier-Leibnitz Zentrum und Physik-Department E21, Technische Universität München, Lichtenbergstr. 1, D-85748 Garching (Germany); Brandl, G. [Heinz Maier-Leibnitz Zentrum und Physik-Department E21, Technische Universität München, Lichtenbergstr. 1, D-85748 Garching (Germany); Physik-Department E21, Technische Universität München, James-Franck-Str. 1, D-85748 Garching (Germany); Georgii, R., E-mail: Robert.Georgii@frm2.tum.de [Heinz Maier-Leibnitz Zentrum und Physik-Department E21, Technische Universität München, Lichtenbergstr. 1, D-85748 Garching (Germany); Physik-Department E21, Technische Universität München, James-Franck-Str. 1, D-85748 Garching (Germany); Stahn, J. [Laboratory for Neutron Scattering, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); Panzner, T. [Material Science and Simulations, Neutrons and Muons, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); Böni, P. [Physik-Department E21, Technische Universität München, James-Franck-Str. 1, D-85748 Garching (Germany)

    2015-09-01

    In view of the trend towards smaller samples and experiments under extreme conditions it is important to deliver small and homogeneous neutron beams to the sample area. For this purpose, elliptic and/or Montel mirrors are ideally suited as the phase space of the neutrons can be defined far away from the sample. Therefore, only the useful neutrons will arrive at the sample position leading to a very low background. We demonstrate the ease of designing neutron transport systems using simple numeric tools, which are verified using Monte-Carlo simulations that allow taking into account effects of gravity and finite beam size. It is shown that a significant part of the brilliance can be transferred from the moderator to the sample. Our results may have a serious impact on the design of instruments at spallation sources such as the European Spallation Source (ESS) in Lund, Sweden.

  4. Phase 0 and phase III transport in various organs: combined concept of phases in xenobiotic transport and metabolism.

    Science.gov (United States)

    Döring, Barbara; Petzinger, Ernst

    2014-08-01

    The historical phasing concept of drug metabolism and elimination was introduced to comprise the two phases of metabolism: phase I metabolism for oxidations, reductions and hydrolyses, and phase II metabolism for synthesis. With this concept, biological membrane barriers obstructing the accessibility of metabolism sites in the cells for drugs were not considered. The concept of two phases was extended to a concept of four phases when drug transporters were detected that guided drugs and drug metabolites in and out of the cells. In particular, water soluble or charged drugs are virtually not able to overcome the phospholipid membrane barrier. Drug transporters belong to two main clusters of transporter families: the solute carrier (SLC) families and the ATP binding cassette (ABC) carriers. The ABC transporters comprise seven families with about 20 carriers involved in drug transport. All of them operate as pumps at the expense of ATP splitting. Embedded in the former phase concept, the term "phase III" was introduced by Ishikawa in 1992 for drug export by ABC efflux pumps. SLC comprise 52 families, from which many carriers are drug uptake transporters. Later on, this uptake process was referred to as the "phase 0 transport" of drugs. Transporters for xenobiotics in man and animal are most expressed in liver, but they are also present in extra-hepatic tissues such as in the kidney, the adrenal gland and lung. This review deals with the function of drug carriers in various organs and their impact on drug metabolism and elimination.

  5. Solid-phase extraction clean-up of ciguatoxin-contaminated coral fish extracts for use in the mouse bioassay.

    Science.gov (United States)

    Wong, Chun Kwan; Hung, Patricia; Lee, Kellie L H; Kam, Kai Man

    2009-02-01

    Florisil solid-phase extraction (SPE) cartridges were used for purifying ciguatoxin (CTX)-contaminated coral fish extracts, with the aim of removing extracted lipid but retaining optimal level of CTXs in the purified fractions. The CTX-containing fraction (target fraction) in fish ether extract was isolated and purified by eluting through a commercially available Florisil cartridge with hexane-acetone-methanol solvent mixtures of increasing polarity (hexane-acetone (4:1, v/v) < acetone-methanol (7:3, v/v) < 100% methanol). Application of Florisil SPE using acetone-methanol (7:3, v/v) condition facilitated the separation of 4.2 +/- 0.4 mg (mean +/- standard error of the mean (SEM)) of purified target fraction from 20 mg ether extract with good retention of CTXs. The mouse bioassay was used to demonstrate that the average CTX recovery of the target fraction from CTX-spiked samples was 75.8% +/- 3.3%, which was significantly increased by 96.7% +/- 15% when compared with CTX recovery from ether extracts (44.8% +/- 5.2%) without performing SPE purification. Over 70% of non-target lipids were removed in which no CTX toxicity was found. Moreover, the target fractions of both CTX-spiked and naturally CTX-contaminated samples gave more prominent toxic responses of hypothermia and/or induced more rapid death of the mice. The use of acetone-methanol (7:3, v/v) condition in the elution could significantly improve overall recovery of CTXs, while minimizing the possible interferences of lipid matrix from co-extractants on mice.

  6. Hollow fiber-based liquid phase microextraction combined with high-performance liquid chromatography for extraction and determination of some antidepressant drugs in biological fluids.

    Science.gov (United States)

    Esrafili, Ali; Yamini, Yadollah; Shariati, Shahab

    2007-12-05

    The applicability of hollow fiber-based liquid phase microextraction (HF-LPME) was evaluated for the extraction and preconcentration of three antidepressant drugs (amitriptyline, imipramine and sertraline) prior to their determination by HPLC-UV. The target drugs were extracted from 11.0 mL of aqueous solution with pH 12.0 (source phase) into an organic extracting solvent (n-dodecane) impregnated in the pores of a hollow fiber and finally back extracted into 24 microL of aqueous solution located inside the lumen of the hollow fiber and adjusted to pH 2.1 using 0.1M of H3PO4 (receiving phase). The extraction was performed due to pH gradient between the inside and outside of the hollow fiber membrane. In order to obtain high extraction efficiency, the parameters affecting the HF-LPME including pH of the source and receiving phases, the type of organic phase, ionic strength and volume of the source phase, stirring rate and extraction time were studied and optimized. Under the optimized conditions, enrichment factors up to 300 were achieved and the relative standard deviation (R.S.D.%) of the method was in the range of 2-12%. The calibration curves were obtained in the range of 5-500 microg L(-1) with reasonable linearity (R2>0.998) and the limits of detection (LODs) ranged between 0.5 and 0.7 microg L(-1) (based on S/N=3). Finally, the applicability of the proposed method was evaluated by extraction and determination of the drugs in urine, plasma and tap water samples. The results indicated that hollow fiber microextraction method has excellent clean-up and high-preconcentration factor and can be served as a simple and sensitive method for monitoring of antidepressant drugs in the biological samples.

  7. Microwave plasma source having improved switching operation from plasma ignition phase to normal ion extraction phase

    International Nuclear Information System (INIS)

    Sakudo, N.; Abe, K.; Koike, H.; Okada, O.; Tokiguchi, K.

    1985-01-01

    In a microwave plasma source, a discharge space supplied with a microwave electric field is supplied with a DC magnetic field. A material to be ionized is introduced into the discharge space to produce plasma, whereby ions are extracted through an ion extracting system. A switch is provided for effecting through switching operation the change-over of the magnetic field applied to the discharge space from the intensity for the ignition of plasma to the intensity for ion extraction in succession to completion of the plasma ignition

  8. Phases for the value chain design and analysis in organizations

    Directory of Open Access Journals (Sweden)

    Emilio García Vega

    2015-09-01

    Full Text Available Value generation is a key issue in the management of organizations because it allows the consumer satisfaction, dynamic face of competition and reward the owners or shareholders. Its treatment reflects both the academic and the business world; i.e. teachers, researchers, executives and managers of the enterprises, whether they are micro, small, medium or large. Although there are different approaches to the subject, this paper will seek to develop an approach from a competitive perspective and through the value chain, as it can be considered a valid tool for designing and analysing how organizations generate value. Also, this research tries to present the evolution of the generation of value, based on the classical models of McKinsey & Co. and Michael Porter. Then some approaches and contributions to the value chain of different authors and from different perspectives are presented, so that we can count with a number of additional ideas, which the author considers relevant to face the value chain design and analysis. Finally, on the basis of capital contribution of the mentioned Harvard University Professor, a series of recommendations for the strategic application of the value chain in the management of today's organizations, which are organized into nine phases (phases for the design and analysis of the value chain are presented.

  9. The effect of vadose zone heterogeneities on vapor phase migration and aquifer contamination by volatile organics

    Energy Technology Data Exchange (ETDEWEB)

    Seneviratne, A.; Findikakis, A.N. [Bechtel Corporation, San Francisco, CA (United States)

    1995-03-01

    Organic vapors migrating through the vadose zone and inter-phase transfer can contribute to the contamination of larger portions of aquifers than estimated by accounting only for dissolved phase transport through the saturated zone. Proper understanding of vapor phase migration pathways is important for the characterization of the extent of both vadose zone and the saturated zone contamination. The multiphase simulation code T2VOC is used to numerically investigate the effect of heterogeneties on the vapor phase migration of chlorobenzene at a hypothetical site where a vapor extraction system is used to remove contaminants. Different stratigraphies consisting of alternate layers of high and low permeability materials with soil properties representative of gravel, sandy silt and clays are evaluated. The effect of the extent and continuity of low permeability zones on vapor migration is evaluated. Numerical simulations are carried out for different soil properties and different boundary conditions. T2VOC simulations with zones of higher permeability were made to assess the role of how such zones in providing enhanced migration pathways for organic vapors. Similarly, the effect of the degree of saturation of the porous medium on vapor migration was for a range of saturation values. Increased saturation reduces the pore volume of the medium available for vapor diffusion. Stratigraphic units with higher aqueous saturation can retard the vapor phase migration significantly.

  10. Efficacy of chitosan supported organic acaricide extract from Melia ...

    African Journals Online (AJOL)

    Conductometric titration, ultraviolet-visible ("UV-Vis") and Fourier transform infrared spectroscopy (FTIR) analysis were conducted with materials to evaluate the chitosan anchoring ability. In vitro test was used in engorged females for each treatment, which consisted of control, raw extract and three treatments with increasing ...

  11. Self-organizing networks for extracting jet features

    International Nuclear Information System (INIS)

    Loennblad, L.; Peterson, C.; Pi, H.; Roegnvaldsson, T.

    1991-01-01

    Self-organizing neural networks are briefly reviewed and compared with supervised learning algorithms like back-propagation. The power of self-organization networks is in their capability of displaying typical features in a transparent manner. This is successfully demonstrated with two applications from hadronic jet physics; hadronization model discrimination and separation of b.c. and light quarks. (orig.)

  12. Quaternary ammonium-functionalized silica sorbents for the solid-phase extraction of aromatic amines under normal phase conditions.

    Science.gov (United States)

    Vidal, Lorena; Robin, Orlane; Parshintsev, Jevgeni; Mikkola, Jyri-Pekka; Riekkola, Marja-Liisa

    2013-04-12

    Quaternary ammonium-functionalized silica materials were synthesized and applied for solid-phase extraction (SPE) of aromatic amines, which are classified as priority pollutants by US Environmental Protection Agency. Hexamethylenetetramine used for silica surface modification for the first time was employed as SPE sorbent under normal phase conditions. Hexaminium-functionalized silica demonstrated excellent extraction efficiencies for o-toluidine, 4-ethylaniline and quinoline (recoveries 101-107%), while for N,N-dimethylaniline and N-isopropylaniline recoveries were from low to moderate (14-46%). In addition, the suitability of 1-alkyl-3-(propyl-3-sulfonate) imidazolium-functionalized silica as SPE sorbent was tested under normal phase conditions. The recoveries achieved for the five aromatic amines ranged from 89 to 99%. The stability of the sorbent was evaluated during and after 150 extractions. Coefficients of variation between 4.5 and 10.2% proved a high stability of the synthesized sorbent. Elution was carried out using acetonitrile in the case of hexaminium-functionalized silica and water for 1-alkyl-3-(propyl-3-sulfonate) imidazolium-functionalized silica sorbent. After the extraction the analytes were separated and detected by liquid chromatography ultraviolet detection (LC-UV). The retention mechanism of the materials was primarily based on polar hydrogen bonding and π-π interactions. Comparison made with activated silica proved the quaternary ammonium-functionalized materials to offer different selectivity and better extraction efficiencies for aromatic amines. Finally, 1-alkyl-3-(propyl-3-sulfonate) imidazolium-functionalized silica sorbent was successfully tested for the extraction of wastewater and soil samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. Extraction of seawater-derived neodymium from different phases of deep sea sediments by selective leaching

    Science.gov (United States)

    Blaser, P.; Lippold, J. A.; Frank, N.; Gutjahr, M.; Böhm, E.

    2014-12-01

    In order to deduce reliable information about the interaction of the oceans with the climate system as a whole in the past, the reconstruction of water mass circulation is crucial. The analysis of seawater-derived neodymium isotopes (143Nd/144Nd, expressed as ɛNd) in marine sediments provides a unique proxy for deep water provenance in particular in the Atlantic [1]. The ɛNd signature and thus the mixing proportion of the local bottom water masses is archived in authigenic phases in the sediment. Obtaining seawater ɛNd from authigenic accretions bound to foraminiferal tests has lately become the preferred since most reliable method [2]. Attempts have also been made to extract the Nd-rich authigenic metal fraction by leaching it off the bulk sediment and thereby use this proxy with less effort, in the highest possible resolution and in sediments where foraminifera are not sufficiently present. However, often other sedimentary components are also leached in the process and contaminate the extracted Nd [3,4]. In this project several core-top and older sediments across the Atlantic have been leached in ten consecutive steps with either dilute buffered acetic acid or an acid-reductive solution. The leachates were analysed on their elemental and Nd isotope compositions, as well as rare earth element (REE) distributions. By graduating the total leaching procedure into smaller stages the results display which processes take place in the course of sediment leaching in the laboratory and which components of the sediment are most reactive. Thus, they help to better evaluate the quality of sediment leaches for ɛNd analysis. Clearly, organic calcite acts as a fast reacting buffer and at the point where its amount is sufficiently reduced the leaching of other components commences and the Nd concentration peaks. Corruption of the extracted ɛNd signal by non-authigenic sources in many cases occured early in the leaching sequence, indicating that only very cautious leaching

  14. Analysis of microcontaminants in aqueous samples by fully automated on-line solid-phase extraction-gas chromatography-mass selective detection.

    NARCIS (Netherlands)

    Louter, A.J.H.; van Beekvelt, C.A.; Cid Montanes, P.; Slobodník, J.; Vreuls, J.J.; Brinkman, U.A.T.

    1996-01-01

    The trace-level analysis of unknown organic pollutants in water requires the use of fast and sensitive methods which also provide structural information. In the present study, an on-line technique was used which combines sample preparation by means of solid-phase extraction (SPE) on a small

  15. A green deep eutectic solvent-based aqueous two-phase system for protein extracting.

    Science.gov (United States)

    Xu, Kaijia; Wang, Yuzhi; Huang, Yanhua; Li, Na; Wen, Qian

    2015-03-15

    As a new type of green solvent, deep eutectic solvent (DES) has been applied for the extraction of proteins with an aqueous two-phase system (ATPS) in this work. Four kinds of choline chloride (ChCl)-based DESs were synthesized to extract bovine serum albumin (BSA), and ChCl-glycerol was selected as the suitable extraction solvent. Single factor experiments have been done to investigate the effects of the extraction process, including the amount of DES, the concentration of salt, the mass of protein, the shaking time, the temperature and PH value. Experimental results show 98.16% of the BSA could be extracted into the DES-rich phase in a single-step extraction under the optimized conditions. A high extraction efficiency of 94.36% was achieved, while the conditions were applied to the extraction of trypsin (Try). Precision, repeatability and stability experiments were studied and the relative standard deviations (RSD) of the extraction efficiency were 0.4246% (n=3), 1.6057% (n=3) and 1.6132% (n=3), respectively. Conformation of BSA was not changed during the extraction process according to the investigation of UV-vis spectra, FT-IR spectra and CD spectra of BSA. The conductivity, dynamic light scattering (DLS) and transmission electron microscopy (TEM) were used to explore the mechanism of the extraction. It turned out that the formation of DES-protein aggregates play a significant role in the separation process. All the results suggest that ChCl-based DES-ATPS are supposed to have the potential to provide new possibilities in the separation of proteins. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Closure of the condensed-phase organic-nitrate reaction unreviewed safety question at Hanford site

    International Nuclear Information System (INIS)

    COWLEY, W.L.

    1999-01-01

    A discovery Unreviewed Safety Question (USQ) was declared on the underground waste storage tanks at the Hanford Site in May 1996. The USQ was for condensed-phase organic-nitrate reactions (sometimes called organic complexant reactions) in the tanks. This paper outlines the steps taken to close the USQ, and resolve the related safety issue. Several processes were used at the Hanford Site to extract and/or process plutonium. These processes resulted in organic complexants (for chelating multivalent cations) and organic extraction solvents being sent to the underground waste storage tanks. This paper addresses the organic complexant hazard. The organic complexants are in waste matrices that include inert material, diluents, and potential oxidizers. In the presence of oxidizing material, the complexant salts can be made to react exothermically by heating to high temperatures or by applying an external ignition source of sufficient energy. The first organic complexant hazard assessments focused on determining whether a hulk runaway reaction could occur, similar to the 1957 accident at Kyshtm (a reprocessing plant in the former U.S.S.R.). Early analyses (1977 through 1994) examined organic-nitrate reaction onset temperatures and concluded that a bulk runaway reaction could not occur at the Hanford Site because tank temperatures were well below that necessary for bulk runaway. Therefore, it was believed that organic-nitrate reactions were adequately described in the then current Authorization Basis (AB). Subsequent studies examined a different accident scenario, propagation resulting from an external ignition source (e.g., lightning or welding slag) that initiates a combustion front that propagates through the organic waste. A USQ evaluation determined that localized high energy ignition sources were credible, and that point source ignition of organic complexant waste was not adequately addressed i n the then existing AB. Consequently, the USQ was declared on the

  17. Phase distribution of ecologically controlled chemical elements in production of extraction phosphoric acid

    International Nuclear Information System (INIS)

    Kazak, V.G.; Agnelov, A.I.; Zajtsev, P.M.

    1995-01-01

    Content of 16 ecologically controlled chemical element (among them Cd, Sr, Th, U, V, Y) in solid and liquid phases of extraction phosphorus acid (EPA) production is determined. These elements are recommended to control by Scientific research institute of human ecology and environment to establish their extraction coefficients to phosphogypsum and EPA and optimal variant of production of ecologically sate phosphorus fertilizers. X-ray fluorescent, atomic-absorption and polarographic methods are used for analysis these elements

  18. Characterization of organic matrix extracted from fresh water pearls

    International Nuclear Information System (INIS)

    Ma Yufei; Gao Yonghua; Feng Qingling

    2011-01-01

    Aragonite pearl and vaterite pearl from cultured Hyriopsis cumingii in Zhuji (Zhejiang province, China) were chosen for the study. The matrix proteins were extracted using water and weak acid, and classified as water soluble matrix (WSM), acid soluble matrix (ASM) and acid insoluble matrix (AIM). The proteins from both pearls were characterized by sodium dodecyl sulphate-polyacrylamide gel electrophoresis (SDS-PAGE), X-ray diffraction (XRD) and Fourier transformation infrared spectra (FTIR). The results showed that, AIM of aragonite pearl and vaterite pearl had an ordered structure of α-helix. ASM conformations of these two pearls were different from each other. WSM differed the most between these two pearls. - Research Highlights: → We use a specific method for extracting matrix proteins from aragonite pearl and vaterite pearl respectively. → The matrix proteins are extracted by water and weak acid, and classified as water soluble matrix (WSM), acid soluble matrix (ASM) and acid insoluble matrix (AIM). → AIM of aragonite pearl and vaterite pearl have an ordered structure. ASM conformations of the two pearls are different from each other. WSM differ the most between these two pearls.

  19. Cogeneration of biodiesel and nontoxic cottonseed meal from cottonseed processed by two-phase solvent extraction

    Energy Technology Data Exchange (ETDEWEB)

    Qian Junfeng, E-mail: qianjunfeng80@126.co [Jiangsu Provincial Key Laboratory of Fine Petrochemical Engineering, Jiangsu Polytechnic University, Changzhou 213016 (China) and College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing 210009 (China); Yun Zhi; Shi Haixian [College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing 210009 (China)

    2010-12-15

    In the present work, the preparation of biodiesel from cottonseed oil produced by two-phase solvent extraction (TSE) was studied. The experimental results of TSE process of cottonseed showed that the optimal extraction conditions were 30 g samples, 240 mL extraction solvent mixture and methanol/petroleum ether volume ratio 60:40, extraction temperature 30 deg. C, extraction time 30 min. Under the extraction conditions, the extraction rate of cottonseed oil could achieve 98.3%, the free fatty acid (FFA) and water contents of cottonseed oil were reduced to 0.20% and 0.037%, respectively, which met the requirement of alkali-catalyzed transesterification. The free gossypol (FG) content in cottonseed meal produced from two-phase solvent extraction could reduce to 0.014% which was far below the FAO standard. And the nontoxic cottonseed meal could be used as animal protein feed resources. After the TSE process of cottonseed, the investigations were carried out on transesterification of methanol with oil-petroleum ether solution coming from TSE process in the presence of sodium hydroxide (CaO) as the solid base catalyst. The influences of weight ratio of petroleum ether to cottonseed oil, reaction temperature, molar ratio of methanol to oil, alkali catalyst amount and reaction time on cottonseed oil conversion were respectively investigated by mono-factor experiments. The conversion of cottonseed oil into fatty acid methyl ester (FAME) could achieve 98.6% with 3:1 petroleum ether/oil weight ratio, 65 deg. C reaction temperature, 9:1 methanol/oil mole ratio, 4% (catalyst/oil weight ratio, w/w) solid base catalyst amount and 3 h reaction time. The properties of FAME product prepared from cottonseed oil produced by two-phase solvent extraction met the ASTM specifications for biodiesel.

  20. Cogeneration of biodiesel and nontoxic cottonseed meal from cottonseed processed by two-phase solvent extraction

    Energy Technology Data Exchange (ETDEWEB)

    Qian, Junfeng [Jiangsu Provincial Key Laboratory of Fine Petrochemical Engineering, Jiangsu Polytechnic University, Changzhou 213016 (China); College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing 210009 (China); Yun, Zhi; Shi, Haixian [College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing 210009 (China)

    2010-12-15

    In the present work, the preparation of biodiesel from cottonseed oil produced by two-phase solvent extraction (TSE) was studied. The experimental results of TSE process of cottonseed showed that the optimal extraction conditions were 30 g samples, 240 mL extraction solvent mixture and methanol/petroleum ether volume ratio 60:40, extraction temperature 30 C, extraction time 30 min. Under the extraction conditions, the extraction rate of cottonseed oil could achieve 98.3%, the free fatty acid (FFA) and water contents of cottonseed oil were reduced to 0.20% and 0.037%, respectively, which met the requirement of alkali-catalyzed transesterification. The free gossypol (FG) content in cottonseed meal produced from two-phase solvent extraction could reduce to 0.014% which was far below the FAO standard. And the nontoxic cottonseed meal could be used as animal protein feed resources. After the TSE process of cottonseed, the investigations were carried out on transesterification of methanol with oil-petroleum ether solution coming from TSE process in the presence of sodium hydroxide (CaO) as the solid base catalyst. The influences of weight ratio of petroleum ether to cottonseed oil, reaction temperature, molar ratio of methanol to oil, alkali catalyst amount and reaction time on cottonseed oil conversion were respectively investigated by mono-factor experiments. The conversion of cottonseed oil into fatty acid methyl ester (FAME) could achieve 98.6% with 3:1 petroleum ether/oil weight ratio, 65 C reaction temperature, 9:1 methanol/oil mole ratio, 4% (catalyst/oil weight ratio, w/w) solid base catalyst amount and 3 h reaction time. The properties of FAME product prepared from cottonseed oil produced by two-phase solvent extraction met the ASTM specifications for biodiesel. (author)

  1. Extraction of Oxytetracycline Hydrochloride in Aqueous Two-phase System of Acetone and Ammonium Sulfate

    International Nuclear Information System (INIS)

    Han, J.

    2013-01-01

    Summary: Aqueous two-phase system (ATPS) is an efficient implement for separation of various substrates, and extracted by an aqueous two-phase system has been successful ly applied in the downstream processing of various biological compounds. In this research, the extraction of oxytetracycline hydrochloride (OTC-HCl) was carried out in an aqueous two-phase system containing acetone and ammonium sulfate solution, which partitioned the antibiotic to the upper phase. The effects of some parameters on the extraction efficiency of OTC-HCl were studied in detail, including temperature, the volume of acetone, the pH value of ammonium sulfate solution, the concentrations of (NH/sub 4/)/sub 2/ SO/sub 4/ and OTC-HCl. The results showed that the volume of acetone, the pH value of ammonium sulfate solution and the concentration of OTC-HCl in feed had significant effects on the extraction efficiency of OTC-HCl, but the effects of temperature on the extraction of OTC-HCl was not obvious. (author)

  2. Extraction of Oxytetracycline Hydrochloride in Aqueous Two-phase System of Acetone and Ammonium Sulfate

    Energy Technology Data Exchange (ETDEWEB)

    Han, J. [Jiangsu Univ., Zhenjiang (China). Dept. of Food and Biological Engineering

    2013-02-15

    Summary: Aqueous two-phase system (ATPS) is an efficient implement for separation of various substrates, and extracted by an aqueous two-phase system has been successful ly applied in the downstream processing of various biological compounds. In this research, the extraction of oxytetracycline hydrochloride (OTC-HCl) was carried out in an aqueous two-phase system containing acetone and ammonium sulfate solution, which partitioned the antibiotic to the upper phase. The effects of some parameters on the extraction efficiency of OTC-HCl were studied in detail, including temperature, the volume of acetone, the pH value of ammonium sulfate solution, the concentrations of (NH/sub 4/)/sub 2/ SO/sub 4/ and OTC-HCl. The results showed that the volume of acetone, the pH value of ammonium sulfate solution and the concentration of OTC-HCl in feed had significant effects on the extraction efficiency of OTC-HCl, but the effects of temperature on the extraction of OTC-HCl was not obvious. (author)

  3. A three-phase microfluidic chip for rapid sample clean-up of alkaloids from plant extracts

    NARCIS (Netherlands)

    Tetala, K.K.R.; Swarts, J.W.; Chen, B.; Janssen, A.E.M.; Beek, van T.A.

    2009-01-01

    A three-phase microchip was developed for the rapid and efficient small-scale purification of alkaloids from plant extracts. As part of the development of such a three-phase microchip, first a two-phase microchip with two channels (3.2 cm and 9.3 cm) was used to study the extraction efficiency of

  4. Solid-phase extraction and determination of trace elements in environmental samples using naphthalene adsorbent

    International Nuclear Information System (INIS)

    Pourreza, N.

    2004-01-01

    Naphthalene co-precipitated with quaternary ammonium salt such as tetraoctyl ammonium bromide and methyltrioctyl ammonium chloride have been used as adsorbent for solid phase extraction of metal ions such as Hg, Cd and Fe. The metal ions are retained on the adsorbent in a column as their complexes with suitable ligands and eluted by an eluent before instrumental measurements. The optimization of the procedures for solid phase extraction and consequent determination of trace elements and application to environmental samples especially water samples will be discussed. (author)

  5. Extracting scattering phase shifts in higher partial waves from lattice QCD calculations

    Energy Technology Data Exchange (ETDEWEB)

    Luu, Thomas; Savage, Martin J.

    2011-06-01

    Lüscher’s method is routinely used to determine meson-meson, meson-baryon, and baryon-baryon s-wave scattering amplitudes below inelastic thresholds from lattice QCD calculations—presently at unphysical light-quark masses. In this work we review the formalism and develop the requisite expressions to extract phase shifts describing meson-meson scattering in partial waves with angular momentum l≤6 and l=9. The implications of the underlying cubic symmetry, and strategies for extracting the phase shifts from lattice QCD calculations, are presented, along with a discussion of the signal-to-noise problem that afflicts the higher partial waves.

  6. Effect of Organic Solvents on Microalgae Growth, Metabolism and Industrial Bioproduct Extraction: A Review.

    Science.gov (United States)

    Miazek, Krystian; Kratky, Lukas; Sulc, Radek; Jirout, Tomas; Aguedo, Mario; Richel, Aurore; Goffin, Dorothee

    2017-07-04

    In this review, the effect of organic solvents on microalgae cultures from molecular to industrial scale is presented. Traditional organic solvents and solvents of new generation-ionic liquids (ILs), are considered. Alterations in microalgal cell metabolism and synthesis of target products (pigments, proteins, lipids), as a result of exposure to organic solvents, are summarized. Applications of organic solvents as a carbon source for microalgal growth and production of target molecules are discussed. Possible implementation of various industrial effluents containing organic solvents into microalgal cultivation media, is evaluated. The effect of organic solvents on extraction of target compounds from microalgae is also considered. Techniques for lipid and carotenoid extraction from viable microalgal biomass (milking methods) and dead microalgal biomass (classical methods) are depicted. Moreover, the economic survey of lipid and carotenoid extraction from microalgae biomass, by means of different techniques and solvents, is conducted.

  7. Sorption of cesium, strontium, and technetium onto organic-extracted shales

    International Nuclear Information System (INIS)

    Ho, P.C.

    1992-01-01

    The sorption of Cs(I), Sr(II), and Tc(VII) onto organic-extracted shales from synthetic brine groundwaters and from 0.03-M NaHCO 3 solution under oxid conditions at room temperature has been studied. The shale samples used in this study were Pumpkin Valley, Upper Dowelltown, Pierre and Green River Formation Shales. The organic content of these shales ranges from less than 2 wt% to 13 wt%. Soxhlet extraction with chloroform and a mixture of chloroform and methanol removed 0.07 to 5.9 wt% of the total organic matter from these shales. In comparison with the results of sorption of these three metal ions onto the corresponding untreated shales, it was observed that there were moderate to significant sorption decreases of Cs(I) and Sr(II) on all four organic-extracted shale samples and moderate sorption decrease of Tc(VII) on the organic-extracted Pumpkin Valley, Pierre, and Green River Shale samples, but only moderate sorption increases of Tc(VII) on the organic-extracted Upper Dowelltown Shale samples from the brine groundwaters. Nevertheless, sorption of Cs(I), Sr(II), and Tc(VII) on all four organic-extracted shale samples from the bicarbonate solution in most cases did not show a consistent pattern. (orig.)

  8. Membrane solid-phase extraction: Field application for isolation of polycyclic aromatic hydrocarbons from water samples

    International Nuclear Information System (INIS)

    Furlong, E.T.; Koleis, J.C.; Gates, P.M.

    1995-01-01

    Solid-phase extraction (SPE) membranes (M-SPE) were used to isolate microgram-per-liter to nanogram-per-liter quantities of polycyclic aromatic hydrocarbons (PAH) in 4- to 8-liter ground-water samples from a crude-oil-contaminated ground-water site near Bemidji, Minnesota. The M-SPE method was evaluated (1) under laboratory conditions using reagent water fortified with individual PAH at 1.23 micrograms per liter, and (2) at the Bemidji site. At the site, ground-water samples were processed and PAH isolated using a M-SPE system connected directly to the well pump. Following sample isolation, all M-SPE samples were extracted using dichloromethane and analyzed by gas chromatography-mass spectrometry with selected-ion monitoring. Operationally, the M-SPE method provided a simple means to isolate PAH on site at the wellhead, particularly for anoxic water samples. Acceptable recoveries, ranging from 56 to over 100 percent, were observed for lower molecular weight PAH (naphthalene to pyrene) using the M-SPE method. Recoveries using M-SPE were somewhat lower, but reproducible, for higher molecular weight PAH (chrysene to benzo[ghi]perylene), ranging from 18 to 56 percent. M-SPE provides the capability to collect and field isolate PAH from a sufficiently large number of samples to identify environmental chemical processes occurring at individual compound concentrations of 50 to 1,200 nanograms per liter. Using M-SPE, the potential for facilitated transport of PAH by in situ-derived dissolved organic carbon (DOC) was evaluated at the site. Plots comparing DOC and PAH concentrations indicate that PAH concentrations increase exponentially with linear increases in DOC concentrations

  9. Estimation of Partition Coefficients of Benzene, Toluene, Ethylbenzene, and ρ-Xylene by Consecutive Extraction with Solid Phase Microextraction

    International Nuclear Information System (INIS)

    Eom, In Yong

    2011-01-01

    The results show that the partition coefficients of the BTEX compound can be estimated using the SPME method under the consecutive extraction mode. The proposed technique is much simpler than previously reported methods. Its novelty is that it eliminated the calibration step in the GC/FID, i. e., liquid injection method. The use of the autosampler for the SPME fiber can facilitate the adoption of consecutive extractions; thus, it allows estimation of the partition coefficients of various analytes. Recently, GC/MS has increasingly been used in analytical laboratories; this may facilitate the identification of an unknown analyte as well as the computation of the corresponding partition coefficients with the proposed method. It is very important to use partition coefficients of organic pollutants to predict their fate in the environment. A liquid-liquid extraction technique was used to determine the partition coefficients of organic compounds between water and organic solvent. The concentration of the target compounds must be determined after equilibrium is established between the two phases. The partition coefficients can be estimated using the capacity factors of HPLC and GC

  10. Application of extraction replicas and analytical electron microscopy to precipitate phase studies

    International Nuclear Information System (INIS)

    Kenik, E.A.; Maziasz, P.J.

    1984-01-01

    Extraction replicas provide a powerful extension of AEM techniques for analysis of fine precipitates. In many cases, replicas allow more accurate analyses to be performed and, in some cases, allow unique analyses which cannot be performed in-foil. However, there are limitations to the use of extraction replicas in AEM, of which the analyst must be aware. Many can be eliminated by careful preparation. Often, combined AEM studies of precipitates in-foil and on extraction replicas provide complementary and corroborative information for the fullest analysis of precipitate phases

  11. Extracting surface waves, hum and normal modes: time-scale phase-weighted stack and beyond

    Science.gov (United States)

    Ventosa, Sergi; Schimmel, Martin; Stutzmann, Eleonore

    2017-10-01

    Stacks of ambient noise correlations are routinely used to extract empirical Green's functions (EGFs) between station pairs. The time-frequency phase-weighted stack (tf-PWS) is a physically intuitive nonlinear denoising method that uses the phase coherence to improve EGF convergence when the performance of conventional linear averaging methods is not sufficient. The high computational cost of a continuous approach to the time-frequency transformation is currently a main limitation in ambient noise studies. We introduce the time-scale phase-weighted stack (ts-PWS) as an alternative extension of the phase-weighted stack that uses complex frames of wavelets to build a time-frequency representation that is much more efficient and fast to compute and that preserve the performance and flexibility of the tf-PWS. In addition, we propose two strategies: the unbiased phase coherence and the two-stage ts-PWS methods to further improve noise attenuation, quality of the extracted signals and convergence speed. We demonstrate that these approaches enable to extract minor- and major-arc Rayleigh waves (up to the sixth Rayleigh wave train) from many years of data from the GEOSCOPE global network. Finally we also show that fundamental spheroidal modes can be extracted from these EGF.

  12. Recent Application of Solid Phase Based Techniques for Extraction and Preconcentration of Cyanotoxins in Environmental Matrices.

    Science.gov (United States)

    Mashile, Geaneth Pertunia; Nomngongo, Philiswa N

    2017-03-04

    Cyanotoxins are toxic and are found in eutrophic, municipal, and residential water supplies. For this reason, their occurrence in drinking water systems has become a global concern. Therefore, monitoring, control, risk assessment, and prevention of these contaminants in the environmental bodies are important subjects associated with public health. Thus, rapid, sensitive, selective, simple, and accurate analytical methods for the identification and determination of cyanotoxins are required. In this paper, the sampling methodologies and applications of solid phase-based sample preparation methods for the determination of cyanotoxins in environmental matrices are reviewed. The sample preparation techniques mainly include solid phase micro-extraction (SPME), solid phase extraction (SPE), and solid phase adsorption toxin tracking technology (SPATT). In addition, advantages and disadvantages and future prospects of these methods have been discussed.

  13. Analysis of small molecular phase in coal involved in pyrolysis and solvent extraction by PGC

    Energy Technology Data Exchange (ETDEWEB)

    Jie Feng; Wen-Ying Li; Ke-Chang Xie [Taiyuan University of Technology, Taiyuan (China). Key Laboratory of Coal Science and Technology

    2004-06-01

    The small molecular phase, which strongly affects coal's reactivity, is the main part of the structure unit in coal. At present, its composition and structure features have not been clearly understood. In this paper, a flash pyrolysis technique with on-line GC (PGC) was used to investigate the properties of the small molecular phase from six kinds of rank coal in China. Experiments were divided into two parts: one is PGC of parent coal; another is PGC of coal extracts from NMP + CS{sub 2} (75:1) solvent extraction at 373 K. Results show that the small molecular phase mainly consists of C12-C16 compounds that could be integrally released when the heating rate was greater than 10 K/ms and the final pyrolysis temperature was 1373 K; other compounds may be the products of decomposition and polymerization from this small molecular phase during pyrolysis. 13 refs., 7 figs., 1 tab.

  14. Organic Rankine Kilowatt Isotope Power System. Final phase I report

    International Nuclear Information System (INIS)

    1978-01-01

    On 1 August 1975 under Department of Energy Contract EN-77-C-02-4299, Sundstrand Energy Systems commenced development of a Kilowatt Isotope Power System (KIPS) directed toward satisfying the higher power requirements of satellites of the 1980s and beyond. The KIPS is a 238 PuO 2 fueled organic Rankine cycle turbine power system which will provide design output power in the range of 500 to 2000 W/sub (e)/ with a minimum of system changes. The principal objectives of the Phase 1 development effort were to: conceptually design a flight system; design a Ground Demonstration System (GDS) that is prototypic of the flight system in order to prove the feasibility of the flight system design; fabricate and assemble the GDS; and performance and endurance test the GDS using electric heaters in lieu of the isotope heat source. Results of the work performed under the Phase 1 contract to 1 July 1978 are presented

  15. Extractability of water-soluble soil organic matter as monitored by spectroscopic and chromatographic analyses.

    Science.gov (United States)

    Nkhili, Ezzhora; Guyot, Ghislain; Vassal, Nathalie; Richard, Claire

    2012-07-01

    Cold and hot water processes have been intensively used to recover soil organic matter, but the effect of extraction conditions on the composition of the extracts were not well investigated. Our objective was to optimize the extraction conditions (time and temperature) to increase the extracted carbon efficiency while minimizing the possible alteration of water extractable organic matter of soil (WEOM). WEOM were extracted at 20°C, 60°C, or 80°C for 24 h, 10-60 min, and 20 min, respectively. The different processes were compared in terms of pH of suspensions, yield of organic carbon, spectroscopic properties (ultraviolet-visible absorption and fluorescence), and by chromatographic analyses. For extraction at 60°C, the time 30 min was optimal in terms of yield of organic carbon extracted and concentration of absorbing and fluorescent species. The comparison of WEOM 20°C, 24 h; 60°C, 30 min; and 80°C, 20 min highlighted significant differences. The content of total organic carbon, the value of specific ultraviolet absorbance (SUVA(254)), the absorbance ratio at 254 and 365 nm (E (2)/E (3)), and the humification index varied in the order: WEOM (20°C, 24 h) < WEOM (80°C, 20 min) < WEOM (60°C, 30 min). The three WEOM contained common fluorophores associated with simple aromatic structures and/or fulvic-like and common peaks of distinct polarity as detected by ultra performance liquid chromatography. For the soil chosen, extraction at 60°C for 30 min is the best procedure for enrichment in organic chemicals and minimal alteration of the organic matter.

  16. Disinfection of vegetable seed by treatment with essential oils, organic acids and plant extract

    NARCIS (Netherlands)

    Wolf, van der J.M.; Birnbaum, Y.E.; Zouwen, van der P.S.; Groot, S.P.C.

    2008-01-01

    Various essential oils, organic acids, Biosept, (grapefruit extract), Tillecur and extracts of stinging nettle and golden rod were tested for their antimicrobial properties in order to disinfect vegetable seed. In in vitro assays, thyme oil, oregano oil, cinnamon oil, clove oil and Biosept had the

  17. Dynamics of dissolved and extractable organic nitrogen upon soil amendment with crop residues

    NARCIS (Netherlands)

    Ros, G.H.; Hoffland, E.

    2010-01-01

    Dissolved organic nitrogen (DON) is increasingly recognized as a pivotal pool in the soil nitrogen (N) cycle. Numerous devices and sampling procedures have been used to estimate its size, varying from in situ collection of soil solution to extraction of dried soil with salt solutions. Extractable

  18. HPLC WITH SOLID PHASE EXTRACTION FOR IDENTIFICATION AND DIAGNOSIS OF ORGANOPHOSPHOROUS POISONING IN GOATS

    Directory of Open Access Journals (Sweden)

    S. Manna

    2014-12-01

    Full Text Available High performance liquid chromatographic determination of organophosphorous compound has been done by reverse phase chromatography in goats. The goats were dying showing the symptoms of organophosphorous poisoning. The viscera and stomach contents sample were received from Project Co-Ordinator, Animal Disease Research Institute, Phulnakhara, Cuttack, Orissa. The analysis of samples by HPLC with UV detector after cleaning up in Solid Phase Extraction (SPE revealed presence of malathion that was later quantified.

  19. Solid-phase extraction and HPLC assay of nicotine and cotinine in plasma and brain.

    Science.gov (United States)

    Dawson, Ralph; Messina, S M; Stokes, C; Salyani, S; Alcalay, N; De Fiebre, N C; De Fiebre, C M

    2002-01-01

    The aim of this study was to develop a simple and reliable assay for nicotine (NIC) and its major metabolite, cotinine (COT), in plasma and brain. A method was developed that uses an extraction method compatible with reverse-phase high-performance liquid chromatography (HPLC) separation and ultraviolet (UV) detection. Sequential solid-phase extraction on silica columns followed by extraction using octadecyl (C18) columns resulted in mean percent recovery (n = 5) of 51 +/- 5, 64 +/- 10, and 52 +/- 10% for NIC, COT, and phenylimidazole (PI), respectively, in spiked 1-mL serum samples. Recovery (mean +/- SEM) of the internal standard (PI) from spiked samples of nicotine-injected rats averaged 64.1 +/- 1.5% (n = 138) from plasma, and 20.7+/-0.8% (n = 128) from brain. The limits of detection of NIC in plasma samples were approximately 8 ng per mL, and of COT, 13.6 ng per mL. Further optimization of our extraction method, using slower flow rates and solid-phase extraction on silica columns, followed by C18 column extraction, yielded somewhat better recoveries (38 +/-3%) for 1-mL brain homogenates. Interassay precision (coefficient of variation) was determined on the basis of daily calibrations for 2 months and was found to be 7%, 9%, and 9% for NIC, COT, and PI, respectively, whereas intra-assay variability was 3.9% for both NIC and COT. Limited studies were performed on analytical columns for comparison of retention, resolution, asymmetry, and column capacity. We concluded that a simple two-step solid-phase extraction method, coupled with HPLC separation and UV detection, can be used routinely to measure NIC and COT in biological fluids and tissues.

  20. Phase extracting algorithms analysis in the white-light spectral interferometry

    Science.gov (United States)

    Guo, Tong; Li, Bingtong; Li, Minghui; Chen, Jinping; Fu, Xing; Hu, Xiaotang

    2018-01-01

    As an optical testing method, white-light spectral interferometry has the characteristics of non-contact, high precision. The phase information can be obtained by analyzing the spectral interference signal of the tested sample, and then the absolute distance is calculated. Fourier transform method, temporal phase-shifting method, spatial phase-shifting method and envelope method can be used to extract the phase information of the spectral interference signal. In this paper, the performance of four methods to extract phase information is simulated and analyzed by using the ideal spectral interference signal. It turns out that temporal phase-shifting method has the performance of high precision, the results of Fourier transform method and envelop method are distorted at the edge of the signal, and spatial phase-shifting method has the worst precision. Adding different levels of white noise to the ideal signal, temporal phase-shifting method is most accurate, while Fourier transform method and envelope method are relatively poor. Finally, the absolute distance measurement experiment is carried out on the constructed test system, and the results are consistent with the simulation ones.

  1. Partitioning of Nanoparticles into Organic Phases and Model Cells

    Energy Technology Data Exchange (ETDEWEB)

    Posner, J.D.; Westerhoff, P.; Hou, W-C.

    2011-08-25

    There is a recognized need to understand and predict the fate, transport and bioavailability of engineered nanoparticles (ENPs) in aquatic and soil ecosystems. Recent research focuses on either collection of empirical data (e.g., removal of a specific NP through water or soil matrices under variable experimental conditions) or precise NP characterization (e.g. size, degree of aggregation, morphology, zeta potential, purity, surface chemistry, and stability). However, it is almost impossible to transition from these precise measurements to models suitable to assess the NP behavior in the environment with complex and heterogeneous matrices. For decades, the USEPA has developed and applies basic partitioning parameters (e.g., octanol-water partition coefficients) and models (e.g., EPI Suite, ECOSAR) to predict the environmental fate, bioavailability, and toxicity of organic pollutants (e.g., pesticides, hydrocarbons, etc.). In this project we have investigated the hypothesis that NP partition coefficients between water and organic phases (octanol or lipid bilayer) is highly dependent on their physiochemical properties, aggregation, and presence of natural constituents in aquatic environments (salts, natural organic matter), which may impact their partitioning into biological matrices (bioaccumulation) and human exposure (bioavailability) as well as the eventual usage in modeling the fate and bioavailability of ENPs. In this report, we use the terminology "partitioning" to operationally define the fraction of ENPs distributed among different phases. The mechanisms leading to this partitioning probably involve both chemical force interactions (hydrophobic association, hydrogen bonding, ligand exchange, etc.) and physical forces that bring the ENPs in close contact with the phase interfaces (diffusion, electrostatic interactions, mixing turbulence, etc.). Our work focuses on partitioning, but also provides insight into the relative behavior of ENPs as either "more like

  2. Molecular imprinting solid phase extraction for selective detection of methidathion in olive oil.

    Science.gov (United States)

    Bakas, Idriss; Oujji, Najwa Ben; Moczko, Ewa; Istamboulie, Georges; Piletsky, Sergey; Piletska, Elena; Ait-Ichou, Ihya; Ait-Addi, Elhabib; Noguer, Thierry; Rouillon, Régis

    2012-07-13

    A specific adsorbent for extraction of methidathion from olive oil was developed. The design of the molecularly imprinted polymer (MIP) was based on the results of the computational screening of the library of polymerisable functional monomers. MIP was prepared by thermal polymerisation using N,N'-methylene bisacrylamide (MBAA) as a functional monomer and ethylene glycol dimethacrylate (EGDMA) as a cross-linker. The polymers based on the itaconic acid (IA), methacrylic acid (MAA) and 2-(trifluoromethyl)acryl acid (TFMAA) functional monomers and one control polymer which was made without functional monomers with cross-linker EGDMA were also synthesised and tested. The performance of each polymer was compared using corresponding imprinting factor. As it was predicted by molecular modelling the best results were obtained for the MIP prepared with MBAA. The obtained MIP was optimised in solid-phase extraction coupled with high performance liquid chromatography (MISPE-HPLC-UV) and tested for the rapid screening of methidathion in olive oil. The proposed method allowed the efficient extraction of methidathion for concentrations ranging from 0.1 to 9 mg L(-1) (r(2)=0.996). The limits of detection (LOD) and quantification (LOQ) in olive oil were 0.02 mg L(-1) and 0.1 mg L(-1), respectively. MIPs extraction was much more effective than traditional C18 reverse-phase solid phase extraction. Copyright © 2012 Elsevier B.V. All rights reserved.

  3. Simultaneous solid phase extraction of cobalt, strontium and cesium from liquid radioactive waste using microcrystalline naphthalene

    International Nuclear Information System (INIS)

    Hamed, Mostafa Mohamed; Attallah, Mohamed Fathy; Metwally, Sayed Sayed

    2014-01-01

    Most of the procedures developed for the extraction of cobalt, strontium and cesium by solid phase extraction do not employ simultaneous extraction of them. In this study, rapid simultaneous removal of Co 2+ , Sr 2+ and Cs + on microcrystalline naphthalene as solid-phase extractant was investigated. These ions were allowed to form chelates with oxine and then adsorbed on freshly microcrystalline naphthalene from aqueous solutions. The solid phase extraction procedure (SPE) was optimized by using model solution containing Co 2+ , Sr 2+ and Cs + in batch system. The effects of different parameters such as variation in pH, reagent concentration, standing time, naphthalene solution concentration and contact time on the simultaneous removal of these ions was studied. The obtained results indicated that, sorption was found to be rapid, and the percentage removal of Co 2+ , Sr 2+ and Cs + was found to be 98, 79 and 68% within 10 min, respectively. The kinetics of the sorption process was investigated to understand the kinetic characteristics of sorption of metal chelates onto microcrystalline naphthalene. The developed procedure has been successfully applied to the removal and recovery of 60 Co and 134 Cs from liquid radioactive waste. The parameters can be used for designing a plant for treatment of wastewater economically.

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

    NARCIS (Netherlands)

    de Jong, GJ; Koster, EHM

    2000-01-01

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

  5. Technical note: New applications for on-line automated solid phase extraction

    OpenAIRE

    MacFarlane, John D.

    1997-01-01

    This technical note explains the disadvantages of manual solid phase extraction (SPE) techniques and the benefits to be gained with automatic systems. The note reports on a number of general and highly specific applications using the Sample Preparation Unit OSP-2A.

  6. Micro versus macro solid phase extraction for monitoring water contaminants: a preliminary study using trihalomethanes.

    Science.gov (United States)

    Alexandrou, Lydon D; Spencer, Michelle J S; Morrison, Paul D; Meehan, Barry J; Jones, Oliver A H

    2015-04-15

    Solid phase extraction is one of the most commonly used pre-concentration and cleanup steps in environmental science. However, traditional methods need electrically powered pumps, can use large volumes of solvent (if multiple samples are run), and require several hours to filter a sample. Additionally, if the cartridge is open to the air volatile compounds may be lost and sample integrity compromised. In contrast, micro cartridge based solid phase extraction can be completed in less than 2 min by hand, uses only microlitres of solvent and provides comparable concentration factors to established methods. It is also an enclosed system so volatile components are not lost. The sample can also be eluted directly into a detector (e.g. a mass spectrometer) if required. However, the technology is new and has not been much used for environmental analysis. In this study we compare traditional (macro) and the new micro solid phase extraction for the analysis of four common volatile trihalomethanes (trichloromethane, bromodichloromethane, dibromochloromethane and tribromomethane). The results demonstrate that micro solid phase extraction is faster and cheaper than traditional methods with similar recovery rates for the target compounds. This method shows potential for further development in a range of applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Development of an interface for directly coupled solid-phase extraction and GC-MS analysis

    NARCIS (Netherlands)

    Öllers, M.J.H.; van Lieshout, H.P.M.; Janssen, J.G.M.; Cramers, C.A.M.G.

    Solid-phase extraction (SPE) is widely used as a sample preparation technique in numerous application areas of chromatography. Large-volume injection is an attractive technique for coupling SPE to gas chromatography (GC) because it provides improved detection limits and circumvents the need for

  8. A simplified radiometabolite analysis procedure for PET radioligands using a solid phase extraction with micellar medium

    International Nuclear Information System (INIS)

    Nakao, Ryuji; Halldin, Christer

    2013-01-01

    A solid phase extraction method has been developed for simple and high-speed direct determination of PET radioligands in plasma. Methods: This methodology makes use of a micellar medium and a solid-phase extraction cartridge for displacement of plasma protein bound radioligand and separation of PET radioligands from their radiometabolites without significant preparation. The plasma samples taken from monkey or human during PET measurements were mixed with a micellar eluent containing an anionic surfactant sodium dodecyl sulphate and loaded onto SPE cartridges. The amount of radioactivity corresponding to parent radioligand (retained on the cartridge) and its radioactive metabolites (eluted with micellar eluent) was measured. Results: Under the optimized conditions, excellent separation of target PET radioligands from their radiometabolites was achieved with a single elution and short run-time of 1 min. This method was successfully applied to study the metabolism for 11 C-labelled radioligands in human or monkey plasma. The amount of parent PET radioligands estimated by micellar solid phase extraction strongly corresponded with that determined by radio-LC. The improved throughput permitted the analysis of a large number of plasma samples (up to 13 samples per one PET study) for accurate estimation of metabolite-corrected input function during quantitative PET imaging studies. Conclusion: Solid phase extraction together with micellar medium is fast, sensitive and easy to use, and therefore it is an attractive alternative method to determine relative composition of PET radioligands in plasma

  9. Analytical and preparative separation of organic acids from water by extraction with trioctylamine

    International Nuclear Information System (INIS)

    Eberle, S.H.; Hoyer, O.; Knobel, K.P.; Hodenberg, S. von

    1977-12-01

    The extraction of pure organic acids and of humic and ligninsulfonic acid from water by a solution of trioctylamine in chloroform was investigated (technical grade amine = ALAMINE). Quantitative separation is achieved by double extraction with 5% ALAMINE at pH 3,5 - 4. The acids may be back-extracted with dilute sodium hydroxide solution. Procedures are described for the analytical extraction of water samples of 200 to 2.000 ml and for the flow-through processing of large water volumes. (orig.) [de

  10. Streamlined Membrane Proteome Preparation for Shotgun Proteomics Analysis with Triton X-100 Cloud Point Extraction and Nanodiamond Solid Phase Extraction

    Directory of Open Access Journals (Sweden)

    Minh D. Pham

    2016-05-01

    Full Text Available While mass spectrometry (MS plays a key role in proteomics research, characterization of membrane proteins (MP by MS has been a challenging task because of the presence of a host of interfering chemicals in the hydrophobic protein extraction process, and the low protease digestion efficiency. We report a sample preparation protocol, two-phase separation with Triton X-100, induced by NaCl, with coomassie blue added for visualizing the detergent-rich phase, which streamlines MP preparation for SDS-PAGE analysis of intact MP and shot-gun proteomic analyses. MP solubilized in the detergent-rich milieu were then sequentially extracted and fractionated by surface-oxidized nanodiamond (ND at three pHs. The high MP affinity of ND enabled extensive washes for removal of salts, detergents, lipids, and other impurities to ensure uncompromised ensuing purposes, notably enhanced proteolytic digestion and down-stream mass spectrometric (MS analyses. Starting with a typical membranous cellular lysate fraction harvested with centrifugation/ultracentrifugation, MP purities of 70%, based on number (not weight of proteins identified by MS, was achieved; the weight-based purity can be expected to be much higher.

  11. Investigation of the remaining major and trace elements in clean coal generated by organic solvent extraction

    Energy Technology Data Exchange (ETDEWEB)

    Jie Wang; Chunqi Li; Kinya Sakanishi; Tetsuya Nakazato; Hiroaki Tao; Toshimasa Takanohashi; Takayuki Takarada; Ikuo Saito [National Institute Advanced Industrial Science and Technology (AIST), Ibaraki (Japan). Energy Technology Research Institute

    2005-09-01

    A sub-bituminous Wyodak coal (WD coal) and a bituminous Illinois No. 6 coal (IL coal) were thermally extracted with 1-methylnaphthalene (1-MN) and N-methyl-2-pyrrolidone (NMP) to produce clean extract. A mild pretreatment with acetic acid was also carried out. Major and trace inorganic elements in the raw coals and resultant extracts were determined by means of inductively coupled plasma optical emission spectrometry (ICP-OES), flow injection inductively coupled plasma mass spectrometry (FI-ICP-MS), and cold vapor atomic absorption spectrometry (CV-AAS). It was found that the extraction with 1-MN resulted in 73-100% reductions in the concentration of Li, Be, V, Ga, As, Se, Sr, Cd, Ba, Hg, and Pb. The extraction with NMP yielded more extract than that with 1-MN, but it retained more organically associated major and trace metals in the extracts. In the extraction of WD coal with NMP, the acid pretreatment not only significantly enhanced the extraction yield but also significantly reduced the concentrations of alkaline earth elements such as Be, Ca, Mg, Sr, and Ba in the extract. In addition, the modes of occurrence of trace elements in the coals were discussed according to their extraction behaviors. 30 refs., 2 figs., 5 tabs.

  12. Efficacy of antimicrobials extracted from organic pecan shell for inhibiting the growth of Listeria spp.

    Science.gov (United States)

    Babu, Dinesh; Crandall, Philip G; Johnson, Casey L; O'Bryan, Corliss A; Ricke, Steven C

    2013-12-01

    Growers and processors of USDA certified organic foods are in need of suitable organic antimicrobials. The purpose of the research reported here was to develop and test natural antimicrobials derived from an all-natural by-product, organic pecan shells. Unroasted and roasted organic pecan shells were subjected to solvent free extraction to produce antimicrobials that were tested against Listeria spp. and L. monocytogenes serotypes to determine the minimum inhibitory concentrations (MIC) of antimicrobials. The effectiveness of pecan shell extracts were further tested using a poultry skin model system and the growth inhibition of the Listeria cells adhered onto the skin model were quantified. The solvent free extracts of pecan shells inhibited Listeria strains at MICs as low as 0.38%. The antimicrobial effectiveness tests on a poultry skin model exhibited nearly a 2 log reduction of the inoculated cocktail mix of Listeria strains when extracts of pecan shell powder were used. The extracts also produced greater than a 4 log reduction of the indigenous spoilage bacteria on the chicken skin. Thus, the pecan shell extracts may prove to be very effective alternative antimicrobials against food pathogens and supplement the demand for effective natural antimicrobials for use in organic meat processing. © 2013 Institute of Food Technologists®

  13. Pipette-tip solid-phase extraction using polypyrrole as efficient adsorbent for extraction of avermectins and milbemycins in milk.

    Science.gov (United States)

    Florez, Diego Hernando Ângulo; Teixeira, Roseane Andrade; da Silva, Ricky Cássio Santos; Pires, Bruna Carneiro; Dutra, Flávia Viana Avelar; Borges, Keyller Bastos

    2018-05-01

    In this work, we developed a HPLC method for the multidetermination of avermectins (AVM) (abamectin-ABA 1b and ABA 1a, eprinomectin-EPR, and ivermectin-IVM) and milbemycins (moxidectin-MOX) in milk samples using polypyrrole (PPy) as adsorbent material in pipette-tip solid-phase extraction (PT-PPy-SPE). PPy was characterized by scanning electron microscopy, thermogravimetric analysis, Fourier transform infrared spectroscopy, and X-ray diffraction and the data agreed with the literature. The sample preparation included the clean-up of the milk by protein precipitation (PP) with acetonitrile and extraction of the analytes by PT-PPy-SPE. The chromatographic method was developed in reverse phase and isocratic mode with flow rate at 1.2 mL min -1 and ultraviolet detection at 250 nm. The mobile phase composition was acetonitrile:methanol:water (55:25:20, v/v/v). The studied parameters and the optimized conditions for the sample preparation were washing solvent (300 μL water), volume and type of eluent (500 μL methanol), volume and pH of sample (1 mL and pH 10), amount of adsorbent material (50 mg PPy), and without addition of salt (NaCl). The method was linear over the concentration range from 20 to 3000 ng mL -1 with coefficients of correlation (r) ≥ 0.99 for all analytes and recoveries around 100%. The method developed and validated was used for the analyses of real milk samples from cow treated with Ivomec ® (IVM 3.5%), in which were found 21.51 ± 2.94 ng mL -1 of IVM. Finally, the results proved that PT-PPy-SPE coupled to HPLC-UV was economical, simple, and easy-to-perform technique. Graphical abstract Pipette-tip solid phase extraction using polypirrole as adsorbent material for determination of avermectins and milbemycins in milk.

  14. An Effective Method to Detect Volatile Intermediates Generated in the Bioconversion of Coal to Methane by Gas Chromatography-Mass Spectrometry after In-Situ Extraction Using Headspace Solid-Phase Micro-Extraction under Strict Anaerobic Conditions.

    Science.gov (United States)

    Liu, Jianmin; Wang, Baoyu; Tai, Chao; Wu, Li; Zhao, Han; Guan, Jiadong; Chen, Linyong

    2016-01-01

    Bioconversion of coal to methane has gained increased attention in recent decades because of its economic and environmental advantages. However, the mechanism of this process is difficult to study in depth, partly because of difficulties associated with the analysis of intermediates generated in coal bioconversion. In this investigation, we report on an effective method to analyze volatile intermediates generated in the bioconversion of coal under strict anaerobic conditions. We conduct in-situ extraction of intermediates using headspace solid-phase micro-extraction followed by detection by gas chromatography-mass spectrometry. Bioconversion simulation equipment was modified and combined with a solid-phase micro-extraction device. In-situ extraction could be achieved by using the combined units, to avoid a breakdown in anaerobic conditions and to maintain the experiment continuity. More than 30 intermediates were identified qualitatively in the conversion process, and the variation in trends of some typical intermediates has been discussed. Volatile organic acids (C2-C7) were chosen for a quantitative study of the intermediates because of their importance during coal bioconversion to methane. Fiber coating, extraction time, and solution acidity were optimized in the solid-phase micro-extraction procedure. The pressure was enhanced during the bioconversion process to investigate the influence of headspace pressure on analyte extraction. The detection limits of the method ranged from 0.0006 to 0.02 mmol/L for the volatile organic acids and the relative standard deviations were between 4.6% and 11.5%. The volatile organic acids (C2-C7) generated in the bioconversion process were 0.01-1.15 mmol/L with a recovery range from 80% to 105%. The developed method is useful for further in-depth research on the bioconversion of coal to methane.

  15. Extraction of Uranium with Amin as solvent and HCl as internal phase at membrane emulsion

    International Nuclear Information System (INIS)

    Ninik Bintarti, A.; Bambang-Edi-HB; Sudibyo, R.

    1996-01-01

    An extraction process of uranium by Tri-n-Actylamine(TOA) solution with kerosene as thinner and surfactant of Span-80 as emulgator to bend a membrane emulsion. HCI 0.01 N is used as an internal phase uranium in HNO 3 as feed and butanol is used to split the membrane. In the case of membrane, the result was 1 % vol. TOA and 5 % vol. Span-80, emulsification time was 30 minutes and 50 % vol. HCI 0.01 N. The product of an extraction was concentration of HNO 3 is 3 M. The time of extraction 20 minutes and uranium concentration in feed of 600 ppm will give distribution coefficient of membrane extraction was 5.830 and coefficient of stripping was 0.276

  16. Separation and Purification of Sulforaphane from Broccoli by Solid Phase Extraction

    Directory of Open Access Journals (Sweden)

    Kyung Ho Row

    2011-03-01

    Full Text Available A simple solid-phase extraction (SPE method for the determination of sulforaphane in broccoli has been developed. The optimal conditions were found to be use of a silica SPE cartridge, and ethyl acetate and dichloromethane as washing and eluting solvents, respectively, which could eliminate interferences originating from the broccoli matrix. The extracts were sufficiently clean to be directly injected into high-performance liquid chromatography (HPLC for further chromatographic analysis. Good linearity was obtained from 0.05 to 200 μg/mL (r = 0.998 for sulforaphane with the relative standard deviations less than 3.6%. The mean recoveries of sulforaphane from broccoli were more than 90.8% and the detection limit (S/N = 3:1 was 0.02 μg/mL. The SPE method provides a higher yield of sulforaphane from crude extracts compared to conventional liquid-liquid extraction.

  17. Selective extraction methods for aluminium, iron and organic carbon from montane volcanic ash soils

    NARCIS (Netherlands)

    Jansen, B.; Tonneijck, F.H.; Verstraten, J.M.

    2011-01-01

    Montane volcanic ash soils contain disproportionate amounts of soil organic carbon and thereby play an often underestimated role in the global carbon cycle. Given the central role of Al and Fe in stabilizing organic matter in volcanic ash soils, we assessed various extraction methods of Al, Fe, and

  18. Batch tests of a microbial fuel cell for electricity generation from spent organic extracts from hydrogenogenic fermentation of organic solid wastes

    International Nuclear Information System (INIS)

    Carmona-Martinez, A.; Solorza-Feria, O.; Poggi-Varaldo, H. M.

    2009-01-01

    Hydrogenogenic fermentative processes of organic solid wastes produce spent solids that contain substantial concentrations of low molecular weight organic acids and solvents. The spent solids can be extracted with wastewater to give a stream containing concentrated, degradable organic compounds. (Author)

  19. Magnetic solid phase extraction and static headspace gas chromatography-mass spectrometry method for the analysis of polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Cai, Ying; Yan, Zhihong; Wang, Lijia; NguyenVan, Manh; Cai, Qingyun

    2016-01-15

    A magnetic solid phase extraction (MSPE) protocol combining a static headspace gas chromatography coupled to mass spectrometry (HS-GC-MS) method has been developed for extraction, and determination of 16 polycyclic aromatic hydrocarbons (PAHs) in drinking water samples. Magnetic nanoparticles (MNPs) were coated with 3-aminopropyltriethoxysilane and modified by cholesterol chloroformate. Transmission electron microscope, vibrating sample magnetometer, Fourier transform infrared spectrometry and X-ray photoelectron spectroscopy were used to characterize the cholesterol-functionalized sorbents, and the main parameters affecting the extraction as well as HS sampling, such as sorbent amount, extraction time, oven temperature and equilibration time have been investigated and established. Combination with HS sampling, the MSPE procedure was simple, fast and environmentally friendly, without need of any organic solvent. Method validation proved the feasibility of the developed sorbents for the quantitation of the investigated analytes at trace levels obtaining the limit of detection (S/N=3) ranging from 0.20 to 7.8 ng/L. Good values for intra and inter-day precision were obtained (RSDs ≤ 9.9%). The proposed method was successfully applied to drinking water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. New poly(styrene/divinylbenzene) based stationary phases for the solid phase extraction of pesticides and the chromatography of carbohydrates

    International Nuclear Information System (INIS)

    Wartusch, I.

    2002-02-01

    The introduced sorbents based on poly(styrene/divinylbenzene) are studied regarding their extraction behavior of pesticides out of water. The sorbents are prepared with different porogens like n-octanol, n-decanol, n-dodecanol and acetone. The comparison of the extraction properties of these substances shows that the use of n-octanol as a porogen leads to the best recoveries. Furthermore this sorbent is compared to a stationary phase prepared via ring opening metathesis polymerization (ROMP) and to commercially available silica-C18. It is shown that the poly(styrene/divinylbenzene) based material on average yields higher recoveries as the other materials. Only the extraction of relatively polar pesticides works better with the ROMP based sorbent. For the chromatography of carbohydrates nonporous particles with diameters of about 3 μm were synthesized via poly(styrene/divinylbenzene) using the activated swelling method. Quaternary ammonia functional groups were introduced into the poly(styrene/divinylbenzene) particles via their nitration, reduction and quaternization. The applicability of these stationary phases for anion exchange chromatography is shown by separation of different kinds of sugars using a pulsed amperometric detection system. Monosaccharides are isocratically separated using an eluent containing sodium hydroxide, separations of disaccharides and oligosaccharides are performed using sodium acetate gradients. Linearity, detection limits and reproducibility of the system are investigated by the analysis of glucose, sucrose and fructose out of the real samples Coca Cola and apple juice. (author)

  1. Solid phase extraction of Am (III) by resins impregnated with multiply diglycolamide-functionalized ligands

    International Nuclear Information System (INIS)

    Gujar, R.B.; Ansari, S.A.; Mohapatra, P.K.; Verboom, W.

    2016-01-01

    Solvent extraction studies with multiply diglycolamide-functionalized extractants such as tripodal diglycolamide (T-DGA) or diglycolamide-functionalized calix(4)arene (C4DGA) ligands have shown excellent results as compared to those of normal DGA ligands such as TODGA. A very high selectivity for Am(III) has been reported with these ligands with respect to U(VI) and Pu(IV). High selectivities and large extraction efficiencies of these ligands towards trivalent f elements were ascribed to a co-operative complexation mechanism. Furthermore, the extraction efficiency of these ligands increased several folds in ionic liquid medium as compared to paraffinic solvents. It was of interest, therefore, to prepare extraction chromatographic resins by impregnation of solvent systems containing these ligands in an ionic liquid. In the present work, solid phase extraction studies were carried out using these two multiply diglycolamide-functionalized extractants, viz. T-DGA (resin I) and C4DGA (resin-II) containing the ionic liquid C 4 mim. NTf 2 impregnated on Chromosorb-W

  2. Ultrathin-shell boron nitride hollow spheres as sorbent for dispersive solid-phase extraction of polychlorinated biphenyls from environmental water samples.

    Science.gov (United States)

    Fu, Meizhen; Xing, Hanzhu; Chen, Xiangfeng; Chen, Fan; Wu, Chi-Man Lawrence; Zhao, Rusong; Cheng, Chuange

    2014-11-21

    Boron nitride hollow spheres with ultrathin-shells were synthesized and used as sorbents for dispersive solid-phase extraction of aromatic pollutants at trace levels from environmental water samples. Polychlorinated biphenyls (PCBs) were selected as target compounds. Sample quantification and detection were performed by gas chromatography-tandem mass spectrometry. Extraction parameters influencing the extraction efficiency were optimized through response surface methodology using the Box-Behnken design. The proposed method achieved good linearity within the concentration range of 0.15-250 ng L(-1) PCBs, low limits of detection (0.04-0.09 ng L(-1), S/N=3:1), good repeatability of the extractions (relative standard deviation, spring waters were analyzed using the developed method. Results demonstrated that the hexagonal boron nitride-based material has significant potential as a sorbent for organic pollutant extraction from environmental water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2018-05-14

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

  4. Halogen bonding: A new retention mechanism for the solid phase extraction of perfluorinated iodoalkanes

    International Nuclear Information System (INIS)

    Yan Xiaoqing; Shen Qianjin; Zhao Xiaoran; Gao Haiyue; Pang Xue; Jin Weijun

    2012-01-01

    Highlights: ► Halogen bonding (XB) is firstly utilised in solid phase extraction. ► The perfluorinated iodine alkanes can be extracted by C-I⋯Cl − halogen bonding. ► The C-I⋯Cl − halogen bond is well characterised by spectroscopy methods. ► The analytes with strong halogen-bonding abilities can be selectively extracted. - Abstract: For the first time, halogen-bonding interaction is utilised in the solid phase extraction of perfluorinated iodoalkane (PFI). Nine PFIs, as model analytes, were tested, and analyses by UV, 19 F NMR and Raman spectroscopies demonstrate that the PFIs are extracted by a strong anion exchange (SAX) sorbent from n-hexane due to the C-I⋯Cl − halogen-bonding interactions. The results also show that the adsorptivities of SAX for the diiodoperfluoro-alkanes (diiodo-PFIs) were much stronger than those for the perfluoroalkyl iodides (monoiodo-PFIs). Specifically, the recoveries for 1,6-diiodoperfluorohexane and 1,8-diiodoperfluorooctane were higher than 80% when 100 mL of sample spiked with a 5 ng mL −1 analyte mixture was extracted. Interestingly, SAX had no adsorption for hexafluorobenzene at all, which is known to be unable to form a halogen bond with Cl − . The analytical performance of the halogen bond-based SPE-GC–MS method for the diiodo-PFIs was also examined in soil samples. The sorbent SAX enabled the selective extraction of four diiodo-PFIs successfully from soil samples. The recoveries of the diiodo-PFIs extracted from 5 g soil sample at the 100 ng g −1 spike level were in the range of 73.2–93.8% except 26.8% for 1,2-diiodoperfluoroethane. The limit of detection varied from 0.02 to 0.04 ng g −1 in soil samples. Overall, this work reveals the great application potential of halogen bonding in the field of solid phase extraction to selectively extract compounds with strong halogen-bonding abilities.

  5. Aptamer-functionalized Fe3 O4 magnetic nanoparticles as a solid-phase extraction adsorbent for the selective extraction of berberine from Cortex phellodendri.

    Science.gov (United States)

    Jiang, Ling-Feng; Chen, Bo-Cheng; Chen, Ben; Li, Xue-Jian; Liao, Hai-Lin; Zhang, Wen-Yan; Wu, Lin

    2017-07-01

    The extraction adsorbent was fabricated by immobilizing the highly specific recognition and binding of aptamer onto the surface of Fe 3 O 4 magnetic nanoparticles, which not only acted as recognition elements to recognize and capture the target molecule berberine from the extract of Cortex phellodendri, but also could favor the rapid separation and purification of the bound berberine by using an external magnet. The developed solid-phase extraction method in this work was useful for the selective extraction and determination of berberine in Cortex phellodendri extracts. Various conditions such as the amount of aptamer-functionalized Fe 3 O 4 magnetic nanoparticles, extraction time, temperature, pH value, Mg 2+ concentration, elution time and solvent were optimized for the solid-phase extraction of berberine. Under optimal conditions, the purity of berberine extracted from Cortex phellodendri was as high as 98.7% compared with that of 4.85% in the extract, indicating that aptamer-functionalized Fe 3 O 4 magnetic nanoparticles-based solid-phase extraction method was very effective for berberine enrichment and separation from a complex herb extract. The applicability and reliability of the developed solid-phase extraction method were demonstrated by separating berberine from nine different concentrations of one Cortex phellodendri extract. The relative recoveries of the spiked solutions of all the samples were between 95.4 and 111.3%, with relative standard deviations ranging between 0.57 and 1.85%. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Experimental and computational studies on molecularly imprinted solid-phase extraction for gonyautoxins 2,3 from dinoflagellate Alexandrium minutum.

    Science.gov (United States)

    Lian, Ziru; Li, Hai-Bei; Wang, Jiangtao

    2016-08-01

    An innovative and effective extraction procedure based on molecularly imprinted solid-phase extraction (MISPE) was developed for the isolation of gonyautoxins 2,3 (GTX2,3) from Alexandrium minutum sample. Molecularly imprinted polymer microspheres were prepared by suspension polymerization and and were employed as sorbents for the solid-phase extraction of GTX2,3. An off-line MISPE protocol was optimized. Subsequently, the extract samples from A. minutum were analyzed. The results showed that the interference matrices in the extract were obviously cleaned up by MISPE procedures. This outcome enabled the direct extraction of GTX2,3 in A. minutum samples with extraction efficiency as high as 83 %, rather significantly, without any need for a cleanup step prior to the extraction. Furthermore, computational approach also provided direct evidences of the high selective isolation of GTX2,3 from the microalgal extracts.

  7. Determination of volatile compounds in grape distillates by solid-phase extraction and gas chromatography.

    Science.gov (United States)

    Lukić, Igor; Banović, Mara; Persurić, Dordano; Radeka, Sanja; Sladonja, Barbara

    2006-01-06

    Solid-phase extraction (SPE) procedure on octadecylsilica (C18) was developed for accumulation of volatile compounds from grape distillates. The procedure was optimised for final analysis by capillary gas chromatography. At mass concentrations in model solutions ranging from 0.1 to 50 mg/l solid-phase extraction recoveries of all analytes ranged from 69% for 2-phenylethanol to 102% for capric acid, with RSD values from 2 to 9%. SPE recoveries of internal standards to be added in the sample solution prior to extraction, higher alcohols 2-ethyl-1-hexanol and 1-undecanol, were 97 and 93%, respectively, with RSD values of 3%. Detection limits of analyzed compounds in model solutions ranged from 0.011 mg/l for isoamyl acetate to 0.037 mg/l for caproic acid. Method efficiency was tested in relation to acetic acid content, volume fraction of ethanol and possible matrix effects. A significant influence of matrix on SPE efficiency for geraniol, cis-2-hexen-1-ol and cis-3-hexen-1-ol was detected. For the same reason, 2-phenylethanol could not be determined by developed SPE method in samples of grape distillates. The developed solid-phase extraction method was successfully applied to determine the differences in volatile compound content in different grape distillates produced by the distillation of crushed, pressed and fermented grapes.

  8. Zinc oxide crystal whiskers as a novel sorbent for solid-phase extraction of flavonoids.

    Science.gov (United States)

    Wang, Licheng; Shangguan, Yangnan; Hou, Xiudan; Jia, Yong; Liu, Shujuan; Sun, Yingxin; Guo, Yong

    2017-08-15

    As a novel solid-phase extraction material, zinc oxide crystal whiskers were used to extract flavonoid compounds and showed good extraction abilities. X-ray diffraction, scanning electron microscopy with energy dispersive X-ray spectroscopy and surface area/pore volume characterized the sorbent. The zinc oxide was packed into a solid-phase extraction micro-column and its extraction ability was evaluated by four model flavonoid compounds. The sample loading and elution parameters were optimized and the zinc oxide based analytical method for flavonoids was established. It showed that the method has wide linearities from 1 to 150μg/L and low limits of detection at 0.25μg/L. The relative standard deviations of a single column repeatability and column to column reproducibility were less than 6.8% and 10.6%. Several real samples were analyzed by the established method and satisfactory results were obtained. The interactions between flavonoids and zinc oxide were calculated and proved to be from the Van der Waals' forces between the 4p and 5d orbitals from zinc atom and the neighboring π orbitals from flavonoid phenyl groups. Moreover, the zinc oxide crystal whiskers showed good stability and could be reused more than 50 times under the operation conditions. This work proves that the zinc oxide crystal whiskers are a good candidate for flavonoids enrichment. Copyright © 2017. Published by Elsevier B.V.

  9. Photocathalytic degradation of organic micropollutants in aqueous phase

    International Nuclear Information System (INIS)

    Driussi, D.

    2009-01-01

    The aim of this study was to design, construct and test a small system for the photo catalytic degradation of organic micropollutants in aqueous phase using solar radiation. The system is a parabolic linear trough type with automatic one-axis (N-S) tracking of the apparent movement of the sun. The tracking algorithm foresees two dispositions of the collector named horizontal and polar, the last is necessary for installations in locations that are higher than 50 o in latitude. The idea that brought to mind this project was to offer the possibility of treat herbicides polluted waters by means of a simple system without using particular oxidizing chemicals (for example hydrogen peroxide) or components (for example mercury vapour UV lamps) and therefore in an eco-sustainable way. [it

  10. Investigating substrate use efficiency across different microbial physiologies in soil-extracted, solubilized organic matter (SESOM)

    Science.gov (United States)

    Cyle, K. T.; Martinez, C. E.

    2017-12-01

    Recent experimental work has elevated the importance of microbial processing for the stabilization of fresh carbon inputs within the soil mineral matrix. Enhancing our understanding of soil carbon and nitrogen dynamics therefore requires a better understanding of how efficiently microbial metabolism can process low molecular weight carbon substrates (carbon use efficiency, CUE) under environmentally relevant conditions. One approach to better understanding microbial uptake rates and CUE is the ecophysiological study of soil isolates in liquid media culture consisting of soil-extracted solubilized organic matter (SESOM). We are using SESOM from an Oa horizon under hemlock hardwood vegetation in upstate New York as liquid media for the growth of 12 isolates from the Oa and B horizon of the same site. Here we seek to test the uptake rates as well as CUE of 5 different low molecular weight substrates spanning compound class and nominal oxidation state (glucose, acetate, formate, glycine, valine) by isolates differing in phylogeny and physiology. The use of a spike of each of the 13C-labeled substrates into SESOM, along with a 0.2 μm filtration step, allows accurate partitioning of labeled carbon between biomass, gaseous CO2 as well as the exometabolome. Coupled UHPLC-MS measurements are being used to identify and determine uptake rates of over 80 potential C substrates present in the extract as well as our labeled substrate of interest along the course of the isolate growth curve. This work seeks to utilize a gradient in substrate class as well as microbial physiologies to inform our understanding of C and N cycling under relevant soil solution conditions. Future experiments may also use labeled biomass from stationary phase to investigate the stabilization potential of anabolic products formed from each substrate with a clay fraction isolated from the same site.

  11. Develonment of novel organic extractants for applications in various radioactive waste remedistion

    International Nuclear Information System (INIS)

    Mowafy, E. A.; El-Naggar, I.A.; Shalash, A.M.

    2004-01-01

    A major goal of our research program is to develop some new amides as extractants for various waste treatments. Heterocyclic amides have been recently employed successfully as extractants for lanthanide and actinide cations and also some fission products from strongly acidic media. Many of these heterocyclic amides extractants have been synthesized in our laboratory and characterized by different techniques. Their synthesis has been improved. By optimization of the formula, it is possible to use aliphatic diluents without third-phase formation in contact with nitric or hydrochloric acids. One of the most interesting applications of amides is their use as extractants in nuclear field. main advantages of these new extractants are ease of synthesis compared with phosphorus compounds, high chemical and radiolytic stability and complete incineration which leads to smaller amounts of radioactive waste. Studies concerning the utilization of these new synthesized reagents for uranium and thorium were explored

  12. Antiviral Activity of Natural Products Extracted from Marine Organisms

    Directory of Open Access Journals (Sweden)

    Sobia Tabassum

    2011-11-01

    Full Text Available Many epidemics have broken out over the centuries. Hundreds and thousands of humans have died over a disease. Available treatments for infectious diseases have always been limited. Some infections are more deadly than the others, especially viral pathogens. These pathogens have continuously resisted all kinds of medical treatment, due to a need for new treatments to be developed. Drugs are present in nature and are also synthesized in vitro and they help in combating diseases and restoring health. Synthesizing drugs is a hard and time consuming task, which requires a lot of man power and financial aid. However, the natural compounds are just lying around on the earth, may it be land or water. Over a thousand novel compounds isolated from marine organisms are used as antiviral agents. Others are being pharmacologically tested. Today, over forty antiviral compounds are present in the pharmacological market. Some of these compounds are undergoing clinical and pre-clinical stages. Marine compounds are paving the way for a new trend in modern medicine.

  13. Solid-phase extraction (SPE) of Iron using Lanthanum Silicate ion exchange

    International Nuclear Information System (INIS)

    Kiarostami, V.; Husain, W.

    2002-01-01

    Solid-phase extraction (SPE) is gaining wide use as an effective and speedy technique which reduces solvent usage, disposal costs and extraction time. The analyte is adsorbed from solution onto a solid adsorbent, which is followed by elution of the analyte with a solvent appropriate for instrumental analysis. However, there is an increasing need for new selective adsorbents to expand the area of this technique. Lanthanum silicate ion exchanger, which shows unusual selectivity elements and in this study, it was employed to develop a SPE method for iron ion. Special experiments such as determination of distribution coefficient for iron ion in different solvent systems have been determined

  14. Linear feature extraction from radar imagery: SBIR (Small Business Innovative Research), phase 2, option 2

    Science.gov (United States)

    Milgram, David L.; Kahn, Philip; Conner, Gary D.; Lawton, Daryl T.

    1988-12-01

    The goal of this effort is to develop and demonstrate prototype processing capabilities for a knowledge-based system to automatically extract and analyze features from Synthetic Aperture Radar (SAR) imagery. This effort constitutes Phase 2 funding through the Defense Small Business Innovative Research (SBIR) Program. Previous work examined the feasibility of and technology issues involved in the development of an automated linear feature extraction system. This final report documents this examination and the technologies involved in automating this image understanding task. In particular, it reports on a major software delivery containing an image processing algorithmic base, a perceptual structures manipulation package, a preliminary hypothesis management framework and an enhanced user interface.

  15. An interior needle electropolymerized pyrrole-based coating for headspace solid-phase dynamic extraction

    Energy Technology Data Exchange (ETDEWEB)

    Bagheri, Habib [Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)], E-mail: bagheri@sharif.edu; Babanezhad, Esmaeil; Khalilian, Faezeh [Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)

    2009-02-23

    A headspace solid-phase dynamic extraction (HS-SPDE) technique was developed by the use of polypyrrole (PPy) sorbent, electropolymerized inside the surface of a needle, as a possible alternative to solid-phase microextraction (SPME). Thermal desorption was subsequently, employed to transfer the extracted analytes into the injection port of a gas chromatography-mass spectrometry (GC-MS). The PPy sorbent including polypyrrole-dodecyl sulfate (PPy-DS) was deposited on the interior surface of a stainless steel needle from the corresponding aqueous electrolyte by applying a constant deposition potential. The homogeneity and the porous surface structure of the coating were examined using the scanning electron microscopy (SEM). The developed method was applied to the trace level extraction of some polycyclic aromatic hydrocarbons (PAHs) from aqueous sample. In order to enhance the extraction efficiency and increase the partition coefficient of analytes, the stainless steel needle was cooled at 5 deg. C, while the sample solution was kept at 80 deg. C. Optimization of influential experimental conditions including the voltage of power supply, the time of PPy electrodeposition, the extraction temperature, the ionic strength and the extraction time were also investigated. The detection limits of the method under optimized conditions were in the range of 0.002-0.01 ng mL{sup -1}. The relative standard deviations (R.S.D.) at a concentration level of 0.1 ng mL{sup -1} were obtained between 7.54 and 11.4% (n = 6). The calibration curves of PAHs showed linearity in the range of 0.01-10 ng mL{sup -1}. The proposed method was successfully applied to the extraction of some selected PAHs from real-life water samples and the relative recoveries were higher than 90% for all the analytes.

  16. Investigation of extractable organic compounds in deep-sea hydrothermal vent fluids along the Mid-Atlantic Ridge

    Science.gov (United States)

    McCollom, Thomas M.; Seewald, Jeffrey S.; German, Christopher R.

    2015-05-01

    The possibility that deep-sea hydrothermal vents may contain organic compounds produced by abiotic synthesis or by microbial communities living deep beneath the surface has led to numerous studies of the organic composition of vent fluids. Most of these studies have focused on methane and other light hydrocarbons, while the possible occurrence of more complex organic compounds in the fluids has remained largely unstudied. To address this issue, the presence of higher molecular weight organic compounds in deep-sea hydrothermal fluids was assessed at three sites along the Mid-Atlantic Ridge that span a range of temperatures (51 to >360 °C), fluid compositions, and host-rock lithologies (mafic to ultramafic). Samples were obtained at several sites within the Lucky Strike, Rainbow, and Lost City hydrothermal fields. Three methods were employed to extract organic compounds for analysis, including liquid:liquid extraction, cold trapping on the walls of a coil of titanium tubing, and pumping fluids through cartridges filled with solid phase extraction (SPE) sorbents. The only samples to consistently yield high amounts of extractable organic compounds were the warm (51-91 °C), highly alkaline fluids from Lost City, which contained elevated concentrations of C8, C10, and C12n-alkanoic acids and, in some cases, trithiolane, hexadecanol, squalene, and cholesterol. Collectively, the C8-C12 acids can account for about 15% of the total dissolved organic carbon in the Lost City fluids. The even-carbon-number predominance of the alkanoic acids indicates a biological origin, but it is unclear whether these compounds are derived from microbial activity occurring within the hydrothermal chimney proximal to the site of fluid discharge or are transported from deeper within the system. Hydrothermal fluids from the Lucky Strike and Rainbow fields were characterized by an overall scarcity of extractable dissolved organic compounds. Trace amounts of aromatic hydrocarbons including

  17. Determination of Wastewater Compounds in Sediment and Soil by Pressurized Solvent Extraction, Solid-Phase Extraction, and Capillary-Column Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Burkhardt, Mark R.; Zaugg, Steven D.; Smith, Steven G.; ReVello, Rhiannon C.

    2006-01-01

    A method for the determination of 61 compounds in environmental sediment and soil samples is described. The method was developed in response to increasing concern over the effects of endocrine-disrupting chemicals in wastewater and wastewater-impacted sediment on aquatic organisms. This method also may be used to evaluate the effects of combined sanitary and storm-sewer overflow on the water and sediment quality of urban streams. Method development focused on the determination of compounds that were chosen on the basis of their endocrine-disrupting potential or toxicity. These compounds include the alkylphenol ethoxylate nonionic surfactants and their degradates, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclic aromatic hydrocarbons, and high-use domestic pesticides. Sediment and soil samples are extracted using a pressurized solvent extraction system. The compounds of interest are extracted from interfering matrix components by high-pressure water/isopropyl alcohol extraction. The compounds were isolated using disposable solid-phase extraction (SPE) cartridges containing chemically modified polystyrene-divinylbenzene resin. The cartridges were dried with nitrogen gas, and then sorbed compounds were eluted with methylene chloride (80 percent)-diethyl ether (20 percent) through Florisil/sodium sulfate SPE cartridge, and then determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-sand samples fortified at 4 to 72 micrograms averaged 76 percent ?13 percent relative standard deviation for all method compounds. Initial method reporting levels for single-component compounds ranged from 50 to 500 micrograms per kilogram. The concentrations of 20 out of 61 compounds initially will be reported as estimated with the 'E' remark code for one of three reasons: (1) unacceptably low-biased recovery (less than 60 percent) or highly variable method performance

  18. State-of-the-art in solid-phase extraction of biofluids (M10)

    International Nuclear Information System (INIS)

    Boos, K.-S.; Fleischer, C.T.

    2002-01-01

    Full text: A major drawback of many SPE protocols in bioanalytical LC is a rather unselective and/or time consuming clean-up procedure. In order to optimize SPE based sample processing with regard to selectivity and speed we investigated tailor-made SPE adorbents, distinct SPE column hardware as well as a novel software (ChromSword ADS, Merck KGaA) for LC(MS)-integrated SPE using column-switching. Restricted Access Materials (RAM) are one family of such special SPE column packing. RAMs are characterized in that they have a defined size-selective exclusion barrier and a non-adsorptive outer particle surface towards macromolecular matrix components (e.g. proteins, nucleic acids, polysaccharides). Low-molecular compounds (e.g. drugs) have free access to the binding centers and thus can be extracted and enriched prior to their analytical separation and MS detection. A RAM-SPE column (e.g. LiChrospher ADS, Merck KGaA, Germany) allows the direct, multiple injection and fractionation of crude, complex samples such as hemolyzed blood, plasma, serum, milk, saliva, urine, fermentation broth and cell-culture or tissue homogenate supernatant. In order to improve the selectivity, we extended this on-line sample clean-up protocol by coupling a reversed-phase modified RAM-SPE column with a second short column packed with a Molecularly Imprinted Polymeric (MIP) adsorbent. MIP-SPE adsorbents can be compared with immunoaffinity adsorbents. Besides selective/specific molecular recognition properties, these artificial antibodies exhibit a high stability with respect to pressure, pH, temperature as well as organic solvents. These innovative adsorbents are also attractive because of the ease, low-cost and high reproducibility of preparation. Using MIPS in combination with RAMs we developed a generic SPE platform and protocol, respectively, for highly selective clean-up of complex (bio)fluids. Finally, we succeeded in speeding up the RAM fractionation step (e.g. extraction of 50 pl of

  19. Matrix supported tailored polymer for solid phase extraction of fluoride from variety of aqueous streams

    International Nuclear Information System (INIS)

    Thakur, Neha; Kumar, Sanjukta A.; Wagh, D.N.; Das, Sadananda; Pandey, Ashok K.; Kumar, Sangita D.; Reddy, A.V.R.

    2012-01-01

    Highlights: ► Th complexed with poly (bis[2-(methacryloyloxy)-ethyl]phosphate) as tailored polymer membranes. ► Membranes offered high capacity and selectivity for fluoride in aqueous media. ► Quantitative uptake (80 ± 5%) of fluoride. ► Fast sorption kinetics. ► Reusability of polymer membranes. - Abstract: Fluoride related health hazards (fluorosis) are a major environmental problem in many regions of the world. It affects teeth; skeleton and its accumulation over a long period can lead to changes in the DNA structure. It is thus absolutely essential to bring down the fluoride levels to acceptable limits. Here, we present a new inorganic–organic hybrid polymer sorbent having tailored fixed-sites for fluoride sorption. The matrix supported poly (bis[2-(methacryloyloxy)-ethyl]phosphate) was prepared by photo-initiator induced graft-polymerization in fibrous and microporous (sheet) host poly(propylene) substrates. These substrates were conditioned for selective fluoride sorption by forming thorium complex with phosphate groups on bis[2-methacryloyloxy)-ethyl] phosphate (MEP). These tailored sorbents were studied for their selectivity towards fluoride in aqueous media having different chemical conditions. The fibrous sorbent was found to take up fluoride with a faster rate (15 min for ≈76% sorption) than the sheet sorbent. But, the fluoride loading capacity of sheet sorbent (4320 mg kg −1 ), was higher than fibrous and any other sorbent reported in the literature so far. The sorbent developed in the present work was found to be reusable after desorption of fluoride using NaOH solution. It was tested for solid phase extraction of fluoride from natural water samples.

  20. Enzymatic vegetable organic extracts as soil biochemical biostimulants and atrazine extenders.

    Science.gov (United States)

    García-Martínez, Ana María; Tejada, Manuel; Díaz, Ana Isabel; Rodríguez-Morgado, Bruno; Bautista, Juan; Parrado, Juan

    2010-09-08

    The purpose of this study was to gather information on the potential effects of organic biostimulants on soil activity and atrazine biodegradation. Carob germ enzymatic extract (CGEE) and wheat condensed distiller solubles enzymatic extract (WCDS-EE) have been obtained using an enzymatic process; their main organic components are soluble carbohydrates and proteins in the form of peptides and free amino acids. Their application to soil results in high biostimulation, rapidly increased dehydrogenase, phosphatase and glucosidase activities, and an observed atrazine extender capacity due to inhibition of its mineralization. The extender capacity of both extracts is proportional to the protein/carbohydrate ratio content. As a result, these enzymatic extracts are highly microbially available, leading to two independent phenomena, fertility and an atrazine persistence that is linked to increased soil activity.

  1. Headspace Solid Phase Microextraction in Pesticide Residues Analysis:1. Optimisation of Extraction Conditions

    Directory of Open Access Journals (Sweden)

    Rada Đurović

    2007-01-01

    Full Text Available The method of headspace solid phase microextraction (HS/SPME was successfully used in a simultaneous multicomponent analysis of hexachlorobenzene (HCB, tefluthrin, heptachlor, aldrin, chlorpyrifos, fenthion and bifenthrin in aqueous medium. Measurementswere performed using a nonpolar polydimethyl siloxane (PDMS fiber. Detection and quantification were done by gas chromatography/mass spectrometry (GC/MS.Optimal conditions for HS/SPME were determined both by performing extraction at different temperatures and examining extraction time profiles at constant temperature. Optimal extraction temperature for each pesticide studied was determined as follows: 60°C for HCB and for heptachlor, 80°C for aldrin and for chlorpyrifos, fenthion and tefluthrin, and temperature exceeding 80°C for bifenthrin. For the pesticide mixture studied, 60°C was identified as the optimum extraction temperature.Based on the time profiles obtained, it was confirmed that satisfactory extraction sensitivity can be obtained even for extraction times shorter than the time required to reach a sorption equilibrium. This conclusion was confirmed by linear concentration profiles obtained for the following ranges: 0.05-10 ng/ml (HCB, 0.05-25 ng/ml (tefluthrin, 0.05-40 ng/ml (heptachlor, 0.05-40 ng/ml (aldrin, 0.05-25 ng/ml (chlorpyrifos, 0.05-25 ng/ml (fenthionand 0.05-25 ng/ml (bifenthrin.Relative standard deviation (RSD values for triplicate measurements did not exceed 15%.

  2. Extraction of liver volumetry based on blood vessel from the portal phase CT dataset

    Science.gov (United States)

    Maklad, Ahmed S.; Matsuhiro, Mikio; Suzuki, Hidenobu; Kawata, Yoshiki; Niki, Noboru; Utsunomiya, Tohru; Shimada, Mitsuo

    2012-02-01

    At liver surgery planning stage, the liver volumetry would be essential for surgeons. Main problem at liver extraction is the wide variability of livers in shapes and sizes. Since, hepatic blood vessels structure varies from a person to another and covers liver region, the present method uses that information for extraction of liver in two stages. The first stage is to extract abdominal blood vessels in the form of hepatic and nonhepatic blood vessels. At the second stage, extracted vessels are used to control extraction of liver region automatically. Contrast enhanced CT datasets at only the portal phase of 50 cases is used. Those data include 30 abnormal livers. A reference for all cases is done through a comparison of two experts labeling results and correction of their inter-reader variability. Results of the proposed method agree with the reference at an average rate of 97.8%. Through application of different metrics mentioned at MICCAI workshop for liver segmentation, it is found that: volume overlap error is 4.4%, volume difference is 0.3%, average symmetric distance is 0.7 mm, Root mean square symmetric distance is 0.8 mm, and maximum distance is 15.8 mm. These results represent the average of overall data and show an improved accuracy compared to current liver segmentation methods. It seems to be a promising method for extraction of liver volumetry of various shapes and sizes.

  3. Molecularly imprinted solid-phase extraction for selective extraction of bisphenol analogues in beverages and canned food.

    Science.gov (United States)

    Yang, Yunjia; Yu, Jianlong; Yin, Jie; Shao, Bing; Zhang, Jing

    2014-11-19

    This study aimed to develop a selective analytical method for the simultaneous determination of seven bisphenol analogues in beverage and canned food samples by using a new molecularly imprinted polymer (MIP) as a sorbent for solid-phase extraction (SPE). Liquid chromatography coupled to triple-quadruple tandem mass spectrometry (LC-MS/MS) was used to identify and quantify the target analytes. The MIP-SPE method exhibited a higher level of selectivity and purification than the traditional SPE method. The developed procedures were further validated in terms of accuracy, precision, and sensitivity. The obtained recoveries varied from 50% to 103% at three fortification levels and yielded a relative standard deviation (RSD, %) of less than 15% for all of the analytes. The limits of quantification (LOQ) for the seven analytes varied from 0.002 to 0.15 ng/mL for beverage samples and from 0.03 to 1.5 ng/g for canned food samples. This method was used to analyze real samples that were collected from a supermarket in Beijing. Overall, the results revealed that bisphenol A and bisphenol F were the most frequently detected bisphenols in the beverage and canned food samples and that their concentrations were closely associated with the type of packaging material. This study provides an alternative method of traditional SPE extraction for screening bisphenol analogues in food matrices.

  4. Polytetrafluorethylene film-based liquid-three phase micro extraction coupled with differential pulse voltammetry for the determination of atorvastatin calcium.

    Science.gov (United States)

    Ensafi, Ali A; Khoddami, Elaheh; Rezaei, Behzad

    2013-01-01

    In this paper, we describe a new combination method based on polytetrafluorethylene (PTFE) film-based liquid three-phase micro extraction coupled with differential pulse voltammetry (DPV) for the micro extraction and quantification of atorvastatin calcium (ATC) at the ultra-trace level. Different factors affecting the liquid-three phases micro extraction of atorvastatin calcium, including organic solvent, pH of the donor and acceptor phases, concentration of salt, extraction time, stirring rate and electrochemical factors, were investigated, and the optimal extraction conditions were established. The final stable signal was achieved after a 50 min extraction time, which was used for analytical applications. An enrichment factor of 21 was achieved, and the relative standard deviation (RSD) of the method was 4.5% (n = 4). Differential pulse voltammetry exhibited two wide linear dynamic ranges of 20.0-1000.0 pmol L(-1) and 0.001-11.0 µmol L(-1) of ATC. The detection limit was found to be 8.1 pmol L(-1) ATC. Finally, the proposed method was used as a new combination method for the determination of atorvastatin calcium in real samples, such as human urine and plasma.

  5. Individual extraction constants of some univalent cations in the two-phase water-phenyltrifluoromethyl sulfone system

    International Nuclear Information System (INIS)

    Makrlik, E.

    2011-01-01

    From extraction experiments and γ-activity measurements, the exchange extraction constants corresponding to the general equilibrium M + (aq) + Cs + (org) ↔ M + (org) + Cs + (aq) taking place in the two-phase water-phenyltrifluoromethyl sulfone (abbrev. FS 13) system (M + Li + , H 3 O + , Na + , NH 4 + , Ag + , Tl + , K + , Rb + ; aq = aqueous phase, org FS 13 phase) were evaluated. Furthermore, the individual extraction constants of the M + cations in the mentioned two-phase system were calculated; they were found to increase in the series of Li + 3 O + + 4 + + + + + + . (author)

  6. Dissolved organic carbon (DOC) in soil extracts investigated by FT-ICR-MS

    Science.gov (United States)

    Hofmann, D.; Steffen, D.; Jablonowski, N. D.; Burauel, P.

    2012-04-01

    Soil drying and rewetting usually increases the release of xenobiotics like pesticides present in agricultural soils. Besides the effect on the release of two aged 14C-labeled pesticide residues we focus on the characterisation of simultaneously remobilized dissolved organic carbon (DOC) to gain new insights into structure and stability aspects of soil organic carbon fractions. The test soil (gleyic cambisol; Corg 1.2%, pH 7.2) was obtained from the upper soil layer of two individual outdoor lysimeter studies containing either environmentally long-term aged 14C residues of the herbicide ethidimuron (0-10 cm depth; time of aging: 9 years) or methabenzthiazuron (0-30 cm depth; time of aging: 17 years). Soil samples (10 g dry soil equivalents) were (A=dry/wet) previously dried (45°C) or (B=wet/wet) directly mixed with pure water (1+2, w:w), shaken (150 rpm, 1 h), and centrifuged (2000 g). This extraction procedure was repeated several individual times, for both setups. The first three individual extractions, respectively were used for further investigations. Salt was removed from samples prior analysis because of a possible quench effect in the electrospray (ESI) source by solid phase extraction (SPE) with Chromabond C18 Hydra-cartridges (Macherey-Nagel) and methanol as backextraction solvent. The so preconcentrated and desalted samples were introduced by flow injection analysis (FIA) in a fourier transform ion cyclotron resonance mass spectrometer (FT-ICR-MS), equipped with an ESI source and a 7 T supra-conducting magnet (LTQ-FT Ultra, ThermoFisher Scientific). This technique is the key technique for complex natural systems attributed by their outstanding mass resolution (used 400.000 at m/z 400 Da) and mass accuracy (≤ 1ppm) by simultaneously providing molecular level details of thousands of compounds and was successful applied for the investigations of natural organic matter (NOM) different sources like marine and surface water, soil, sediment, bog and crude oil

  7. Extraction of Betulin, Trimyristin, Eugenol and Carnosic Acid Using Water-Organic Solvent Mixtures

    Directory of Open Access Journals (Sweden)

    Fulgentius N. Lugemwa

    2012-08-01

    Full Text Available A solvent system consisting of ethyl acetate, ethyl alcohol and water, in the volume ratio of 4.5:4.5:1, was developed and used to extract, at room temperature, betulin from white birch bark and antioxidants from spices (rosemary, thyme, sage, and oregano and white oak chips. In addition, under reflux conditions, trimyristin was extracted from nutmeg using the same solvent system, and eugenol from olives was extracted using a mixture of salt water and ethyl acetate. The protocol demonstrates the use of water in organic solvents to extract natural products from plants. Measurement of the free-radical scavenging activity using by 2,2-diphenyl-1-picrylhydrazyl (DPPH indicated that the extraction of plant material using ethyl acetate, ethyl alcohol and water (4.5:4.5:1, v/v/v was exhaustive when carried out at room temperature for 96 h.

  8. Chemical Composition and Antioxidant Activity of Essential Oil and Organic Extracts of Premna integrifolia Linn

    Directory of Open Access Journals (Sweden)

    Sharif M. Al-Reza

    Full Text Available ABSTRACT This study was designed to examine the chemical composition and in vitro antioxidant activity of the hydrodistillated essential oil and various extracts obtained from Premna integrifolia Linn. GC-MS analysis of the essential oil was resulted in determination 29 different compounds, representing 95.73% of total oil. Antioxidant activities of the essential oil and organic extracts of chloroform, ethyl acetate and methanol were determined by three different test systems namely DPPH (2,2-diphenyl-1-picrylhydrazyl, superoxide and nitric oxide radical scavenging assays. The essential oil and methanol extract showed potent antioxidant activity among all the tested samples. Furthermore, the amount of total phenolic compounds was determined and its content in methanol extract was the highest as compared to other samples. The results indicate that the essential oil and extracts of Premna integrifolia could serve as an important bio-resource of antioxidants for using in the pharmaceutical industries.

  9. Multiturn extraction and injection by means of adiabatic capture in stable islands of phase space

    Directory of Open Access Journals (Sweden)

    R. Cappi

    2004-02-01

    Full Text Available Recently a novel approach has been proposed for performing multiturn extraction from a circular machine. Such a technique consists of splitting the beam by means of stable islands created in transverse phase space by magnetic elements creating nonlinear fields, such as sextupoles and octupoles. Provided a slow time variation of the linear tune is applied, adiabatic with respect to the betatron motion, the islands can be moved in phase space and eventually charged particles may be trapped inside the stable structures. This generates a certain number of well-separated beamlets. Originally, this principle was successfully tested using a fourth-order resonance. In this paper the approach is generalized by considering other types of resonances as well as the possibility of performing multiple multiturn extractions. The results of numerical simulations are presented and described in detail. Of course, by time reversal, the proposed approach could be used also for multiturn injection.

  10. A chromatographic determination of water in non-aqueous phases of solvent extraction systems

    International Nuclear Information System (INIS)

    Lyle, S.J.; Smith, D.B.

    1975-01-01

    The disadvantages of the Karl Fischer method for the determination of water in the non-aqueous phases of solvent extraction systems are pointed out, and a gas chromatographic method is described which is claimed to be potentially capable of overcoming these disadvantages. The method, as described, was developed to satisfy conditions relevant to measurement of the transfer rate of water from an aqueous phase into tri-n-butylphosphate in toluene, but it can be used for water determination in other solvent extraction systems. The apparatus used is described in detail. The concentration of water in water-saturated TBP was found to be 3.56 mol/litre, compared with a value of 3.55 obtained by Karl Fischer titration and previous literature values of 3.59 and 3.57. Measurements of water content in benzene solutions of long chain alkylamines were also sucessfully carried out. (U.K.)

  11. Solid-phase extraction NMR studies of chromatographic fractions of saponins from Quillaja saponaria.

    Science.gov (United States)

    Nyberg, Nils T; Baumann, Herbert; Kenne, Lennart

    2003-01-15

    The saponin mixture QH-B from the tree Quillaja saponaria var. Molina was fractionated by RP-HPLC in several steps. The fractions were analyzed by solid-phase extraction NMR (SPE-NMR), a technique combining the workup by solid-phase extraction with on-line coupling to an NMR flow probe. Together with MALDI-TOF mass spectrometry and comparison with chemical shifts of similar saponins, the structures of both major and minor components in QH-B could be obtained. The procedure described is a simple method to determine the structure of components in a complex mixture. The two major fractions of the mixture were found to contain at least 28 saponins, differing in the carbohydrate substructures. Eight of these have not previously been determined. The 28 saponins formed 14 equilibrium pairs by the migration of an O-acyl group between two adjacent positions on a fucosyl residue.

  12. Magnetic solid-phase extraction of protein with deep eutectic solvent immobilized magnetic graphene oxide nanoparticles.

    Science.gov (United States)

    Xu, Kaijia; Wang, Yuzhi; Ding, Xueqin; Huang, Yanhua; Li, Na; Wen, Qian

    2016-01-01

    As a new type of green solvent, four kinds of choline chloride (ChCl)-based deep eutectic solvents (DESs) have been synthesized, and then a core-shell structure magnetic graphene oxide (Fe3O4-NH2@GO) nanoparticles have been prepared and coated with the ChCl-based DESs. Magnetic solid-phase extraction (MSPE) based Fe3O4-NH2@GO@DES was studied for the first time for the extraction of proteins. The characteristic results of vibrating sample magnetometer (VSM), X-ray diffraction (XRD), Fourier transform infrared spectrometry (FT-IR), thermal gravimetric analysis (TGA) and field emission scanning electron microscopy (FESEM) indicated the successful preparation of Fe3O4-NH2@GO@DES. The concentrations of proteins in studies were determined by a UV-vis spectrophotometer. The advantages of Fe3O4-NH2@GO@DES in protein extraction were compared with Fe3O4-NH2@GO and Fe3O4-NH2, and Fe3O4-NH2@GO@ChCl-glycerol was selected as the suitable extraction solvent. The influence factors of the extraction process such as the pH value, the temperature, the extraction time, the concentration of protein and the amount of Fe3O4-NH2@GO@ChCl-glycerol were evaluated. Desorption experimental result showed 98.73% of BSA could be eluted from the solid extractant with 0.1 mol/L Na2HPO4 solution contained 1 mol/L NaCl. Besides, the conformation of BSA was not changed during the elution by the investigation of circular dichromism (CD) spectra. Furthermore, the analysis of real sample demonstrated that the prepared magnetic nanoparticles did have extraction ability on proteins in bovine whole blood. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Extraction optimization and pixel-based chemometric analysis of semi-volatile organic compounds in groundwater

    DEFF Research Database (Denmark)

    Christensen, Peter; Tomasi, Giorgio; Kristensen, Mette

    2017-01-01

    . In this study, we tested the combination of solid phase extraction (SPE) with dispersive liquid-liquid micro extraction (DLLME), or with stir bar sorptive extraction (SBSE), as an extraction method for semi-VOCs in groundwater. Combining SPE with DLLME or SBSE resulted in better separation of peaks...... in an unresolved complex mixture. SPE-DLLME was chosen as the preferred extraction method. SPE-DLLME covered a larger polarity range (logKo/w 2.0-11.2), had higher extraction efficiency at logKo/w 2.0-3.8 and 5.8-11.2, and was faster compared to SPE-SBSE. SPE-DLLME extraction combined with chemical analysis by gas...... chromatography-mass spectrometry (GC-MS) and pixel-based data analysis of summed extraction ion chromatograms (sEICs) was tested as a new method for chemical fingerprinting of semi-VOCs in 15 groundwater samples. The results demonstrate that SPE-DLLME-GC-MS provides an excellent compromise between compound...

  14. Rapid determination of ions by combined solid-phase extraction--diffuse reflectance spectroscopy

    Science.gov (United States)

    Fritz, James S.; Arena, Matteo P.; Steiner, Steven A.; Porter, Marc D.

    2003-01-01

    We introduce colorimetric solid-phase extraction (C-SPE) for the rapid determination of selected ions. This new technique links the exhaustive concentration of an analyte by SPE onto a membrane disk surface for quantitative measurement with a hand-held diffuse reflectance spectrometer. The concentration/measurement procedure is complete in approximately 1 min and can be performed almost anywhere. This method has been used to monitor iodine and iodide in spacecraft water in the 0.1-5.0 ppm range and silver(I) in the range of 5.0-1000 microg/l. Applications to the trace analysis of copper(II), nickel(II), iron(III) and chromium(VI) are described. Studies on the mechanism of extraction showed that impregnation of the disk with a surfactant as well as a complexing reagent results in uptake of additional water, which markedly improves the extraction efficiency.

  15. Visual monitoring of solid-phase extraction using chromogenic fluorous synthesis supports.

    Science.gov (United States)

    Blackburn, Christopher

    2012-03-12

    Reductive aminations and further transformations of an azo dye and fluorous tagged aldehyde are described. The intensely colored 2,4-dialkoxybenzyl protected amines undergo Fmoc-based peptide coupling, Suzuki reactions, and sulfonamide formation with product isolation facilitated by visual monitoring of fluorous solid phase extraction. Target compounds are released from the supports in high yields and purities by treatment with trifluoroacetic acid (TFA).

  16. Integration of Solid-phase Extraction with Electrothermal Atomic Absorption Spectrometry for Determination of Trace Elements

    OpenAIRE

    NUKATSUKA, Isoshi; OHZEKI, Kunio

    2006-01-01

    An enrichment step in a sample treatment is essential for trace analysis to improve the sensitivity and to eliminate the matrix of the sample. Solid-phase extraction (SPE) is one of the widely used enrichment technique. Electrothermal atomic absorption spectrometry (ETAAS) is a well-established determination technique for trace elements. The integration of SPE with ETAAS leads to further improvement of sensitivity, an automation of the measurement and the economy in the sample size, amounts o...

  17. Kinetics of hydrophobic organic contaminant extraction from sediment by granular activated carbon

    NARCIS (Netherlands)

    Rakowska, M.I.; Kupryianchyk, D.; Smit, M.; Koelmans, A.A.; Meent, van de D.

    2014-01-01

    Ex situ solid phase extraction with granular activated carbon (GAC) is a promising technique to remediate contaminated sediments. The methods' efficiency depends on the rate by which contaminants are transferred from the sediment to the surface of GAC. Here, we derive kinetic parameters for

  18. A rapid solid-phase extraction fluorometric method for thiamine and riboflavin in salmonid eggs

    Science.gov (United States)

    Zajicek, James L.; Tillitt, Donald E.; Brown, Scott B.; Brown, Lisa R.; Honeyfield, Dale C.; Fitzsimons, John D.

    2005-01-01

    A new method has been developed and successfully applied to the selective measurement of thiamine (nonphosphorylated), total thiamine (sum of thiamine, thiamine monophosphate [TMP], thiamine diphosphate [TDP], and thiamine triphosphate [TTP]), and potentially interfering riboflavin in acidic (2% trichloroacetic acid) extracts of selected salmonid and walleye egg samples. Acidic extracts of eggs were applied directly to end-capped C18, reversed-phase solid-phase extraction (SPE) columns and separated into three fractions by elution with mixtures of PO4 buffer (pH 2), methanol (10%), and acetonitrile (20%). All thiamine compounds recovered in the first two fractions were oxidized to their corresponding thiochromes with alkaline potassium hexacyanoferrate, and we measured the thiochrome fluorescence (excitation at 360 nm, emission at 460 nm) in a 96-well microplate reader. Riboflavin, recovered in third fraction (eluted with pH 2, 20% acetonitrile), was analyzed directly by measuring the fluorescence of this fraction (excitation at 450 nm, emission at 530 nm). Significant portions of the phosphate esters of thiamine (TMP, TDP, and presumably TTP), when present at low concentrations (extract thiamine compounds into 2% trichlororacetic acid solution; an inexpensive, commercially available SPE column; small amounts of sample (0.5-1 g); microliter volumes of solvents per sample; a traditional, relatively nonhazardous, oxidation of thiamine compounds to fluorescent thiochromes; and an ultraviolet-visible-wavelength-filter fluorometer for the measurements. ?? Copyright by the American Fisheries Society 2005.

  19. Solid phase extraction of uranium from phosphoric acid. Kinetic and thermodynamic study

    Energy Technology Data Exchange (ETDEWEB)

    Abdel-Magied, Ahmed Fawzy [Nuclear Materials Authority, Cairo (Egypt); Stockholm Univ. (Sweden). Dept. of Organic Chemistry

    2017-07-01

    There is a high interest to develop suitable solid phase extractants for uranium separation from aqueous solutions in order to reduce cost and enhance the efficiency. This paper describes solid phase extraction of uranium(VI) from aqueous phosphoric acid solution using MCM-41 based D2HEPA-TOPO organophosphorous extractants. The mixture of D2HEPA (di-2-ethyl-hexylphosphoric acid) and TOPO (tri-n-octylphosphine oxide) was impregnated into the pores of MCM-41 and the synthesized sorbent was fully characterized. The influences of different factors such as synergistic mixture ratio, phosphoric acid concentration, mixing time and temperature were investigated. The results showed that 90% of uranium(VI) extraction can be achieved within 5 min, using D2HEPA-TOPO rate at MCM-41 (mass ratio 2:1 w/w) from 1 M phosphoric acid containing 64 ppm of uranium at room temperature. High adsorption capacity of uranium(VI) have been achieved at the mentioned conditions. The rate constant for the chemical adsorption of uranium(VI) was 0.988 g mg{sup -1} min{sup -1} calculated by the pseudo-second order rate equation. The obtained thermodynamics parameters showed that uranium(VI) adsorption from H{sub 3}PO{sub 4} is an exothermic and spontaneous process.

  20. Extraction of surface plasmons in organic light-emitting diodes via high-index coupling.

    Science.gov (United States)

    Scholz, Bert J; Frischeisen, Jörg; Jaeger, Arndt; Setz, Daniel S; Reusch, Thilo C G; Brütting, Wolfgang

    2012-03-12

    The efficiency of organic light-emitting diodes (OLEDs) is still limited by poor light outcoupling. In particular, the excitation of surface plasmon polaritons (SPPs) at metal-organic interfaces represents a major loss channel. By combining optical simulations and experiments on simplified luminescent thin-film structures we elaborate the conditions for the extraction of SPPs via coupling to high-index media. As a proof-of-concept, we demonstrate the possibility to extract light from wave-guided modes and surface plasmons in a top-emitting white OLED by a high-index prism.

  1. Study of phase separation in liquid-liquid systems using LIX 984N in organic phase; Estudio de separacion de fases en sistemas liquido-liquido usando LIX 984N en fase organica

    Energy Technology Data Exchange (ETDEWEB)

    Castillo-Segura, J.; Biela-Cornejo, F.; Navarro-Donoso, P.

    2012-11-01

    In this work we studied the sedimentation and coalescence phenomena in liquid-liquid dispersion without chemical reaction, the aqueous electrolyte consisted of 0.25 M sodium sulfate and an organic phase characteristic organic extractant for copper (LIX 984N) diluted in a commercial solvent (Shellsol 24 AR). The phenomena that dominate the phase separation have been studied by several researchers, which proposed a number of models to predict sedimentation and coalescence profiles. In this work we applied a semi-empirical model to describe the phenomena involved, varying the following experimental conditions: percentage of extractant in organic phase (5 - 30 % v / v), continuous phase (aqueous and organic), time and stirring speed (30 - 1800 s and 400 - 1200 rpm respectively). The main results show that from the 800 rpm of agitation this variable has no influence on primary breakup time, in the same way for 180 seconds of stirring produces the same effect. The fraction of dispersed phase in the packing zone found was 0.74. For higher levels of percentage of extractant in organic phase increased the phase separation time as when the organic phase was used as the continuous phase relative to the aqueous phase. We found a partial adjustment of the experimental data in relation to the simulated values , which is attributable to two factors: the initial inertia of the system once the agitation stopped and the existence of different times of inflection points of the curves of sedimentation and coalescence. In the different articles found in literature assume that the above phenomena occur simultaneously. (Author) 16 refs.

  2. Determination of organophosphorus pesticides using molecularly imprinted polymer solid phase extraction

    International Nuclear Information System (INIS)

    Mohd Marsin Sanagi; Syairah Salleh; Wan Aini Wan Ibrahim

    2011-01-01

    Molecularly imprinted polymer solid phase extraction (MIP-SPE) method has been developed for the determination of organophosphorus pesticides (OPPs) in water samples. The MIP was prepared by thermo-polymerization method using methacrylic acid (MAA) as functional monomer, ethylene glycol dimethacrylate (EGDMA) as crosslinker, acetonitrile as porogenic solvent and quinalphos as the template molecule. The three OPPs (diazinon, quinalphos and chloropyrifos) were selected as target analytes as they are widely used in agriculture sector. Various parameters affecting the extraction efficiency of the imprinted polymers have been evaluated to optimize the selective preconcentration of OPPs from aqueous samples. The characteristics of the MIP-SPE method were validated by high performance liquid chromatography (HPLC). The accuracy and selectivity of the MIP-SPE process developed were verified using non-imprinted polymer solid phase extraction (NIP-SPE) and a commercial C 18 -SPE was used for comparison. The recoveries of the target analytes obtained using the MIPs as the solid phase sorbent ranged from 83% to 98% (RSDs 1.05 - 1.98 %; n=3) for water sample. The developed MIP-SPE method demonstrates that it could be applied for the determination of OPPs in water samples. (author)

  3. Determination of Iron Species by Combination of Solvent Assisted-Dispersive Solid Phase Extraction and Spectrophotometry

    Directory of Open Access Journals (Sweden)

    Zahra Dehghani

    2015-06-01

    Full Text Available A simple, rapid and sensitive solvent assisted-dispersive solid phase extraction method was developed for the extraction of iron(II prior to its spectrophotometric determination. The Fe(II reacted with 2,4,6-tris(2-pyridyl-1,3,5-triazine, neutralized with sodium dodecyl sulfate and extracted onto the fine particles of benzophenone which were formed upon rapid injection of a mixture of benzophenone as the sorbent and ethanol as the disperser solvent into the aqueous solution. After phase separation, the sedimented phase containing the complex was dissolved in ethanol and the analyte concentration was determined by measuring its absorption at 594 nm. Total iron was determined after the reduction of Fe(III to Fe(II with hydroxylamine hydrochloride. Under the optimized conditions, an enhancement factor of 32, the detection limit of 0.16 µg l-1, and the relative standard deviation of 1.9% (n = 6 at 20 µg l-1 concentration level of Fe(II were achieved. The method was successfully applied to the determination of iron species in water samples and total iron in infant dry formula milk, apple, rice, spinach and parsley samples.

  4. A Simple Method for Automated Solid Phase Extraction of Water Samples for Immunological Analysis of Small Pollutants.

    Science.gov (United States)

    Heub, Sarah; Tscharner, Noe; Kehl, Florian; Dittrich, Petra S; Follonier, Stéphane; Barbe, Laurent

    2016-01-01

    A new method for solid phase extraction (SPE) of environmental water samples is proposed. The developed prototype is cost-efficient and user friendly, and enables to perform rapid, automated and simple SPE. The pre-concentrated solution is compatible with analysis by immunoassay, with a low organic solvent content. A method is described for the extraction and pre-concentration of natural hormone 17β-estradiol in 100 ml water samples. Reverse phase SPE is performed with octadecyl-silica sorbent and elution is done with 200 µl of methanol 50% v/v. Eluent is diluted by adding di-water to lower the amount of methanol. After preparing manually the SPE column, the overall procedure is performed automatically within 1 hr. At the end of the process, estradiol concentration is measured by using a commercial enzyme-linked immune-sorbent assay (ELISA). 100-fold pre-concentration is achieved and the methanol content in only 10% v/v. Full recoveries of the molecule are achieved with 1 ng/L spiked de-ionized and synthetic sea water samples.

  5. Determination of catechins and catechin gallates in tissues by liquid chromatography with coulometric array detection and selective solid phase extraction.

    Science.gov (United States)

    Chu, Kai On; Wang, Chi Chiu; Chu, Ching Yan; Rogers, Michael Scott; Choy, Kwong Wai; Pang, Chi Pui

    2004-10-25

    Catechins levels in organ tissues, particularly liver, determined by published methods are unexpectedly low, probably due to the release of oxidative enzymes, metal ions and reactive metabolites from tissue cells during homogenization and to the pro-oxidant effects of ascorbic acid during sample processing in the presence of metal ions. We describe a new method for simultaneous analysis of eight catechins in tissue: (+)-catechin (C), (-)-epicatechin (EC), (-)-gallocatechin (GC), (-)-epigallocatechin (EGC), (-)-catechin gallate (CG), (-)-epicatechin gallate (ECG), (-)-gallocatechin gallate (GCG) and (-)-epigallocatechin gallate (EGCG) (Fig. 1). The new extraction procedure utilized a methanol/ethylacetate/dithionite (2:1:3) mixture during homogenization for simultaneous enzyme precipitation and antioxidant protection. Selective solid phase extraction was used to remove most interfering bio-matrices. Reversed phase HPLC with CoulArray detection was used to determine the eight catechins simultaneously within 25 min. Good linearity (>0.9922) was obtained in the range 20-4000 ng/g. The coefficients of variance (CV) were less than 5%. Absolute recovery ranged from 62 to 96%, accuracy 92.5 +/- 4.5 to 104.9 +/- 6%. The detection limit was 5 ng/g. This method is capable for determining catechins in rat tissues of liver, brain, spleen, and kidney. The method is robust, reproducible, with high recovery, and has been validated for both in vitro and in vivo sample analysis.

  6. Solid-Phase Extraction of Sulfur Mustard Metabolites Using an Activated Carbon Fiber Sorbent.

    Science.gov (United States)

    Lee, Jin Young; Lee, Yong Han

    2016-01-01

    A novel solid-phase extraction method using activated carbon fiber (ACF) was developed and validated. ACF has a vast network of pores of varying sizes and microporous structures that result in rapid adsorption and selective extraction of sulfur mustard metabolites according to the pH of eluting solvents. ACF could not only selectively extract thiodiglycol and 1-methylsulfinyl-2-[2-(methylthio)-ethylsulfonyl]ethane eluting a 9:1 ratio of dichloromethane to acetone, and 1,1'-sulfonylbis[2-(methylsulfinyl)ethane] and 1,1'-sulfonylbis- [2-S-(N-acetylcysteinyl)ethane] eluting 3% hydrogen chloride in methanol, but could also eliminate most interference without loss of analytes during the loading and washing steps. A sample preparation method has been optimized for the extraction of sulfur mustard metabolites from human urine using an ACF sorbent. The newly developed extraction method was applied to the trace analysis of metabolites of sulfur mustard in human urine matrices in a confidence-building exercise for the analysis of biomedical samples provided by the Organisation for the Prohibition of Chemical Weapons. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  7. Searching for life on Mars: degradation of surfactant solutions used in organic extraction experiments.

    Science.gov (United States)

    Court, Richard W; Sims, Mark R; Cullen, David C; Sephton, Mark A

    2014-09-01

    Life-detection instruments on future Mars missions may use surfactant solutions to extract organic matter from samples of martian rocks. The thermal and radiation environments of space and Mars are capable of degrading these solutions, thereby reducing their ability to dissolve organic species. Successful extraction and detection of biosignatures on Mars requires an understanding of how degradation in extraterrestrial environments can affect surfactant performance. We exposed solutions of the surfactants polysorbate 80 (PS80), Zonyl FS-300, and poly[dimethylsiloxane-co-[3-(2-(2-hydroxyethoxy)ethoxy)propyl]methylsiloxane] (PDMSHEPMS) to elevated radiation and heat levels, combined with prolonged storage. Degradation was investigated by measuring changes in pH and electrical conductivity and by using the degraded solutions to extract a suite of organic compounds spiked onto grains of the martian soil simulant JSC Mars-1. Results indicate that the proton fluences expected during a mission to Mars do not cause significant degradation of surfactant compounds. Solutions of PS80 or PDMSHEPMS stored at -20 °C are able to extract the spiked standards with acceptable recovery efficiencies. Extraction efficiencies for spiked standards decrease progressively with increasing temperature, and prolonged storage at 60°C renders the surfactant solutions ineffective. Neither the presence of ascorbic acid nor the choice of solvent unequivocally alters the efficiency of extraction of the spiked standards. Since degradation of polysorbates has the potential to produce organic compounds that could be mistaken for indigenous martian organic matter, the polysiloxane PDMSHEPMS may be a superior choice of surfactant for the exploration of Mars.

  8. Overestimation of organic phosphorus in wetland soils by alkaline extraction and molybdate colorimetry.

    Science.gov (United States)

    Turner, Benjamin L; Newman, Susan; Reddy, K Ramesh

    2006-05-15

    Accurate information on the chemical nature of soil phosphorus is essential for understanding its bioavailability and fate in wetland ecosystems. Solution phosphorus-31 nuclear magnetic resonance (31P NMR) spectroscopy was used to assess the conventional colorimetric procedure for phosphorus speciation in alkaline extracts of organic soils from the Florida Everglades. Molybdate colorimetry markedly overestimated organic phosphorus by between 30 and 54% compared to NMR spectroscopy. This was due in large part to the association of inorganic phosphate with organic matter, although the error was exacerbated in some samples by the presence of pyrophosphate, an inorganic polyphosphate that is not detected by colorimetry. The results have important implications for our understanding of phosphorus biogeochemistry in wetlands and suggest that alkaline extraction and solution 31p NMR spectroscopy is the only accurate method for quantifying organic phosphorus in wetland soils.

  9. Solvent extraction of aurocyanide by extractant CTMAB and TBP

    International Nuclear Information System (INIS)

    Yan Wenfei; Zhang Tianxi; Wu Jinguang

    2000-01-01

    A novel extraction system using KAu(CN) 2 -CTMAB as aqueous phase and 30% TBP-dodecane as organic phase is studied by 198 Au radioactive tracer and FT-IR spectroscopy. The results show that the organic phase separates into two phases, when the gold concentration is bigger than 20 g/L. From the analysis of FT-IR it is seen that the most of gold is in the lower organic phase

  10. Determination of basicity of neutral organic phosphorus extractants in nonpolar solvents by the 31P NMR method

    International Nuclear Information System (INIS)

    Yakshin, V.V.; Meshcheryakov, N.M.; Il'in, E.G.; Ignatov, M.E.; Laskorin, B.N.

    1984-01-01

    The variant of the NMR method application is developed for quantitative description of acidic-basic properties of neutral organic phosphorus extractants, R 3 P--O (NPE), in non-polar organic solvents. For the NPE basicity determination the dependence of the chemical shift value in NMR 31 P spectra of 0.1 M NPE solutions in the dodecane on sulfuric acid acitivity in aqueous phase at 0-12 M acidity is studied. The linear equation relating NPE basicity and electronic structure of these compounds expressed through the sum: of Kabachnik reaction constants is derived. Linear dependences between the NPE basicity value in dodecane and NPE basicity in nitromethane as well as enthalpies of complexes formation with charge transport with standard acid-iodine in heptane, enthalpies of hydrogen complexes formation with phenol and water have been found

  11. Monitoring of chloropesticide methoxychlor preconcentration from waste water using hplc - solid phase extraction (abstract)

    International Nuclear Information System (INIS)

    Butt, S.B.; Saqlin, M.; Riaz, M.

    2011-01-01

    The method involves preconcentration of methoxychlor by solid phase extraction (SPE) with 1 mL silica based C-18 and 3 mL polymer based C-18 cartridge and then quantification by high performance liquid chromatography with UV detector (HPLC-UV). Optimization of HPLC parameters was done by determining max of methoxychlor on a double beam UV/Visible spectrophotometer, flow rate of mobile phase on reversed phase columns. Lowest detection limit for methoxychlor dissolved in water and methanol was 0.2ppm and 0.1ppm respectively. For solid phase extraction recovery studies and effect of different parameters such as initial concentration of analyte 0.01 to 0.05 ppm, loading rate 1 and 2mL/min, nature of desorbing solvent (methanol, ethyl acetate and acetonitrile) were investigated. Periodic self degradation of methoxychlor, and reusing potential of both SPE materials was also explored. Lower initial concentrations and slower loading rate of methoxychlor solutions gave improved recoveries. Recoveries were in the range of 80 to 90% for new SPE cartridge and reduced to 35 to 57% for once used silica based C-18 tubes. It was around 73 % for HLB C18 on their second use, and decreased on their repeated reuse. Lastly recoveries for stimulant and real waste water samples were determined to be 77 and 60% respectively. (author)

  12. Mode extraction on wind turbine blades via phase-based video motion estimation

    Science.gov (United States)

    Sarrafi, Aral; Poozesh, Peyman; Niezrecki, Christopher; Mao, Zhu

    2017-04-01

    In recent years, image processing techniques are being applied more often for structural dynamics identification, characterization, and structural health monitoring. Although as a non-contact and full-field measurement method, image processing still has a long way to go to outperform other conventional sensing instruments (i.e. accelerometers, strain gauges, laser vibrometers, etc.,). However, the technologies associated with image processing are developing rapidly and gaining more attention in a variety of engineering applications including structural dynamics identification and modal analysis. Among numerous motion estimation and image-processing methods, phase-based video motion estimation is considered as one of the most efficient methods regarding computation consumption and noise robustness. In this paper, phase-based video motion estimation is adopted for structural dynamics characterization on a 2.3-meter long Skystream wind turbine blade, and the modal parameters (natural frequencies, operating deflection shapes) are extracted. Phase-based video processing adopted in this paper provides reliable full-field 2-D motion information, which is beneficial for manufacturing certification and model updating at the design stage. The phase-based video motion estimation approach is demonstrated through processing data on a full-scale commercial structure (i.e. a wind turbine blade) with complex geometry and properties, and the results obtained have a good correlation with the modal parameters extracted from accelerometer measurements, especially for the first four bending modes, which have significant importance in blade characterization.

  13. Evaluation of Anaerobic Biodegradation of Organic Carbon Extracted from Aquifer Sediment

    OpenAIRE

    Kelly, Catherine Aileen

    2006-01-01

    In conjunction with ongoing studies to develop a method for quantifying potentially biodegradable organic carbon (Rectanus et al 2005), this research was conducted to evaluate the extent to which organic carbon extracted using this method will biodegrade in anaerobic environments. The ultimate goal is to use this method for the evaluation of chloroethene contaminated sites in order to estimate the long-term sustainability of monitored natural attenuation (MNA) as a remediation strategy. Alt...

  14. The Use of TOC Reconciliation as a Means of Establishing the Degree to Which Chromatographic Screening of Plastic Material Extracts for Organic Extractables Is Complete.

    Science.gov (United States)

    Jenke, Dennis; Couch, Thomas R; Robinson, Sarah J; Volz, Trent J; Colton, Raymond H

    2014-01-01

    Extracts of plastic packaging, manufacturing, and delivery systems (or their materials of construction) are analyzed by chromatographic methods to establish the system's extractables profile. The testing strategy consists of multiple orthogonal chromatographic methods, for example, gas and liquid chromatography with multiple detection strategies. Although this orthogonal testing strategy is comprehensive, it is not necessarily complete and members of the extractables profile can elude detection and/or accurate identification/quantification. Because the chromatographic methods rarely indicate that some extractables have been missed, another means of assessing the completeness of the profiling activity must be established. If the extracts are aqueous and contain no organic additives (e.g., pH buffers), then they can be analyzed for their total organic carbon content (TOC). Additionally, the TOC of an extract can be calculated based on the extractables revealed by the screening analyses. The measured and calculated TOC can be reconciled to establish the completeness and accuracy of the extractables profile. If the reconciliation is poor, then the profile is either incomplete or inaccurate and additional testing is needed to establish the complete and accurate profile. Ten test materials and components of systems were extracted and their extracts characterized for organic extractables using typical screening procedures. Measured and calculated TOC was reconciled to establish the completeness of the revealed extractables profile. When the TOC reconciliation was incomplete, the profiling was augmented with additional analytical testing to reveal the missing members of the organic extractables profile. This process is illustrated via two case studies involving aqueous extracts of sterile filters. Plastic materials and systems used to manufacture, contain, store, and deliver pharmaceutical products are extracted and the extracts analyzed to establish the materials' (or

  15. Comparative study of hypoglycemic and antibacterial activity of organic extracts of four Bangladeshi plants

    Directory of Open Access Journals (Sweden)

    Mohammad Shah Hafez Kabir

    2016-03-01

    Full Text Available Objective: To examine hypoglycemic and antibacterial activity against some Gram-positive and Gram-negative bacteria of organic extracts of four Bangladeshi plants. Methods: An in vivo hypoglycemic effect on mice model was used to check the hypoglycemic effect of four Bangladeshi herbal organic extracts viz., roots of Curculigo recurvata W. T. Aiton (Satipata (C. recurvata, leaf of Amorphophallus bulbifer Roxb. (Olkachu (A. bulbifer, whole plant of Thunbergia grandiflora Roxb. (Nillata (T. grandiflora and leaf of Steudnera colocasiifolia K. Koch (Yunnan (S. colocasiifolia using glibenclamide as a positive control and water as a negative control. They were also tested for antibacterial activity on three Grampositive and four Gram-negative bacteria by disk diffusion method. C. recurvata, A. bulbifer and T. grandiflora were extracted with methanol and S. colocasiifolia was extracted with ethanol. Results: Among all the plant extract, only ethanol extract of S. colocasiifolia leaves at 800 mg/ kg dose significantly (P < 0.01 reduced fasting glucose level in normal mice as compared to standard drug glibenclamide (5 mg/kg. Ethanol extract of S. colocasiifolia leaves at 800 mg/ kg dose decreased 20.28% of blood glucose level after 2 h of administration in normal mice, where glibenclamide decreased 39.63%. Methanol extract of T. grandiflra didn’t show any zone of inhibition against the tested bacteria, but other three extracts showed a wide range of zone of inhibition. However, none of the extract showed antibacterial activity against all the tested bacteria. Methanol extract of C. recurvata showed maximum zone of inhibition against Bacillus cereus [(10.50 ± 0.50 mm], Salmonella typhi [(16.20 ± 1.26 mm], Escherichia coli [(13.00 ± 1.00 mm] and ethanol extract of S. colocasiifolia showed maximum zone of inhibition against Staphylococcus aureus [(11.20 ± 1.26 (mm], Bacillus subtilis [(12.00 ± 0.50 (mm], Salmonella paratyphi [(10.80 ± 0.29 (mm

  16. Automated Solid Phase Extraction (SPE) LC/NMR Applied to the Structural Analysis of Extractable Compounds from a Pharmaceutical Packaging Material of Construction.

    Science.gov (United States)

    Norwood, Daniel L; Mullis, James O; Davis, Mark; Pennino, Scott; Egert, Thomas; Gonnella, Nina C

    2013-01-01

    The structural analysis (i.e., identification) of organic chemical entities leached into drug product formulations has traditionally been accomplished with techniques involving the combination of chromatography with mass spectrometry. These include gas chromatography/mass spectrometry (GC/MS) for volatile and semi-volatile compounds, and various forms of liquid chromatography/mass spectrometry (LC/MS or HPLC/MS) for semi-volatile and relatively non-volatile compounds. GC/MS and LC/MS techniques are complementary for structural analysis of leachables and potentially leachable organic compounds produced via laboratory extraction of pharmaceutical container closure/delivery system components and corresponding materials of construction. Both hyphenated analytical techniques possess the separating capability, compound specific detection attributes, and sensitivity required to effectively analyze complex mixtures of trace level organic compounds. However, hyphenated techniques based on mass spectrometry are limited by the inability to determine complete bond connectivity, the inability to distinguish between many types of structural isomers, and the inability to unambiguously determine aromatic substitution patterns. Nuclear magnetic resonance spectroscopy (NMR) does not have these limitations; hence it can serve as a complement to mass spectrometry. However, NMR technology is inherently insensitive and its ability to interface with chromatography has been historically challenging. This article describes the application of NMR coupled with liquid chromatography and automated solid phase extraction (SPE-LC/NMR) to the structural analysis of extractable organic compounds from a pharmaceutical packaging material of construction. The SPE-LC/NMR technology combined with micro-cryoprobe technology afforded the sensitivity and sample mass required for full structure elucidation. Optimization of the SPE-LC/NMR analytical method was achieved using a series of model compounds

  17. The development of quantitative determination method of organic acids in complex poly herbal extraction

    Directory of Open Access Journals (Sweden)

    I. L. Dyachok

    2016-08-01

    Full Text Available Aim. The development of sensible, economical and expressive method of quantitative determination of organic acids in complex poly herbal extraction counted on izovaleric acid with the use of digital technologies. Materials and methods. Model complex poly herbal extraction of sedative action was chosen as a research object. Extraction is composed of these medical plants: Valeriana officinalis L., Crataégus, Melissa officinalis L., Hypericum, Mentha piperita L., Húmulus lúpulus, Viburnum. Based on chemical composition of plant components, we consider that main pharmacologically active compounds, which can be found in complex poly herbal extraction are: polyphenolic substances (flavonoids, which are contained in Crataégus, Viburnum, Hypericum, Mentha piperita L., Húmulus lúpulus; also organic acids, including izovaleric acid, which are contained in Valeriana officinalis L., Mentha piperita L., Melissa officinalis L., Viburnum; the aminoacid are contained in Valeriana officinalis L. For the determination of organic acids content in low concentration we applied instrumental method of analysis, namely conductometry titration which consisted in the dependences of water solution conductivity of complex poly herbal extraction on composition of organic acids. Result. The got analytical dependences, which describes tangent lines to the conductometry curve before and after the point of equivalence, allow to determine the volume of solution expended on titration and carry out procedure of quantitative determination of organic acids in the digital mode. Conclusion. The proposed method enables to determine the point of equivalence and carry out quantitative determination of organic acids counted on izovaleric acid with the use of digital technologies, that allows to computerize the method on the whole.

  18. 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)

  19. Synthesis of surface Cr (VI)-imprinted magnetic nanoparticles for selective dispersive solid-phase extraction and determination of Cr (VI) in water samples.

    Science.gov (United States)

    Qi, Xue; Gao, Shuang; Ding, Guosheng; Tang, An-Na

    2017-01-01

    A facile, rapid and selective magnetic dispersed solid-phase extraction (dSPE) method for the extraction and enrichment of Cr (VI) prior to flame atomic absorption spectrometry (AAS) was introduced. For highly selective and efficient extraction, magnetic Cr (VI)-imprinted nanoparticles (Fe 3 O 4 @ Cr (VI) IIPs) were prepared by hyphenating surface ion-imprinted with sol-gel techniques. In the preparation process, chromate (Cr(VI)) was used as the template ion; vinylimidazole and 3-aminopropyltriethoxysilane were selected as organic functional monomer and co-monomer respectively. Another reagent, methacryloxypropyltrimethoxysilane was adopted as coupling agent to form the stable covalent bonding between organic and inorganic phases. The effects of various parameters on the extraction efficiency, such as pH of sample solution, the amount of adsorbent, extraction time, the type and concentration of eluent were systematically investigated. Furthermore, the thermodynamic and kinetic properties of the adsorption process were studied to explore the internal adsorption mechanism. Under optimized conditions, the preconcentration factor, limit of detection and linear range of the established dSPE-AAS method for Cr (VI) were found to be 98, 0.29μgL -1 and 4-140μgL -1 , respectively. The developed method was also successfully applied to the analysis of Cr (VI) in different water samples with satisfactory results, proving its reliability and feasibility in real sample analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Evaluation of single-walled carbon nanohorns as sorbent in dispersive micro solid-phase extraction

    Energy Technology Data Exchange (ETDEWEB)

    Jimenez-Soto, Juan Manuel; Cardenas, Soledad [Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus de Rabanales, University of Cordoba, 14071 Cordoba (Spain); Valcarcel, Miguel, E-mail: qa1meobj@uco.es [Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus de Rabanales, University of Cordoba, 14071 Cordoba (Spain)

    2012-02-10

    Highlights: Black-Right-Pointing-Pointer The potential of single walled carbon nanohorns in dispersive solid phase microextraction has been evaluated. Black-Right-Pointing-Pointer The method was characterized for the extraction of PAHs from waters. Black-Right-Pointing-Pointer Single walled carbon nanohorns were better extractant than carbon nanotubes and carbon nanocones. Black-Right-Pointing-Pointer The limits of detection were adequate for the target analytes in environmental waters. - Abstract: A new dispersive micro solid-phase extraction method which uses single-walled carbon nanohorns (SWNHs) as sorbent is proposed. The procedure combines the excellent sorbent properties of the nanoparticles with the efficiency of the dispersion of the material in the sample matrix. Under these conditions, the interaction with the analytes is maximized. The determination of polycyclic aromatic hydrocarbons was selected as model analytical problem. Two dispersion strategies were evaluated, being the functionalization via microwave irradiation better than the use of a surfactant. The extraction was accomplished by adding 1 mL of oxidized SWHNs (o-SWNHs) dispersion to 10 mL of water sample. After extraction, the mixture was passed through a disposable Nylon filter were the nanoparticles enriched with the PAHs were retained. The elution was carried out with 100 {mu}L of hexane. The limits of detection achieved were between 30 and 60 ng L{sup -1} with a precision (as repeatability) better than 12.5%. The recoveries obtained for the analytes in three different water samples were acceptable in all instances. The performance of o-SWNHs was favourably compared with that provided by carboxylated single-walled carbon nanotubes and thermally treated carbon nanocones.

  1. Remediation of soils, sediments and sludges by extraction with organic solvents

    NARCIS (Netherlands)

    Noordkamp, E.R.

    1999-01-01

    Remediation of contaminated soils, sediments and sludges by extraction with organic solvents is still in the initial stages of development. So far hardly any scientific research has been carried out into this approach. Therefore, the main objective of the present investigation was to study

  2. Removal of H2S and volatile organic sulfur compounds by silicone membrane extraction

    NARCIS (Netherlands)

    Manconi, I.; Lens, P.N.L.

    2009-01-01

    BACKGROUND: This study explores an alternative process for the abatement and/or desulfurization of H2S and volatile organic sulfur compounds (VOSC) containing waste streams, which employs a silicone-based membrane to simultaneously remove H2S and VOSC. An extractive membrane reactor allows the

  3. Mixing in three-phase systems: Implications for enhanced oil recovery and unconventional gas extraction

    Science.gov (United States)

    Jimenez-Martinez, J.; Porter, M. L.; Hyman, J.; Carey, J. W.; Viswanathan, H. S.

    2015-12-01

    Although the mixing of fluids within a porous media is a common process in natural and industrial systems, how the degree of mixing depends on the miscibility of multiple phases is poorly characterized. Often, the direct consequence of miscible mixing is the modification of the resident fluid (brine and hydrocarbons) rheological properties. We investigate supercritical (sc)CO2 displacement and mixing processes in a three-phase system (scCO2, oil, and H2O) using a microfluidics experimental system that accommodates the high pressures and temperatures encountered in fossil fuel extraction operations. The miscibility of scCO2 with the resident fluids, low with aqueous solutions and high with hydrocarbons, impacts the mixing processes that control sweep efficiency in enhanced oil recovery (EOR) and the unlocking of the system in unconventional oil and gas extraction. Using standard volume-averaging techniques we upscale the aqueous phase saturation to the field-scale (i.e., Darcy scale) and interpret the results as a simpler two-phase system. This process allows us to perform a statistical analysis to quantify i) the degree of heterogeneity in the system resulting from the immiscible H2O and ii) how that heterogeneity impacts mixing between scCO2 and oil and their displacement. Our results show that when scCO2 is used for miscible displacement, the presence of an aqueous solution, which is common in secondary and tertiary EOR and unconventional oil and gas extraction, strongly impacts the mixing of scCO2 with the hydrocarbons due to low scCO2-H2O miscibility. H2O, which must be displaced advectively by the injected scCO2, introduces spatio-temporal variability into the system that acts as a barrier between the two miscibile fluids. This coupled with the effect of viscosity contrast, i.e., viscous fingering, has an impact on the mixing of the more miscible pair.

  4. Dual-wavelength phase-shifting digital holography selectively extracting wavelength information from wavelength-multiplexed holograms.

    Science.gov (United States)

    Tahara, Tatsuki; Mori, Ryota; Kikunaga, Shuhei; Arai, Yasuhiko; Takaki, Yasuhiro

    2015-06-15

    Dual-wavelength phase-shifting digital holography that selectively extracts wavelength information from five wavelength-multiplexed holograms is presented. Specific phase shifts for respective wavelengths are introduced to remove the crosstalk components and extract only the object wave at the desired wavelength from the holograms. Object waves in multiple wavelengths are selectively extracted by utilizing 2π ambiguity and the subtraction procedures based on phase-shifting interferometry. Numerical results show the validity of the proposed technique. The proposed technique is also experimentally demonstrated.

  5. Study of the Performance of the Organic Extracts of Chenopodium ambrosioides for Ag Nanoparticle Synthesis

    Directory of Open Access Journals (Sweden)

    Luis M. Carrillo-López

    2016-01-01

    Full Text Available There are many ways to obtain metal nanoparticles: biological, physical, and chemical ways and combinations of these approaches. Synthesis assisted with plant extracts has been widely documented. However, one issue that is under discussion refers to the metabolites responsible for reduction and stabilization that confine nanoparticle growth and prevent coalescence between nanoparticles in order to avoid agglomeration/precipitation. In this study, Ag nanoparticles were synthesized using organic extracts of Chenopodium ambrosioides with different polarities (hexane, dichloromethane, and methanol. Each extract was phytochemically characterized to identify the nature of the metabolites responsible for nanoparticle formation. With methanol extract, the compounds responsible for reducing and stabilizing silver nanoparticle were associated with the presence of phenolic compounds (flavonoids and tannins, while, with dichloromethane and hexane extracts, the responsible compounds were mainly terpenoids. Large part of the reducing activity of secondary metabolites in C. ambrosioides is closely related to compounds with antioxidant capacity, such as phenolic compounds (flavone glycoside and isorhamnetin, which are the main constituents of the methanol extracts. Otherwise, terpenoids (trans-diol, α-terpineol, monoterpene hydroperoxides, and apiole are the central metabolites present in dichloromethane and hexane extracts.

  6. 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.

  7. Development of andrographolide molecularly imprinted polymer for solid-phase extraction

    Science.gov (United States)

    Yin, Xiaoying; Liu, Qingshan; Jiang, Yifan; Luo, Yongming

    2011-06-01

    A method employing molecularly imprinted polymer (MIP) as selective sorbent for solid-phase extraction (SPE) to pretreat samples was developed. The polymers were prepared by precipitation polymerization with andrographolide as template molecule. The structure of MIP was characterized and its static adsorption capacity was measured by the Scatchard equation. In comparison with C 18-SPE and non-imprinted polymer (NIP) SPE column, MIP-SPE column displays high selectivity and good affinity for andrographolide and dehydroandrographolide for extract of herb Andrographis paniculata ( Burm.f.) Nees (APN). MIP-SPE column capacity was 11.9 ± 0.6 μmol/g and 12.1 ± 0.5 μmol/g for andrographolide and dehydroandrographolide, respectively and was 2-3 times higher than that of other two columns. The precision and accuracy of the method developed were satisfactory with recoveries between 96.4% and 103.8% (RSD 3.1-4.3%, n = 5) and 96.0% and 104.2% (RSD 2.9-3.7%, n = 5) for andrographolide and dehydroandrographolide, respectively. Various real samples were employed to confirm the feasibility of method. This developed method demonstrates the potential of molecularly imprinted solid phase extraction for rapid, selective, and effective sample pretreatment.

  8. EEMD Independent Extraction for Mixing Features of Rotating Machinery Reconstructed in Phase Space

    Directory of Open Access Journals (Sweden)

    Zaichao Ma

    2015-04-01

    Full Text Available Empirical Mode Decomposition (EMD, due to its adaptive decomposition property for the non-linear and non-stationary signals, has been widely used in vibration analyses for rotating machinery. However, EMD suffers from mode mixing, which is difficult to extract features independently. Although the improved EMD, well known as the ensemble EMD (EEMD, has been proposed, mode mixing is alleviated only to a certain degree. Moreover, EEMD needs to determine the amplitude of added noise. In this paper, we propose Phase Space Ensemble Empirical Mode Decomposition (PSEEMD integrating Phase Space Reconstruction (PSR and Manifold Learning (ML for modifying EEMD. We also provide the principle and detailed procedure of PSEEMD, and the analyses on a simulation signal and an actual vibration signal derived from a rubbing rotor are performed. The results show that PSEEMD is more efficient and convenient than EEMD in extracting the mixing features from the investigated signal and in optimizing the amplitude of the necessary added noise. Additionally PSEEMD can extract the weak features interfered with a certain amount of noise.

  9. Solid phase extraction of magnetic carbon doped Fe3O4 nanoparticles.

    Science.gov (United States)

    Yang, Jing; Li, Jia-yuan; Qiao, Jun-qin; Lian, Hong-zhen; Chen, Hong-yuan

    2014-01-17

    Carbon decorated Fe3O4 nanoparticles (Fe3O4/C) are promising magnetic solid-phase extraction (MSPE) sorbents in environmental and biological analysis. Fe3O4/C based MSPE method shows advantages of easy operation, rapidness, high sensitivity, and environmental friendliness. In this paper, the MSPE mechanism of Fe3O4/C nanoparticles has been comprehensively investigated, for the first time, through the following three efforts: (1) the comparison of extraction efficiency for polycyclic aromatic hydrocarbons (PAHs) between the Fe3O4/C sorbents and activated carbon; (2) the chromatographic retention behaviors of hydrophobic and hydrophilic compounds on Fe3O4/C nanoparticles as stationary phase; (3) related MSPE experiments for several typical compounds such as pyrene, naphthalene, benzene, phenol, resorcinol, anisole and thioanisole. It can be concluded that there are hybrid hydrophobic interaction and hydrogen bonding interaction or dipole-dipole attraction between Fe3O4/C sorbents and analytes. It is the existence of carbon and oxygen-containing functional groups coated on the surface of Fe3O4/C nanoparticles that is responsible for the effective extraction process. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. Improved detection limits for phthalates by selective solid-phase micro-extraction

    KAUST Repository

    Zia, Asif I.

    2016-03-30

    Presented research reports on an improved method and enhanced limits of detection for phthalates; a hazardous additive used in the production of plastics by solid-phase micro-extraction (SPME) polymer in comparison to molecularly imprinted solid-phase extraction (MISPE) polymer. The polymers were functionalized on an interdigital capacitive sensor for selective binding of phthalate molecules from a complex mixture of chemicals. Both polymers owned predetermined selectivity by formation of valuable molecular recognition sites for Bis (2-ethylhexyl) phthalate (DEHP). Polymers were immobilized on planar electrochemical sensor fabricated on a single crystal silicon substrate with 500 nm sputtered gold electrodes fabricated using MEMS fabrication techniques. Impedance spectra were obtained using electrochemical impedance spectroscopy (EIS) to determine sample conductance for evaluation of phthalate concentration in the spiked sample solutions with various phthalate concentrations. Experimental results revealed that the ability of SPME polymer to adsorb target molecules on the sensing surface is better than that of MISPE polymer for phthalates in the sensing system. Testing the extracted samples using high performance liquid chromatography with photodiode array detectors validated the results.

  11. NEMO: Extraction and normalization of organization names from PubMed affiliations.

    Science.gov (United States)

    Jonnalagadda, Siddhartha Reddy; Topham, Philip

    2010-10-04

    Today, there are more than 18 million articles related to biomedical research indexed in MEDLINE, and information derived from them could be used effectively to save the great amount of time and resources spent by government agencies in understanding the scientific landscape, including key opinion leaders and centers of excellence. Associating biomedical articles with organization names could significantly benefit the pharmaceutical marketing industry, health care funding agencies and public health officials and be useful for other scientists in normalizing author names, automatically creating citations, indexing articles and identifying potential resources or collaborators. Large amount of extracted information helps in disambiguating organization names using machine-learning algorithms. We propose NEMO, a system for extracting organization names in the affiliation and normalizing them to a canonical organization name. Our parsing process involves multi-layered rule matching with multiple dictionaries. The system achieves more than 98% f-score in extracting organization names. Our process of normalization that involves clustering based on local sequence alignment metrics and local learning based on finding connected components. A high precision was also observed in normalization. NEMO is the missing link in associating each biomedical paper and its authors to an organization name in its canonical form and the Geopolitical location of the organization. This research could potentially help in analyzing large social networks of organizations for landscaping a particular topic, improving performance of author disambiguation, adding weak links in the co-author network of authors, augmenting NLM's MARS system for correcting errors in OCR output of affiliation field, and automatically indexing the PubMed citations with the normalized organization name and country. Our system is available as a graphical user interface available for download along with this paper.

  12. Comparison of different types of coatings in headspace solid phase micro extraction for the analysis of pesticide residues in vegetables and fruits

    International Nuclear Information System (INIS)

    Chai, Mee Kin; Tan, Guan Huat

    2008-01-01

    Despite the continuing development of solid-phase micro extraction (SPME) fiber coatings, their selection presents some difficulties for analytes in choosing the appropriate fiber for a particular application. There are many types of SPME coatings available commercially. The most widely used for determination of pesticide residues in vegetable and fruits are polydimethylsiloxane (PDMS) and polyacrylate (PA). A headspace solid phase micro extraction (HS-SPME) procedure using these two commercialized fibers (PDMS and PA) is presented for the determination of selected groups of organo chlorine and organophosphorus pesticides. The extraction performances of these compounds were compared using these two fibers. The optimal experimental procedures for the adsorption and desorption of pesticides were determined. An explanation for the extraction differences is suggested based on the different thickness, polarity of the polymeric film of fibers and the different extracting matrices. In addition, the higher detector response of the pesticides after addition of aliquots of water and an organic solvent to the vegetable and fruit samples are also discussed. The SPME fibers were reusable until a maximum of 120 extractions. Finally, the optimized procedures were applied successfully for the determination of these compounds in vegetable and fruits samples. Mean recoveries for all pesticides were between 75.0-97 % with RSD below 7 %. (author)

  13. [Determination of Arsenic in Food Package Aluminum by Ultrasound Assisted Solid Phase Extraction/ICP-AES].

    Science.gov (United States)

    Qin, Wen-xia; Gong, Qi; Li, Min; Deng, Li-xin; Mo, Li-shu; Li, Yan-lin

    2015-04-01

    Determination of arsenic in pure aluminum by inductively coupled plasma atomic emission spectrometry was interfered by aluminum matrix. The experiment showed that when the mass concentration of Al was greater than or equal to 5 000 times the As in the test solution, the measurement error was greater than 5%. In order to eliminate the interference, strong acid cation exchange fiber (SACEF) was used as solid phase extraction agent to adsorb Al(3+). The extraction conditions included amount of SACEF, extraction time, temperature and pH were investigated. The optimal extraction conditions were that 0.9000 g SACEF was used to extract the aluminum from the sample solution of pH 2.0 at 55 °C for 5 min with the ultrasonic assist, and in this case, the arsenic in the form of arsenic acid was not extracted and left in the solution for the determination. The results showed that after treating 10. 00 mL test solution containing 1.00 µg arsenic and 20.0 mg aluminum, arsenic did not lose. The mass concentration of residual aluminum in the raffinate was about 2,000 times the As, which had not interfered the determination of arsenic. The detection limit (3 s) was 0.027 µg · mL(-1) and quantification limit (10 s) was 0.0091 µg · mL(-1). The proposed method was successfully applied to the separation and determination of arsenic in the synthetic samples, the aluminum cans and the barbecue aluminum foil. Recovery was in the range of 98.3%-105% and RSD (n = 3) was in the range of 0.1%-4.3%. The results showed that the content of arsenic in the aluminum cans and the aluminum barbecue foil was below the limited value of national standard (GB/T 3190-2008).

  14. An absorbing microwave micro-solid-phase extraction device used in non-polar solvent microwave-assisted extraction for the determination of organophosphorus pesticides.

    Science.gov (United States)

    Wang, Ziming; Zhao, Xin; Xu, Xu; Wu, Lijie; Su, Rui; Zhao, Yajing; Jiang, Chengfei; Zhang, Hanqi; Ma, Qiang; Lu, Chunmei; Dong, Deming

    2013-01-14

    A single-step extraction-cleanup method, including microwave-assisted extraction (MAE) and micro-solid-phase extraction (μ-SPE), was developed for the extraction of ten organophosphorus pesticides in vegetable and fruit samples. Without adding any polar solvent, only one kind of non-polar solvent (hexane) was used as extraction solvent in the whole extraction step. Absorbing microwave μ-SPE device, was prepared by packing activated carbon with microporous polypropylene membrane envelope, and used as not only the sorbent in μ-SPE, but also the microwave absorption medium. Some experimental parameters effecting on extraction efficiency was investigated and optimized. 1.0 g of sample, 8 mL of hexane and three absorbing microwave μ-SPE devices were added in the microwave extraction vessel, the extraction was carried out under 400 W irradiation power at 60°C for 10 min. The extracts obtained by MAE-μ-SPE were directly analyzed by GC-MS without any clean-up process. The recoveries were in the range of 93.5-104.6%, and the relative standard deviations were lower than 8.7%. Copyright © 2012 Elsevier B.V. All rights reserved.

  15. Molecular dynamics simulation of cyclodextrin aggregation and extraction of Anthracene from non-aqueous liquid phase

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Xinzhe [Shenzhen Key Laboratory for Coastal Ocean Dynamic and Environment, Division of Ocean Science and Technology, Graduate School at Shenzhen, Tsinghua University, Shenzhen 518055 (China); School of Environment, Tsinghua University, Beijing 100084 (China); Wu, Guozhong [Shenzhen Key Laboratory for Coastal Ocean Dynamic and Environment, Division of Ocean Science and Technology, Graduate School at Shenzhen, Tsinghua University, Shenzhen 518055 (China); Chen, Daoyi, E-mail: chen.daoyi@sz.tsinghua.edu.cn [Shenzhen Key Laboratory for Coastal Ocean Dynamic and Environment, Division of Ocean Science and Technology, Graduate School at Shenzhen, Tsinghua University, Shenzhen 518055 (China)

    2016-12-15

    Cyclodextrin (CD) extraction is widely used for the remediation of polycyclic aromatic hydrocarbons (PAH) pollution, but it remains unclear about the influence of CD aggregation on the PAH transport from non-aqueous liquid phase to water. The atomistic adsorption and complexation of PAHs (32 anthracenes) by CD aggregates (48 β-cyclodextrins) were studied by molecular dynamics simulations at hundreds of nanoseconds time scale. Results indicated that high temperature promoted the βCD aggregation in bulk oil, which was not found in bulk water. Nevertheless, the fractions of anthracenes entrapped inside the βCDs cavity in both scenarios were significantly increased when temperature increased from 298 to 328 K. Free energy calculation for the sub-steps of CD extraction demonstrated that the anthracenes could be extracted when the βCDs arrived at the water-oil interface or after the βCDs entered the bulk oil. The former was kinetic-controlled while the latter was thermodynamic-limited process. Results also highlighted the formation of porous structures by CD aggregates in water, which was able to sequestrate PAH clusters with the size obviously larger than the cavity diameter of individual CD. This provided an opportunity for the extraction of recalcitrant PAHs with molecular size larger than anthracenes by cyclodextrins.

  16. 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.

  17. Solid phase microextraction and stir bar sorptive extraction for organotin compounds - a comparison (P9)

    International Nuclear Information System (INIS)

    Mothes, S.; Wennrich, R.

    2002-01-01

    Full text: Organotin compounds have been largely used in agricultural and industrial applications. Hyphenated techniques were developed for the sensitive and selective determination of such species. For this task GC has been coupled with atomic emission detection. Derivatization to transform the Sn-compounds into sufficiently volatile compounds was necessary and carried out using sodium tetrapropylborate. For sample preparation the application of solid phase microextraction (SPME) give recent advances in comparison to classical liquid-liquid extraction (LEE). A problem in the usage of SPME exists however in the small volume of the PDMS coating for enrichment the analytes. For improvement of both sample enrichment and extraction of the organotin compounds stir bar sorptive extraction (SBSE) was applied. It base on the application of stir bars coated with PDMS. Here the extraction yield is substantially higher. Aim of this study was to compare the capabilities of GC-AED in combination with SPME and SBSE. After optimization of the experimental parameters it was possible to reach detection limits in the pg / 1 - level. A comparison of both methods shows the expected results. By application of SBSE it was possible to increase the detection limits one order of magnitude. With SPME the reproducibility of the analytical results (in the 1 ng / 1 concentration range) was found to be between 10 and 15 %, it could be enhanced to 5-8 % by application of SBSE. These low limits of detection and the good reproducibility allowed the determination of organotin compounds according required regulations. Ref. 1 (author)

  18. Volatile composition of peppermint (Mentha piperita L.) commercial teas through solid phase extraction.

    Science.gov (United States)

    Riachi, L G; Abi-Zaid, I E; Moreira, R F A; De Maria, C A B

    2012-12-01

    Volatiles from aqueous extract of peppermint commercial sachets were investigated through gas chromatography/flame ionization detection (GC/FID) and GC/mass spectrometry (MS). Samples were prepared under similar conditions as in homemade tea. Volatiles were isolated using solid phase extraction method (SPE) with Porapak Q trap followed by desorption with acetone. Estimated mean values for short and medium chain carboxylic acids (C2-C12) and ketones lay in the range of 50-64 microg kg(-1) whilst aliphatic alcohols and acyclic hydrocarbons had values lower than 6 microg kg(-1). The major volatiles were terpenes (275-382 microg kg(-1)) that reached 89 % of the total composition. A total of 16 compounds, among them dodecane, acetoin, acetol, citral, geraniol and octanoic acid have been described by the first time in peppermint tea. These findings could be attributed to the different analytical approach employed, mainly to the use of different extraction/pre-concentration techniques. Given the apparently lower proportion of terpenes in the aqueous extract it may be that the chemical properties of the peppermint essential oil are not entirely reproduced with homemade tea.

  19. Two-Phase Extraction for Comprehensive Analysis of the Plant Metabolome by NMR.

    Science.gov (United States)

    Schripsema, Jan; Dagnino, Denise

    2018-01-01

    Metabolomics is the area of research, which strives to obtain complete metabolic fingerprints, to detect differences between them, and to provide hypothesis to explain those differences [1]. But obtaining complete metabolic fingerprints is not an easy task. Metabolite extraction is a key step during this process, and much research has been devoted to finding the best solvent mixture to extract as much metabolites as possible.Here a procedure is described for analysis of both polar and apolar metabolites using a two-phase extraction system. D 2 O and CDCl 3 are the solvents of choice, and their major advantage is that, for the identification of the compounds, standard databases can be used because D 2 O and CDCl 3 are the solvents most commonly used for pure compound NMR spectra. The procedure enables the absolute quantification of components via the addition of suitable internal standards. The extracts are also suitable for further analysis with other systems like LC-MS or GC-MS.

  20. Novel Displacement Agents for Aqueous 2-Phase Extraction Can Be Estimated Based on Hybrid Shortcut Calculations.

    Science.gov (United States)

    Kress, Christian; Sadowski, Gabriele; Brandenbusch, Christoph

    2016-10-01

    The purification of therapeutic proteins is a challenging task with immediate need for optimization. Besides other techniques, aqueous 2-phase extraction (ATPE) of proteins has been shown to be a promising alternative to cost-intensive state-of-the-art chromatographic protein purification. Most likely, to enable a selective extraction, protein partitioning has to be influenced using a displacement agent to isolate the target protein from the impurities. In this work, a new displacement agent (lithium bromide [LiBr]) allowing for the selective separation of the target protein IgG from human serum albumin (represents the impurity) within a citrate-polyethylene glycol (PEG) ATPS is presented. In order to characterize the displacement suitability of LiBr on IgG, the mutual influence of LiBr and the phase formers on the aqueous 2-phase system (ATPS) and partitioning is investigated. Using osmotic virial coefficients (B22 and B23) accessible by composition gradient multiangle light-scattering measurements, the precipitating effect of LiBr on both proteins and an estimation of both protein partition coefficients is estimated. The stabilizing effect of LiBr on both proteins was estimated based on B22 and experimentally validated within the citrate-PEG ATPS. Our approach contributes to an efficient implementation of ATPE within the downstream processing development of therapeutic proteins. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

  1. An Experimental Design Approach for the Analysis of Liquid Phase Products in Water for Hydrogenolysis of Glycerol using Immersed Solid-Phase Micro extraction

    International Nuclear Information System (INIS)

    Noraini Hamzah; Rozita Osman; Noraini Hamzah; Mohd Ambar Yarmo

    2013-01-01

    In this study, a response surface methodology (RSM) was applied to optimize the immersed-solid-phase micro extraction (immersed-SPME) conditions for the first time using a polyacrylate (PA) coated fiber. This was to determine liquid phase compounds in water for hydrogenolysis reaction of glycerol. There are a three-factor response surface experimental design was used to evaluate the interactive effects of extraction temperature (30-70 degree Celsius), extraction time (10-30 minutes) and desorption time (2-18 minutes) on the analysis of liquid phase compounds in water for hydrogenolysis of glycerol using immersed-solid-phase micro extraction (immersed-SPME). The extraction conditions using immersed-SPME were optimized in order to achieve high enrichment of the analytes from aqueous samples. The isolated compounds from the SPME fiber were desorbed and separated on a capillary polar column of a gas chromatography-flame ionization detector (GC-FID). The extraction time and desorption time were found significant in increasing the amount of glycerol in aqueous hydrogenolysis of glycerol. Nevertheless, the effect of extraction temperature was not significant. In terms of interactions between the effects, the relation between extraction temperature and extraction time was the most significant. The optimised immersed-SPME conditions were at extraction temperature of 27 degree Celsius, extraction time of 30 minutes and 15 minutes of desorption time. Thus, the application of SPME was found to be a rapid and effective technique in the determination of glycerol and propylene glycol compounds in aqueous hydrogenolysis glycerol. (author)

  2. Solid phase extraction of polychlorinated biphenyls from water containing humic substances

    Energy Technology Data Exchange (ETDEWEB)

    Bonifazi, P.; Pierini, E.; Bruner, F. [Centro di Studio per la Chimica dell`Ambiente e le Tecnologie Strumentali Avanzate dell` Universita degli Studi di Urbino, Ist. di Scienze Chimiche (Italy)

    1997-06-01

    A study was carried out of the recovery by solid phase extraction of the eleven most toxic polychlorinated biphenyls from water containing humic acids. Experiments were performed using water polluted with a humic acid (sodium salt) concentration of 9-18 mg L{sup -1}. The effect of humic acids on the recoveries was noticeable, especially where the more chlorinated congeners were concerned. The effect was also evident with river water containing naturally dissolved humic acids. A method for destroying humic acids prior to extraction was applied. The recoveries after the destruction of humic acids were in the range of 90%, even in the case of river water, demonstrating the applicability of the method to real samples. (orig.)

  3. Linear feature extraction from radar imagery: SBIR (Small Business Innovative Research) phase 2, option 1

    Science.gov (United States)

    Conner, Gary D.; Milgram, David L.; Lawton, Daryl T.; McConnell, Christopher C.

    1988-04-01

    The goal of this effort is to develop and demonstrate prototype processing capabilities for a knowledge-based system to automatically extract and analyze linear features from synthetic aperture radar (SAR) imagery. This effort constitutes Phase 2 funding through the Defense Small Business Innovative Research (SBIR) Program. Previous work examined the feasibility of the technology issues involved in the development of an automatedlinear feature extraction system. This Option 1 Final Report documents this examination and the technologies involved in automating this image understanding task. In particular, it reports on a major software delivery containing an image processing algorithmic base, a perceptual structures manipulation package, a preliminary hypothesis management framework and an enhanced user interface.

  4. Phytotoxicity of the organic phase and major compound obtained from the fruit pulp of Crescentia cujete L. (Bignoniaceae

    Directory of Open Access Journals (Sweden)

    Sinval Garcia Pereira

    2015-09-01

    Full Text Available http://dx.doi.org/10.5007/2175-7925.2015v28n4p51 The phytotoxity of ethanol extracts, of the organic phase and major compound (cinnamic acid obtained from the fruit pulp of Crescentia cujete L., were evaluated for their potential to inhibit seed germination, hypocotyl development and radicle development of the invasive weeds Senna obtusifolia (L. Irwin & Barneby and Mimosa pudica Mill. The organic phase at a concentration of 0.5% inhibited 100% seed germination of both weeds. Cinnamic acid obtained from the organic phase inhibited seed germination by 95% for S. obtusifolia and 99% for M. pudica at a concentration of 0.1%, with concentrations (% inhibiting 50% (IC50 seed germination equal to 0.063% and 0.037%, respectively. For the seedling growth bioassays, the toxicity of the cinnamic acid was more efficient for the S. obtusifolia radicle (IC50 equal to 0.009%, and for M. pudica the IC50 values were 0.097% and 0.117% for the radicle and hypocotyl, respectively. This research reinforces the phytotoxic potential of cinnamic acid, verified initially in the organic phase (in ethyl acetate, which is rich in this phenylpropanoid. he rainiest months in the Amazon region. The increased BAP and GA3 concentrations in the culture medium provided significant improvements in the material multiplication rates. In spite of the results obtained, the species shows peculiarities and limitations to in vitro cultivation that were identified and described in this paper.

  5. Phytotoxicity of the organic phase and major compound obtained from the fruit pulp of Crescentia cujete L. (Bignoniaceae

    Directory of Open Access Journals (Sweden)

    Sinval Garcia Pereira

    2015-12-01

    Full Text Available The phytotoxity of ethanol extracts, of the organic phase and major compound (cinnamic acid obtained from the fruit pulp of Crescentia cujete L., were evaluated for their potential to inhibit seed germination, hypocotyl development and radicle development of the invasive weeds Senna obtusifolia (L. Irwin & Barneby and Mimosa pudica Mill. The organic phase at a concentration of 0.5% inhibited 100% seed germination of both weeds. Cinnamic acid obtained from the organic phase inhibited seed germination by 95% for S. obtusifolia and 99% for M. pudica at a concentration of 0.1%, with concentrations (% inhibiting 50% (IC50 seed germination equal to 0.063% and 0.037%, respectively. For the seedling growth bioassays, the toxicity of the cinnamic acid was more efficient for the S. obtusifolia radicle (IC50 equal to 0.009%, and for M. pudica the IC50 values were 0.097% and 0.117% for the radicle and hypocotyl, respectively. This research reinforces the phytotoxic potential of cinnamic acid, verified initially in the organic phase (in ethyl acetate, which is rich in this phenylpropanoid.

  6. Design Implementation and Testing of a VLSI High Performance ASIC for Extracting the Phase of a Complex Signal

    National Research Council Canada - National Science Library

    Altmeyer, Ronald

    2002-01-01

    This thesis documents the research, circuit design, and simulation testing of a VLSI ASIC which extracts phase angle information from a complex sampled signal using the arctangent relationship: (phi=tan/-1 (Q/1...

  7. Assessment of solid phase microfiber extraction fibers for the monitoring of volatile organoarsinicals emitted from a plant-soil system.

    Science.gov (United States)

    Ruppert, L; Lin, Z-Q; Dixon, R P; Johnson, K A

    2013-11-15

    Phytoremediation, the use of plants and microbes to clean up inorganic and organic pollutants, has shown great promise as an inexpensive and feasible form of remediation. More recently, studies have shown that some plants have an amazing capacity to volatilize contaminants and can be an effective remediation strategy if the chemicals released are non-toxic. Arsenic contamination and remediation has drawn great attention in the scientific community. However, its toxicity also varies depending on its form. We evaluated, optimized, and then utilized a solid phase microfiber extraction (SPME) head space sampling technique to characterize the organoarsinical emissions from rabbitfoot grass (Polypogon monspeliensis) in arsenic treated soils to determine if the potentially more toxic organic forms of arsenic (AsH3, AsH2CH3, AsH(CH3)2, and As(CH3)3) were being emitted from the plant-soil system. The SPME fiber that proved best fitted for this application was the DVB/CAR/PDMS fiber with a 45 min sampling period. We did detect and confirm the emissions of dimethylchloroarsine (AsCl(CH3)2) and pentamethylarsine (As(CH3)5). However, it was determined that the more toxic organic forms of arsenic were not released during phytovolatilization. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. Novel nanoporous sorbent for solid-phase extraction in petroleum fingerprinting

    Science.gov (United States)

    Alayande, S. Oluwagbemiga; Hlengilizwe, Nyoni; Dare, E. Olugbenga; Msagati, Titus A. M.; Akinlabi, A. Kehinde; Aiyedun, P. O.

    2016-04-01

    Sample preparation is crucial in the analysis of petroleum and its derivatives. In this study, developing affordable sorbent for petroleum fingerprinting analysis using polymer waste such expanded polystyrene was explored. The potential of electrospun expanded polystyrene (EPS) as a sorbent for the solid-phase extraction (SPE) technique was investigated, and its efficiency was compared with commercial cartridges such as alumina, silica and alumina/silica hybrid commercial for petroleum fingerprinting analysis. The chromatograms showed that the packed electrospun EPS fibre demonstrated excellent properties for SPE applications relative to the hybrid cartridges.

  9. VOLATILE COMPOUNDS OF LITHRAEA CAUSTICA (LITRE) DETERMINATED BY SOLID PHASE MICRO-EXTRACTION (SPME)

    OpenAIRE

    GARBARINO, JUAN A; SALVATORE, GIUSEPPE; PIVANOVO, MARISA; CHAMY, MARÍA CRISTINA; NICOLETTI, MARCELLO; DE IOANNES, ALFREDO

    2002-01-01

    The head space of the aerial parts of Lithraea caustica was analyzed by Solid Phase Micro-Extraction (SPME) technique, obtaining as main volatile compounds the monoterpenes, myrcene, a -pinene, , p-cymene and limonene, as well as the sesquiterpene caryophylene. De las partes áereas de Lithraea caustica y usando la técnica de Micro-Extracción en Fase Sólida (MEFS), fueron identificados y cuantificados los principales compuestos volátiles: los monoterpenos, mirceno, a -pineno, p-cimeno y lim...

  10. Automated solid-phase extraction of herbicides from water for gas chromatographic-mass spectrometric analysis

    Science.gov (United States)

    Meyer, M.T.; Mills, M.S.; Thurman, E.M.

    1993-01-01

    An automated solid-phase extraction (SPE) method was developed for the pre-concentration of chloroacetanilide and triazine herbicides, and two triazine metabolites from 100-ml water samples. Breakthrough experiments for the C18 SPE cartridge show that the two triazine metabolites are not fully retained and that increasing flow-rate decreases their retention. Standard curve r2 values of 0.998-1.000 for each compound were consistently obtained and a quantitation level of 0.05 ??g/l was achieved for each compound tested. More than 10,000 surface and ground water samples have been analyzed by this method.

  11. Development of magnetic micro-solid phase extraction for analysis of phthalate esters in packaged food.

    Science.gov (United States)

    Makkliang, Fonthip; Kanatharana, Proespichaya; Thavarungkul, Panote; Thammakhet, Chongdee

    2015-01-01

    A novel, simple and low cost magnetic multi-walled carbon nanotubes-poly (vinyl alcohol) cryogel-micro-solid phase extraction (magnetic-MWCNTs-PVA cryogel-μ-SPE) sorbent was synthesized by incorporating magnetic particles and MWCNTs into a PVA cryogel. The magnetic-MWCNTs-PVA cryogel-μ-SPE sorbent developed, with a large surface area and macro-porous structure, provided good sorbent-to-sorbent reproducibility (%RSDclear chicken soup samples in the range 0.02-0.07 μg mL(-1). Copyright © 2014 Elsevier Ltd. All rights reserved.

  12. Purification of nattokinase by reverse micelles extraction from fermentation broth: effect of temperature and phase volume ratio.

    Science.gov (United States)

    Liu, Jun-Guo; Xing, Jian-Min; Chang, Tian-Shi; Liu, Hui-Zhou

    2006-03-01

    Nattokinase is a novel fibrinolytic enzyme that is considered to be a promising agent for thrombosis therapy. In this study, reverse micelles extraction was applied to purify and concentrate nattokinase from fermentation broth. The effects of temperature and phase volume ratio used for the forward and backward extraction on the extraction process were examined. The optimal temperature for forward and backward extraction were 25 degrees C and 35 degrees C respectively. Nattokinase became more thermosensitive during reverse micelles extraction. And it could be enriched in the stripping phase eight times during backward extraction. It was found that nattokinase could be purified by AOT reverse micelles with up to 80% activity recovery and with a purification factor of 3.9.

  13. Effect of organic amendments and compost extracts on tomato production and storability in ecological production systems

    Directory of Open Access Journals (Sweden)

    ghorbani reza

    2009-06-01

    Full Text Available A field experiment was conducted in Shiravan, Iran, during 2005 in order to investigate the effects of organic amendments, synthetic fertilizers and compost extracts on crop health, productivity and storability of commonly used tomato (Lycopersicon esculentum Mill.. Treatments included different fertilizers of cattle, sheep and poultry manures, house-hold compost and chemical fertilizers, and five aqueous extracts from cattle manure, poultry manures, green-waste and house-hold composts and water as control. The effect of fertilizer type on tomato yield and marketable yield was significant (P

  14. Extraction of polycyclic aromatic hydrocarbons from polluted soils with binary and ternary supercritical phases

    International Nuclear Information System (INIS)

    Hollender, J.; Shneine, J.; Dott, W.; Heinzel, M.; Hagemann, H.W.; Gotz, G.K.E.

    1997-01-01

    The paper describes how supercritical fluid extractions (SFE) using carbon dioxide and modifiers (n-hexane, cyclohexane, toluene, methyl tert-butyl ether, methoxybenzene, dichloromethane, propanone, pyridine, methanol) as well as modifier mixtures (methanol-containing diethylamide, 2-aminoethan-1-ol, acetic acid) were performed to extract polycyclic aromatic hydrocarbons (PAHs) from real environmental samples polluted to a minor extent by mineral oil products and highly contaminated by brown coal tar. Comparing the results with those from Soxhlet extraction utilizing dichloromethane and SFE using pure carbon dioxide show that acidic or basic co-solvents give the highest PAH yields. Extraction efficiency decreases with reduced polarity of the modifier used and increases at higher concentrations of co-solvent. To explain the SFE results, several mechanisms of disruption of matrix-PAH interactions are considered: the competition between the modifier molecules and the active sites of soil's organic and inorganic matter to interact with non-covalent bondings to the analytes; and the splitting of electron donor-acceptor complexes between humic substances and PAHs induced by Lewis acids or Lewis bases

  15. 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

  16. Solid-phase extraction and high-performance liquid chromatographic separation of pigments of red wines.

    Science.gov (United States)

    Csiktusnádi Kiss, G A; Forgács, E; Cserháti, T; Candeias, M; Vilas-Boas, L; Bronze, R; Spranger, I

    2000-08-11

    The adsorption and desorption capacities of 11 different solid-phase extraction sorbents were tested for the preconcenration of pigments of various Hungarian red wines. The concentrates were evaluated by multiwavelengh spectrophotometry combined with a spectral mapping technique (SPM) and by reversed-phase high-performance liquid chromatography. The highest (10-fold) concentration of pigments was achieved on octadecylsilica sorbent. It can be used five times without losing adsorption and desorption characteristics. SPM indicated that multiwavelength spectrophotometry can be employed for the differentiation of red wines. Comparison of the chromatograms of pigments with and without preconcentration showed that preconcentration makes possible the separation and detection of pigments present in low concentration in red wines.

  17. Application of mercapto-silica polymerized high internal phase emulsions for the solid-phase extraction and preconcentration of trace lead(II).

    Science.gov (United States)

    Su, Rihui; Ruan, Guihua; Chen, Zhengyi; Du, Fuyou; Li, Jianping

    2015-12-01

    A new class of solid-phase extraction column prepared with grafted mercapto-silica polymerized high internal phase emulsion particles was used for the preconcentration of trace lead. First, mercapto-silica polymerized high internal phase emulsion particles were synthesized by using high internal phase emulsion polymerization and carefully assembled in a polyethylene syringe column. The influences of various parameters including adsorption pH value, adsorption and desorption solvents, flow rate of the adsorption and desorption procedure were optimized, respectively, and the suitable uploading sample volumes, adsorption capacity, and reusability of solid phase extraction column were also investigated. Under the optimum conditions, Pb(2+) could be preconcentrated quantitatively over a wide pH range (2.0-5.0). In the presence of foreign ions, such as Na(+) , K(+) , Ca(2+) , Zn(2+) , Mg(2+) , Cu(2+) , Fe(2+) , Cd(2+) , Cl(-) and NO3 (-) , Pb(2+) could be recovered successfully. The prepared solid-phase extraction column performed with high stability and desirable durability, which allowed more than 100 replicate extractions without measurable changes of performance. The feasibility of the developed method was further validated by the extraction of Pb(2+) in rice samples. At three spiked levels of 40.0, 200 and 800 μg/kg, the average recoveries for Pb(2+) in rice samples ranged from 87.3 to 105.2%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Desorption atmospheric pressure photoionization with polydimethylsiloxane as extraction phase and sample plate material

    Energy Technology Data Exchange (ETDEWEB)

    Vaikkinen, A. [Division of Pharmaceutical Chemistry, Faculty of Pharmacy, P.O. Box 56, FIN-00014 University of Helsinki (Finland); Kotiaho, T. [Division of Pharmaceutical Chemistry, Faculty of Pharmacy, P.O. Box 56, FIN-00014 University of Helsinki (Finland); Laboratory of Analytical Chemistry, Department of Chemistry, P.O. Box 55, FIN-00014 University of Helsinki (Finland); Kostiainen, R. [Division of Pharmaceutical Chemistry, Faculty of Pharmacy, P.O. Box 56, FIN-00014 University of Helsinki (Finland); Kauppila, T.J., E-mail: tiina.kauppila@helsinki.fi [Division of Pharmaceutical Chemistry, Faculty of Pharmacy, P.O. Box 56, FIN-00014 University of Helsinki (Finland)

    2010-12-03

    Desorption atmospheric pressure photoionization (DAPPI) is an ambient ionization technique for mass spectrometry (MS) that can be used to ionize polar as well as neutral and completely non-polar analytes. In this study polydimethylsiloxane (PDMS) was used as a solid phase extraction sorbent for DAPPI-MS analysis. Pieces of PDMS polymer were soaked in an aqueous sample, where the analytes were sorbed from the sample solution to PDMS. After this, the extracted analytes were desorbed directly from the polymer by the hot DAPPI spray solvent plume, without an elution step. Swelling and extracting the PDMS with a cleaning solvent prior to extraction diminished the high background in the DAPPI mass spectrum caused by PDMS oligomers. Acetone, hexane, pentane, toluene, diisopropylamine and triethylamine were tested for this purpose. The amines were most efficient in reducing the PDMS background, but they also suppressed the signals of low proton affinity analytes. Toluene was chosen as the optimum cleaning solvent, since it reduced the PDMS background efficiently and gave intensive signals of most of the studied analytes. The effects of DAPPI spray solvents toluene, acetone and anisole on the PDMS background and the ionization of analytes were also compared and extraction conditions were optimized. Anisole gave a low background for native PDMS, but toluene ionized the widest range of analytes. Analysis of verapamil, testosterone and anthracene from purified, spiked wastewater was performed to demonstrate that the method is suited for in-situ analysis of water streams. In addition, urine spiked with several analytes was analyzed by the PDMS method and compared to the conventional DAPPI procedure, where sample droplets are applied on PMMA surface. With the PDMS method the background ion signals caused by the urine matrix were lower, the S/N ratios of analytes were 2-10 times higher, and testosterone, anthracene and benzo[a]pyrene that were not detected from PMMA in urine

  19. Desorption atmospheric pressure photoionization with polydimethylsiloxane as extraction phase and sample plate material

    International Nuclear Information System (INIS)

    Vaikkinen, A.; Kotiaho, T.; Kostiainen, R.; Kauppila, T.J.

    2010-01-01

    Desorption atmospheric pressure photoionization (DAPPI) is an ambient ionization technique for mass spectrometry (MS) that can be used to ionize polar as well as neutral and completely non-polar analytes. In this study polydimethylsiloxane (PDMS) was used as a solid phase extraction sorbent for DAPPI-MS analysis. Pieces of PDMS polymer were soaked in an aqueous sample, where the analytes were sorbed from the sample solution to PDMS. After this, the extracted analytes were desorbed directly from the polymer by the hot DAPPI spray solvent plume, without an elution step. Swelling and extracting the PDMS with a cleaning solvent prior to extraction diminished the high background in the DAPPI mass spectrum caused by PDMS oligomers. Acetone, hexane, pentane, toluene, diisopropylamine and triethylamine were tested for this purpose. The amines were most efficient in reducing the PDMS background, but they also suppressed the signals of low proton affinity analytes. Toluene was chosen as the optimum cleaning solvent, since it reduced the PDMS background efficiently and gave intensive signals of most of the studied analytes. The effects of DAPPI spray solvents toluene, acetone and anisole on the PDMS background and the ionization of analytes were also compared and extraction conditions were optimized. Anisole gave a low background for native PDMS, but toluene ionized the widest range of analytes. Analysis of verapamil, testosterone and anthracene from purified, spiked wastewater was performed to demonstrate that the method is suited for in-situ analysis of water streams. In addition, urine spiked with several analytes was analyzed by the PDMS method and compared to the conventional DAPPI procedure, where sample droplets are applied on PMMA surface. With the PDMS method the background ion signals caused by the urine matrix were lower, the S/N ratios of analytes were 2-10 times higher, and testosterone, anthracene and benzo[a]pyrene that were not detected from PMMA in urine

  20. Simultaneous Extraction, Enrichment and Removal of Dyes from Aqueous Solutions Using a Magnetic Aqueous Micellar Two-Phase System

    Directory of Open Access Journals (Sweden)

    Shuanggen Wu

    2017-12-01

    Full Text Available The magnetic aqueous micellar two-phase system (MAMTPS has the advantages combined of magnetic solid phase extraction (MSPE and aqueous micellar two-phase system (AMTPS. Thus, MAMTPS based on Fe3O4 magnetic nanoparticles (MNPs and a nonionic surfactant Triton X-114 (TX-114 was developed for the extraction, enrichment and removal of three dyes (Congo red, methyl blue, and methyl violet from aqueous solutions in this study. The MNPs Fe3O4@NH2 was screened as the optimal MNPs benefiting the extraction. Then, the influencing factors of MNPs amount, TX-114 concentration, vibration time, and extraction temperature were investigated in detail. The results showed that the extraction efficiencies of three dyes almost reached 100% using MAMTPS under the optimal conditions; MAMTPS had higher extraction ability than the individual MSPE or AMTPS. Thus, MAMTPS had the advantages of simple operation, high extraction ability, easy recycling of MNPs, and short phase-separation time, which showspotential for use in the extraction and analysis of contaminants from water samples.

  1. Investigation of water-soluble organic matter extracted from shales during leaching experiments

    Science.gov (United States)

    Zhu, Yaling; Vieth-Hillebrand, Andrea; Wilke, Franziska D. H.; Horsfield, Brian

    2017-04-01

    The huge volumes and unknown composition of flowback and produced waters cause major public concerns about the environmental and social compatibility of hydraulic fracturing and the exploitation of gas from unconventional reservoirs. Flowback and produced waters contain not only residues of fracking additives but also chemical species that are dissolved from the shales themselves during fluid-rock interaction. Knowledge of the composition, size and structure of dissolved organic carbon (DOC) as well as the main controls on the release of DOC are a prerequisite for a better understanding of these interactions and its effects on composition of flowback and produced water. Black shales from four different geological settings and covering a maturity range Ro = 0.3-2.6% were extracted with deionized water. The DOC yields were found to decrease rapidly with increasing diagenesis and remain low throughout catagenesis. Four DOC fractions have been qualitatively and quantitatively characterized using size-exclusion chromatography. The concentrations of individual low molecular weight organic acids (LMWOA) decrease with increasing maturity of the samples except for acetate extracted from the overmature Posidonia shale, which was influenced by hydrothermal brines. The oxygen content of the shale organic matter also shows a significant influence on the release of organic acids, which is indicated by the positive trend between oxygen index (OI) and the concentrations of formate and acetate. Based on our experiments, both the properties of the organic matter source and the thermal maturation progress of the shale organic matter significantly influence the amount and quality of extracted organic compounds during the leaching experiments.

  2. Selective extraction of phospholipids from dairy products by micro-solid phase extraction based on titanium dioxide microcolumns followed by MALDI-TOF-MS analysis

    DEFF Research Database (Denmark)

    Calvano, Cosima; Jensen, Ole; Zambonin, Carlo

    2009-01-01

    A new micro-solid phase extraction (micro-SPE) procedure based on titanium dioxide microcolumns was developed for the selective extraction of phospholipids (PLs) from dairy products before matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) analysis. All...... the extraction steps (loading, washing, and elution) have been optimized using a synthetic mixture of PLs standard and the procedure was subsequently applied to food samples such as milk, chocolate milk and butter. The whole method demonstrated to be simpler than traditional approaches and it appears very...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-04-10

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

  4. Resolution dependence on phase extraction by the Hilbert transform in phase calibrated and dispersion compensated ultrahigh resolution spectrometer-based OCT

    DEFF Research Database (Denmark)

    Israelsen, Niels Møller; Maria, Michael; Feuchter, Thomas

    2018-01-01

    -linearities lead together to an unknown chirp of the detected interferogram. One method to compensate for the chirp is to perform a pixel-wavenumber calibration versus phase that requires numerical extraction of the phase. Typically a Hilbert transform algorithm is employed to extract the optical phase versus...... wavenumber for calibration and dispersion compensation. In this work we demonstrate UHR-OCT at 1300 nm using a Super continuum source and highlight the resolution constraints in using the Hilbert transform algorithm when extracting the optical phase for calibration and dispersion compensation. We demonstrate...... that the constraints cannot be explained purely by the numerical errors in the data processing module utilizing the Hilbert transform but must be dictated by broadening mechanisms originating from the experimentally obtained interferograms....

  5. Antinociceptive activities of crude methanolic extract and phases, n-butanolic, chloroformic and ethyl acetate from Caulerpa racemosa (Caulerpaceae

    Directory of Open Access Journals (Sweden)

    Everton T. Souza

    Full Text Available In this study, we attempted to identify the possible antinociceptive actions of n-butanolic phase, chloroformic phase, ethyl acetate phase and crude methanolic extract obtained from Caulerpa racemosa. This seaweed is cosmopolitan in world, mainly in tropical regions. The n-butanolic, chloroformic, ethyl acetate phases and crude methanolic extract, all administered orally in the concentration of 100 mg/kg, reduced the nociception produced by acetic acid by 47.39%, 70.51%, 76.11% and 72.24%, respectively. In the hotplate test the chloroformic and ethyl acetate phase were activite in this models. In the neurogenic phase on formalin test, were observed that crude methanolic extract (51.77%, n-butanolic phase (35.12%, chloroformic phase (32.70% and indomethacin (32.06% were effective in inhibit the nociceptive response. In the inflammatory phase, only the ethyl acetate phase (75.43% and indomethacin (47.83% inhibited significantly the nociceptive response. Based on these data, we can infer that the ethyl acetate phase shows a significant anti-inflammatory profile, whose power has not yet been determined. However, pharmacological and chemical studies are continuing in order to characterize the mechanism(s responsible for the antinociceptive action and also to identify other active principles present in Caulerpa racemosa.

  6. Larvicidal efficacy of Scabiosa arenaria Forssk. (Dipsacaceae organs extracts against Culex pipiens L.

    Directory of Open Access Journals (Sweden)

    Malek Besbes Hlila

    2017-11-01

    Full Text Available Objective: To determine the larvicidal activity of sixteen extracts of Scabiosa arenaria Forssk. (S. arenaria against the third instar larvae of Culex pipiens L. (C. pipiens. Methods: Larvicidal activity of S. arenaria extracts was determined according to World Health Organization. Twenty third instars of the C. pipiens were exposed to different concentrations (15 µg/mL to 60 µg/mL of extracts. Mortality was recorded after 24 h of exposure. Results: The roots ethyl acetate fraction of S. arenaria had a significant toxic effect on larvae of C. pipiens, with high mortality percentage (100.0% ± 2.2% at 60 µg/mL, and 50% lethal concentration value of LC50 = (15.00 ± 0.09 µg/mL. Conclusions: Results show that roots ethyl acetate could be used for the production of natural bio-pesticides which could decrease our dependence on chemical pesticides.

  7. Extraction of organic materials from red water by metal-impregnated lignite activated carbon

    Energy Technology Data Exchange (ETDEWEB)

    Wei, Fangfang [State Key Laboratory of Geological Processes and Mineral Resources, National Laboratory of Mineral Materials, School of Materials Science and Technology, China University of Geosciences, Beijing 100083 (China); Zhang, Yihe, E-mail: zyh@cugb.edu.cn [State Key Laboratory of Geological Processes and Mineral Resources, National Laboratory of Mineral Materials, School of Materials Science and Technology, China University of Geosciences, Beijing 100083 (China); Department of Physics and Materials Science, City University of Hong Kong, Tat Chee Avenue, Kowloon, Hong Kong (China); Lv, Fengzhu [State Key Laboratory of Geological Processes and Mineral Resources, National Laboratory of Mineral Materials, School of Materials Science and Technology, China University of Geosciences, Beijing 100083 (China); Chu, Paul K. [Department of Physics and Materials Science, City University of Hong Kong, Tat Chee Avenue, Kowloon, Hong Kong (China); Ye, Zhengfang, E-mail: zhengfangye@163.com [Department of Environmental Engineering, Key Laboratory of Water and Sediment Sciences of the Ministry of Education, Peking University, Beijing 100871 (China)

    2011-12-15

    Highlights: Black-Right-Pointing-Pointer Metal-impregnated lignite activated carbon was investigated as adsorbent. Black-Right-Pointing-Pointer Adsorbent for the extraction of organic materials from 2,4,6-trinitrotoluene (TNT) red water. Black-Right-Pointing-Pointer Effects of different metals on the extraction were investigated and discussed. Black-Right-Pointing-Pointer Many loading factors of Cu{sup 2+} were found having great influences on the extraction. Black-Right-Pointing-Pointer Extraction performances and mechanism of TNT red water on Cu/LAC were investigated. - Abstract: Extraction of organic materials from 2,4,6-trinitrotoluene (TNT) red water by lignite activated carbon (LAC) impregnated with Cu{sup 2+}, Ba{sup 2+}, Sn{sup 2+}, Fe{sup 3+}, Ca{sup 2+} and Ag{sup +} was investigated. The affinity to organic materials in red water was found to follow the order: Cu/LAC > Sn/LAC > Ag/LAC > Ba/LAC > Fe/LAC > Ca/LAC, which was explained by the hard and soft acid base (HSAB) theory. Cu{sup 2+} showed the best performance and several parameters were further studied. X-ray photoelectron spectroscopy (XPS) verified effective loading of Cu{sup 2+} on the LAC surface. The water quality before and after treated by Cu/LAC was evaluated using high performance liquid chromatograph, Gas Chromatography/Mass Spectroscopy (GC/MS), UV-vis spectroscopy and other analyses. The extraction performances and mechanism of organic materials on Cu/LAC were investigated through static methods. The experimental results showed that Cu/LAC possessed stronger extraction ability for the sulfonated nitrotoluenes than the non-sulfonated nitrotoluenes, the kinetic data fitted the pseudo-second-order kinetic model well. In addition, the leaching out of Cu{sup 2+} from Cu/LAC was found much lower in the 100 times diluted red water (0.074%) than in the raw water (10.201%). Column adsorptions with more concentrated red water were also studied. Finally, Cu/LAC was observed to possess excellent

  8. 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....

  9. Immobilized humic substances and immobilized aggregates of humic substances as sorbent for solid phase extraction.

    Science.gov (United States)

    Erny, Guillaume L; Gonçalves, Bruna M; Esteves, Valdemar I

    2013-09-06

    In this work, humic substances (HS) immobilized, as a thin layer or as aggregates, on silica gel were tested as material for solid phase extraction. Some triazines (simazine, atrazine, therbutylazine, atrazine-desethyl-desisopropyl-2-hydroxy, ametryn and terbutryn), have been selected as test analytes due to their environmental importance and to span a large range of solubility and octanol/water partition coefficient (logP). The sorbent was obtained immobilizing a thin layer of HS via physisorption on a pre-coated silica gel with a cationic polymer (polybrene). While the sorbent could be used as it is, it was demonstrated that additional HS could be immobilized, via weak interactions, to form stable humic aggregates. However, while a higher quantity of HS could be immobilized, no significant differences were observed in the sorption parameters. This sorbent have been tested for solid phase extraction to concentrate triazines from aqueous matrixes. The sorbent demonstrated performances equivalent to commercial alternatives as a concentration factor between 50 and 200, depending on the type of triazines, was obtained. Moreover the low cost and the high flow rate of sample through the column allowed using high quantity of sorbent. The analytical procedure was tested with different matrixes including tap water, river water and estuarine water. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. Fabricating and Characterizing the Microfluidic Solid Phase Extraction Module Coupling with Integrated ESI Emitters

    Directory of Open Access Journals (Sweden)

    Hangbin Tang

    2018-05-01

    Full Text Available Microfluidic chips coupling with mass spectrometry (MS will be of great significance to the development of relevant instruments involving chemical and bio-chemical analysis, drug detection, food and environmental applications and so on. In our previous works, we proposed two types of microfluidic electrospray ionization (ESI chip coupling with MS: the two-phase flow focusing (FF ESI microfluidic chip and the corner-integrated ESI emitter, respectively. However the pretreatment module integrated with these ESI emitters is still a challenging problem. In this paper, we concentrated on integrating the solid phase micro-extraction (SPME module with our previous proposed on-chip ESI emitters; the fabrication processes of such SPME module are fully compatible with our previous proposed ESI emitters based on the multi-layer soft lithography. We optimized the structure of the integrated chip and characterized its performance using standard samples. Furthermore, we verified its abilities of salt removal, extraction of multiple analytes and separation through on-chip elution using mimic biological urine spiked with different drugs. The results indicated that our proposed integrated module with ESI emitters is practical and effective for real biological sample pretreatment and MS detection.

  11. Study on Solid Phase Extraction and Spectrophotometric Determination of Nickel in Waters and Biological Samples

    International Nuclear Information System (INIS)

    Hu, Qiufen; Yang, Guangyu; Huang, Zhangjie; Yin, Jiayuan

    2004-01-01

    A sensitive, selective and rapid method for the determination of nickel based on the rapid reaction of nickel(II) with QADMAA and the solid phase extraction of the Ni(II)-QADMAA chelate with C 18 membrane disks has been developed. In the presence of pH 6.0 buffer solution and sodium dodecyl sulfonate (SDS) medium, QADMAA reacts with nickel to form a violet complex of a molar ratio of 1 : 2 (nickel to QADMAA). This chelate was enriched by solid phase extraction with C 18 membrane disks. An enrichment factor of 50 was obtained by elution of the chelates form the disks with the minimal amount of isopentyl alcohol. The molar absorptivity of the chelate was 1.32 x 10 5 L mol -1 cm -1 at 590 nm in the measured solution. Beer's law was obeyed in the range of 0.01-0.6 μg/mL. This method was applied to the determination of nickel in water and biological samples with good results

  12. Aqueous two-phase extraction as a platform in the biomanufacturing industry: economical and environmental sustainability.

    Science.gov (United States)

    Rosa, P A J; Azevedo, A M; Sommerfeld, S; Bäcker, W; Aires-Barros, M R

    2011-01-01

    The biotech industry is, nowadays, facing unparalleled challenges due to the enhanced demand for biotechnology-based human therapeutic products, such as monoclonal antibodies (mAbs). This has led companies to improve substantially their upstream processes, with the yield of monoclonals increasing to titers never seen before. The downstream processes have, however, been overlooked, leading to a production bottleneck. Although chromatography remains the workhorse of most purification processes, several limitations, such as low capacity, scale-related packing problems, low chemical and proteolytic stability and resins' high cost, have arisen. Aqueous two-phase extraction (ATPE) has been successfully revisited as a valuable alternative for the capture of antibodies. One of the important remaining questions for this technology to be adopted by the biotech industries is, now, how it compares to the currently established platforms in terms of costs and environmental impact. In this report, the economical and environmental sustainability of the aqueous two-phase extraction process is evaluated and compared to the currently established protein A affinity chromatography. Accordingly, the ATPE process was shown to be considerably advantageous in terms of process economics, especially when processing high titer cell culture supernatants. This alternative process is able to purify continuously the same amount of mAbs reducing the annual operating costs from 14.4 to 8.5 million (US$/kg) when cell culture supernatants with mAb titers higher than 2.5 g/L are processed. Copyright © 2011 Elsevier Inc. All rights reserved.

  13. A nanoscale study of charge extraction in organic solar cells: the impact of interfacial molecular configurations.

    Science.gov (United States)

    Tang, Fu-Ching; Wu, Fu-Chiao; Yen, Chia-Te; Chang, Jay; Chou, Wei-Yang; Gilbert Chang, Shih-Hui; Cheng, Horng-Long

    2015-01-07

    In the optimization of organic solar cells (OSCs), a key problem lies in the maximization of charge carriers from the active layer to the electrodes. Hence, this study focused on the interfacial molecular configurations in efficient OSC charge extraction by theoretical investigations and experiments, including small molecule-based bilayer-heterojunction (sm-BLHJ) and polymer-based bulk-heterojunction (p-BHJ) OSCs. We first examined a well-defined sm-BLHJ model system of OSC composed of p-type pentacene, an n-type perylene derivative, and a nanogroove-structured poly(3,4-ethylenedioxythiophene) (NS-PEDOT) hole extraction layer. The OSC with NS-PEDOT shows a 230% increment in the short circuit current density compared with that of the conventional planar PEDOT layer. Our theoretical calculations indicated that small variations in the microscopic intermolecular interaction among these interfacial configurations could induce significant differences in charge extraction efficiency. Experimentally, different interfacial configurations were generated between the photo-active layer and the nanostructured charge extraction layer with periodic nanogroove structures. In addition to pentacene, poly(3-hexylthiophene), the most commonly used electron-donor material system in p-BHJ OSCs was also explored in terms of its possible use as a photo-active layer. Local conductive atomic force microscopy was used to measure the nanoscale charge extraction efficiency at different locations within the nanogroove, thus highlighting the importance of interfacial molecular configurations in efficient charge extraction. This study enriches understanding regarding the optimization of the photovoltaic properties of several types of OSCs by conducting appropriate interfacial engineering based on organic/polymer molecular orientations. The ultimate power conversion efficiency beyond at least 15% is highly expected when the best state-of-the-art p-BHJ OSCs are combined with present arguments.

  14. Application of solid phase micro extraction (SPME) in profiling hydrocarbons in oil spill cases

    International Nuclear Information System (INIS)

    Zuraidah Abdullah Munir; Norashikin Saim; Nurul Huda Mamat Ghani

    2008-01-01

    In environmental forensic, it is extremely important to have a fast and reliable method in identifying sources of spilled oil and petroleum products. In this study, solid phase micro extraction (SPME) method coupled to gas chromatography-mass spectrometry was developed for the analysis of hydrocarbons in diesel and petroleum contaminated soil samples. Optimization of SPME parameters such as extraction time, extraction temperature and desorption time, was performed using 100-μm poly dimethylsiloxane (PDMS) fiber. These parameters were studied at three levels by means of a central composite experimental design and the optimum experimental conditions were determined using response surface method. The developed SPME method was applied to determine the profiles of hydrocarbons in several oil contaminated soil sample. The SPME method was also used to study the effects of weathering on the profiles of hydrocarbons in unleaded gasoline, diesel and kerosene contaminated soil samples. After several days, significant losses of the lighter hydrocarbons were observed compared to the heavier ones. From these data, SPME method can be used to differentiate possible candidate sources in oil spill cases. (author)

  15. Analysis of trace dicyandiamide in stream water using solid phase extraction and liquid chromatography UV spectrometry.

    Science.gov (United States)

    Qiu, Huidong; Sun, Dongdi; Gunatilake, Sameera R; She, Jinyan; Mlsna, Todd E

    2015-09-01

    An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction. The extraction procedure (including loading, washing, and eluting) used a flow rate of 1.0mL/min, and dicyandiamide was eluted with 20mL of a methanol/acetonitrile mixture (V/V=2:3), followed by pre-concentration using nitrogen evaporation and analysis with high performance liquid chromatography-ultraviolet spectroscopy (HPLC-UV). Sample extraction was carried out using a Waters Sep-Pak AC-2 Cartridge (with activated carbon). Separation was achieved on a ZIC(®)-Hydrophilic Interaction Liquid Chromatography (ZIC-HILIC) (50mm×2.1mm, 3.5μm) chromatography column and quantification was accomplished based on UV absorbance. A reliable linear relationship was obtained for the calibration curve using standard solutions (R(2)>0.999). Recoveries for dicyandiamide ranged from 84.6% to 96.8%, and the relative standard deviations (RSDs, n=3) were below 6.1% with a detection limit of 5.0ng/mL for stream water samples. Copyright © 2015. Published by Elsevier B.V.

  16. Extraction and recovery of 2-butoxyethanol from aqueous phases containing high saline concentration

    Directory of Open Access Journals (Sweden)

    Katherine E. Manz

    2016-09-01

    Full Text Available Ethylene glycol monobutyl ether (EGBE, also known as 2-butoxyethanol (2-BE, has been identified as a contaminant in hydraulic fracturing fluids. In order to determine the presence of 2-BE in hydraulic fracturing chemical additives, a reliable method for recovering 2-BE from aqueous phases by liquid-liquid extraction combined with gas chromatography/mass spectrometry (GC/MS was established. The liquid-liquid extraction method was applied to samples matrices containing various amounts of salt. Using methylene chloride for liquid-liquid extraction in a sample to solvent ratio of 1:3, ≥99% 2-BE recovery may be achieved with less than 5% standard error. The limit of detection was determined to be 0.957 mg L−1 2-BE. Accuracy was determined to be 2.58% and precision was determined using the coefficient of variation, which was 3.5%. The method was used to recover 2-BE in a hydraulic fracturing chemical additive called Revert Flow and to quantify the weight percent of 2-BE in the chemical additive. Weight percent of two additional components of Revert Flow, D-limonene and 1-butoxy-2-propanol, were also determined. We also used the method to determine the abiotic of 2-BE in water, which was 5.55 days. The persistence of 2-BE in hydraulic fracturing fluid was also investigated and determined that 2-BE is more persistent in this environment.

  17. Improved solid-phase extraction method for systematic toxicological analysis in biological fluids.

    Science.gov (United States)

    Soriano, T; Jurado, C; Menéndez, M; Repetto, M

    2001-03-01

    A method for the simultaneous qualitative and quantitative determination of drugs of abuse (opiates, cocaine, or amphetamines) and prescribed drugs (tricyclic antidepressants, phenotiazines, benzodiazepines, etc.) in biological fluids--blood, urine, bile, and gastric contents--was developed. This procedure involves solid-phase extraction with Bond-Elut Certify columns followed by analysis by gas chromatography-nitrogen-phosphorus detection (GC-NPD) and confirmation by gas chromatography-mass spectrometry (GC-MS), after derivatization, when necessary. Pretreatment was performed on all samples: sonication for 15 min plus enzymatic hydrolysis with beta-glucuronidase in urine. With respect to the internal standards, nalorphine and trihexylamine were used for basic substances, allobarbital for acidic drugs, and prazepam for benzodiazepines. Acidic and basic compounds were extracted from different aliquots of samples at different pH levels: 6-6.5 for the acidic and neutral and 8-8.5 for the basic and the benzodiazepines. Several areas of experimental design were considered in the process of method optimization. These included internal standards, pH, sonication, flow rate and washing solvents. It was found that systematic analysis could be reliably performed using optimized extraction conditions. The recovery rates for the compounds tested were always higher than 61.02%.

  18. Ultra trace analysis of PAHs by designing simple injection of large amounts of analytes through the sample reconcentration on SPME fiber after magnetic solid phase extraction.

    Science.gov (United States)

    Khodaee, Nader; Mehdinia, Ali; Esfandiarnejad, Reyhaneh; Jabbari, Ali

    2016-01-15

    A simple solventless injection method was introduced based on the using of a solid-phase microextraction (SPME) fiber for injection of large amounts of the analytes extracted by the magnetic solid phase extraction (MSPE) procedure. The resulted extract from MSPE procedure was loaded on a G-coated SPME fiber, and then the fiber was injected into the gas chromatography (GC) injection port. This method combines the advantages of exhaustive extraction property of MSPE and the solvent-less injection of SPME to improve the sensitivity of the analysis. In addition, the analytes were re-concentrated prior to inject into the gas chromatography (GC) inlet because of the organic solvent removing from the remaining extract of MSPE technique. Injection of the large amounts of analytes was made possible by using the introduced procedure. Fourteen polycyclic aromatic hydrocarbons (PAHs) with different volatility were used as model compounds to investigate the method performance for volatile and semi-volatile compounds. The introduced method resulted in the higher enhancement factors (5097-59376), lower detection limits (0.29-3.3pgmL(-1)), and higher sensitivity for the semi-volatile compounds compared with the conventional direct injection method. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Simultaneous Enrichment of Polycyclic Aromatic Hydrocarbons and Cu(2+) in Water Using Tetraazacalix[2]arene[2]triazine as a Solid-Phase Extraction Selector.

    Science.gov (United States)

    Zhao, Wenjie; Yang, Liu; He, Lijun; Zhang, Shusheng

    2016-08-10

    On the basis of the definite retention mechanism proven by the stationary phase for high-performance liquid chromatography, tetraazacalix[2]arene[2]triazine featuring multiple recognition sites was assessed as a solid-phase extraction (SPE) selector. The applicability of its silica support was used for the extraction of trace amounts of polycyclic aromatic hydrocarbons (PAHs) and Cu(2+) in aqueous samples, followed by high-performance liquid chromatography fluorometric and graphite furnace atomic absorption spectrometric determination. On the basis of the π-π interaction with PAHs and the chelating interaction with Cu(2+), the simultaneous extraction of PAHs and Cu(2+) and stepwise elution through tuning the eluent were successfully achieved, respectively. The SPE conditions affecting the extraction efficiency were optimized, including type and concentration of organic modifier, sample solution pH, flow rate, and volume. As a result of the special adsorption and desorption mechanism, high extraction efficiency was achieved with relative recoveries of 94.3-102.4% and relative standard deviations of less than 10.5%. The limits of detection were obtained with 0.4-3.1 ng L(-1) for PAHs and 15 ng L(-1) for Cu(2+), respectively. The method was applied to the analyses of PAHs and Cu(2+) in Xiliu Lake water samples collected in Zhengzhou, China.

  20. Coacervative extraction as a green technique for sample preparation for the analysis of organic compounds.

    Science.gov (United States)

    Melnyk, A; Wolska, L; Namieśnik, J

    2014-04-25

    One of the present trends in analytical chemistry is miniaturization, which is one of the methods of green analytical chemistry application. A particular emphasis is placed on the elimination of the use of large amounts of organic solvents which are toxic and harmful to the environment, maintaining high efficiency of the extraction process, high recovery values and low values of quantification (LOQ) and detection (LOD) limits. These requirements are fulfilled by coacervative extraction (CAE) technique. In this review, theoretical aspects of the coacervation process are presented along with environmental and bioanalytical applications of this technique, its advantages, limitations and competitiveness with other techniques. Due to its simplicity and rapidity, CAE is an excellent alternative for currently practiced procedures of sample preparation for the analysis of organic compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Separation of lanthanum (3) and neodymium (3) by tributyl phosphate extraction in the presence of solid phase

    International Nuclear Information System (INIS)

    Korotkevich, I.B.; Kolesnikov, A.A.; Bomshtejn, V.E.; Shikhaleeva, N.N.

    1987-01-01

    Lanthanum (3) and neodymium (3) extraction from nitric acid solutions by tributyl phosphate in the presence of solid phase of the element nitrates is investigated. An increase in distribution of neodymium nitrate in the presence of solid phase with the decrease in its concentration in the initial solution and with the increase in lanthanum nitrate concentration is detected. The highest effect of extractive-crystallizational separation is observed in the range of neodymium nitrate microconcentrations. A method of neodymium quantitative extraction from lanthanum nitrate solutions with neodymium - lanthanum separation coefficient exceeding 25 is suggested

  2. Improved resins and novel materials and methods for solid phase extraction and high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Freeze, Ronald [Iowa State Univ., Ames, IA (United States)

    1997-10-08

    Solid-phase extraction (SPE) has grown to be one of the most widely used methods for isolation and preconcentration of a vast range of compounds from aqueous solutions. By modifying polymeric SPE resins with chelating functional groups, the selective uptake of metals was accomplished. The resin, along with adsorbed metals, was vaporized in the ICP and detection of the metals was then possible using either mass or emission spectroscopy. Drug analyses in biological fluids have received heightened attention as drug testing is on the increase both in sports and in the work environment. By using a direct-injection technique, biological fluids can be injected directly into the liquid chromatographic system with no pretreatment. A new surfactant, a sulfonated form of Brij-30 (Brij-S) is shown to prevent the uptake of serum proteins on commercial HPLC columns by forming a thin coating on the silica C18 surface. Excellent separations of eight or more drugs with a wide range of retention times were obtained. The separations had sharper peaks and lower retention times than similar separations performed with the surfactant sodium dodecylsulfate (SDS). Quantitative recovery of a number of drugs with limits of detection near 1 ppm with a 5 μl injection volume were obtained. Finally, a method for solid-phase extraction in a syringe is introduced. The system greatly reduced the volume of solvent required to elute adsorbed analytes from the SPE bed while providing a semi-automated setup. SPE in a syringe consists of a very small bed of resin-loaded membrane packed into a GC or HPLC syringe. After extraction, elution was performed with just a few μl of solvent. This small elution volume allowed injection of the eluent directly from the syringe into the chromatographic system, eliminating the handling problems associated with such small volumes.

  3. Direct determination of uranium in the organic phase D2EHPA-TOPO using XRF spectroscopy

    International Nuclear Information System (INIS)

    Stas, J.; Al-Merey, R.; Karajo, J.

    2000-06-01

    Three calibration curves have been carried out to determine uranium concentration in the organic phase (D2EHPA-TOPO) using XRF technique with Cd 109 as a primary exciting source. Copper was used as an internal standard, so the linear relation between relative intensity of uranium against its concentration has been obtained. The range of uranium concentrations studies are (0-100 μg.mL -1 ), (100-1000 μg.mL -1 ) and (1000-6500 μg.mL -1 ), which covered all uranium against its concentration concerning first and second cycles of uranium extraction from phosphoric acid. detection limit was found to be 1.1 μg/ml. The effect of different range of (0.2-0.6 M) D2EHPA and (0.025-0.15 M) TOPO and iron (0-500 μg.mL -1 ) on the accuracy and the precision of uranium determination have been studied and no effect was found. Unknown organic samples have been analyzed using XRF technique and compared with γ-ray, UV and volumetric techniques, obtained results were comparable. (Author)

  4. Analysis of Free Amino Acids in Different Extracts of Orthosiphon stamineus Leaves by High-Performance Liquid Chromatography Combined with Solid-Phase Extraction.

    Science.gov (United States)

    Shafaei, Armaghan; Halim, Nor Hidayah Ab; Zakaria, Norhidayah; Ismail, Zhari

    2017-10-01

    Orthosiphon stamineus (OS) Benth is a medicinal plant and native in Southeast Asia. Previous studies have shown that OS leaves possess antioxidant, cytotoxic, diuretic, antihypertensive, and uricosuric effects. These beneficial effects have been attributed to the presence of primary and secondary metabolites such as polyphenols, amino acids, and flavonoids. To develop and validate an high-performance liquid chromatography (HPLC)-diode array detector (DAD) method combined with solid-phase extraction that involves precolumn derivatization with O -phthaladehyde for simultaneous analysis of free amino acids in OS leaves extracts. OS leaves were extracted with water (OS-W), ethanol (OS-E), methanol (OS-M), 50% ethanol (OS-EW), and 50% methanol (OS-MW). The extracts were treated by C18 cartridge before derivatization, resulting in great improvement of separation by Zorbox Eclipse XDB-C 18 column. The HPLC-DAD method was successfully developed and validated for analyzing the contents of free amino acids in OS extracts. The results showed that l-aspartic acid with 0.93 ± 0.01 nmol/mg was the major free amino acid in OS-W extract. However, in OS-E, OS-M, OS-EW, and OS-MW, l-glutamic acid with 3.53 ± 0.16, 2.17 ± 0.10, 4.01 ± 0.12, and 2.49 ± 0.12 nmol/mg, respectively, was the major free amino acid. Subsequently, l-serine, which was detected in OS-W, OS-E, and OS-M, was the minor free amino acid with 0.33 ± 0.02, 0.12 ± 0.01, and 0.06 ± 0.01 nmol/mg, respectively. However, l-threonine with 0.26 ± 0.02 and 0.19 ± 0.08 nmol/mL in OS-EW and OS-MW, respectively, had the lowest concentration compared with other amino acid components. All validation parameters of the developed method indicate that the method is reliable and efficient to simultaneously determine the free amino acids content for routine analysis of OS extracts. The HPLC-DAD method combined with solid phase extraction was successfully developed and validated for simultaneous determination and

  5. Impact of solvent extraction organics on adsorption and bioleaching of A. ferrooxidans and L. ferriphilum

    Science.gov (United States)

    Hualong, Yu; Xiaorong, Liu

    2017-04-01

    Copper solvent extraction entrained and dissoluted organics (SX organics) in the raffinate during SX operation can contaminated chalcopyrite ores and influence bioleaching efficiency by raffinate recycling. The adsorption and bioleaching of A. ferrooxidans and L. ferriphilum with contaminated ores were investigated. The results showed that, A. ferrooxidans and L. ferriphilum cells could adsorb quickly on minerals, the adsorption rate on contaminated ores were 83% and 60%, respectively, larger than on uncontaminated ores. However, in the bioleaching by the two kinds of acid bacterias, contaminated ores presented a lower bioleaching efficiency.

  6. Determination of Scopolamine in Human Saliva Using Solid Phase Extraction and LC/MS/MS

    Science.gov (United States)

    Wang, Zuwei; Vaksman, Zalman; Boyd, Jason; Putcha, Lakshmi

    2007-01-01

    Purpose: Scopolamine is the preferred treatment for motion sickness during space flight because of its quick onset of action, short half-life and favorable side-effect profile. The dose administered depends on the mode of administration and usually ranges between 0.1 and 0.8 mg. Such small doses make it difficult to detect concentrations of scopolamine in biological fluids by using conventional HPLC methods. To measure scopolamine in saliva and thereby to evaluate the pharmacokinetics of scopolamine, we developed an LC/MS/MS method using off-line solid phase extraction. Method: Samples (0.5mL) were loaded onto Waters Oasis HLB co-polymer cartridges (10 mg, 1 mL) and eluted with 0.5 mL methanol without evaporation and reconstitution. HPLC separation of the eluted sample was performed using an Agilent Zorbax SB-CN column (50 x 2.1 mm) at a flow rate of 0.2 mL/min for 4 minutes. The mobile phase for separation was 90:10 (v/v) methanol: ammonium acetate (2 mM) in water, pH 5.0 +/- 0.1. Concentrations of scopolamine were determined using a Micromass Quattro Micro(TM) mass spectrometer with electrospray ionization (ESI). ESI mass spectra were acquired in positive ion mode with multiple reaction monitoring for the determination of scopolamine m/z = 304.2 yields 138.1 and internal standard (IS) hyoscyamine m/z = 290.2 yields 124.1. Results: The method is rapid, reproducible, specific and has the following parameters: scopolamine and the IS are eluted at 1.7 and 3.2 min respectively. The linear range is 50-5000 pg/mL for scopolamine in saliva with correlation coefficients > 0.99 with a CV < 0.5 %. The intra-day and inter-day CVs are < 15 % for quality control samples with concentrations of 75, 300, 750 and 3000 pg/mL of scopolamine in human saliva. Conclusion: Solid phase extraction allows more rapid sample preparation and greater precision than liquid extraction. Furthermore, we increased the sensitivity and specificity by adjusting the LC mobile phase and using an MS

  7. Extracting the emitter orientation in organic light-emitting diodes from external quantum efficiency measurements

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt, Tobias D., E-mail: Tobias.Schmidt@physik.uni-augsburg.de; Reichardt, Lukas J.; Wehrmeister, Sebastian; Scholz, Bert J.; Mayr, Christian; Brütting, Wolfgang, E-mail: Wolfgang.Bruetting@physik.uni-augsburg.de [Institute of Physics, University of Augsburg, 86135 Augsburg (Germany); Rausch, Andreas F.; Wehlus, Thomas; Reusch, Thilo C. G. [OSRAM OLED GmbH, Wernerwerkstrasse 2, 93049 Regensburg (Germany); Ciarnáin, Rossá Mac; Danz, Norbert [Fraunhofer Institute for Applied Optics and Precision Engineering, 07745 Jena (Germany)

    2014-07-28

    Emitter orientation will play a major role in future applications of organic light-emitting diodes due to its strong impact on the efficiency of the devices. Up to now, determining the orientation of transition dipole moments required elaborate angular-dependent measurements of the light emission pattern. In this paper, we present a simplified and straightforward method to extract the emitter orientation from external quantum efficiency measurements. We demonstrate the validity of the method on three different dye-doped emitting systems.

  8. Oxidative Desulfurization of Gasoline by Ionic Liquids Coupled with Extraction by Organic Solvents

    OpenAIRE

    Abro, Rashid; Gao, Shurong; Chen, Xiaochun; Yu, Guangren; Abdeltawab, Ahmed A.; Al-Deyab, Salem S.

    2016-01-01

    In this work, desulfurization of real fluidized catalytic cracking (FCC) gasoline was investigated in dual steps; first in oxidative desulfurization (ODS) using imidazolium and pyrrolidonium based Brønsted acidic ionic liquids (ILs) as solvent and catalyst and hydrogen peroxide as oxidant. In second step, extractive desulfurization took place using organic solvents of furfural, furfural alcohol and ethylene glycol. Variety of factors such as temperature, time, mass ratio of oil/ILs and regene...

  9. Microfunnel-supported liquid-phase microextraction: application to extraction and determination of Irgarol 1051 and diuron in the Persian Gulf seawater samples.

    Science.gov (United States)

    Saleh, Abolfazl; Sheijooni Fumani, Neda; Molaei, Saeideh

    2014-08-22

    In the present work, microfunnel-supported liquid-phase microextraction method (MF-LPME) based on applying low density organic solvent was developed for the determination of antifoulings (Irgarol 1051, diuron and 3,4-dichloroaniline) from seawater samples. In this method, home-designed MF device was used for facile loading and retrieving of organic solvent during the extraction procedure. The extraction was carried out with introduction of 400 μL of toluene via syringe into the MF device placed on the surface of sample solution (300 mL) containing analytes. After the extraction, extractant layer was narrowed into the capillary part of MF by pushing the device inside the sample and withdrawn by using a syringe to evaporate by nitrogen purging. The residual redissolved into 50 μL methanol, diluted to 100 μL with deionized water and injected into the high performance liquid chromatography with UV detection (HPLC-UV). Several factors influencing the extraction such as the type and volume of extraction solvent, sample pH, extraction time and ionic strength were investigated and optimized. Under the optimized conditions, the limits of detection in seawater were 1.4, 4.8 and 1.0 ng L(-1) for 3,4-dichloroaniline (DCA), diuron and Irgarol 1051, respectively. Enrichment factors were obtained 333, 150 and 373 for DCA, diuron and Irgarol 1051, respectively. The precision of the technique was evaluated in terms of repeatability which was less than 12.0% (n=5). The applicability of the proposed method was evaluated by the extraction and determination of antifoulings from seawater samples collected from harbors of Bushehr located in northern Persian Gulf coast. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2015-01-01

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

  11. Optimization of phenol extraction procedures for preparation of RNA from mammalian lymphoid organs

    Energy Technology Data Exchange (ETDEWEB)

    Griffin, G.D.; Sellin, H.G.; Novelli, G.D.

    1978-07-01

    Methods have been developed to optimize the extraction of RNA from mammalian lymphoid organs (spleen) with respect to both quantity and quality of RNA and with minimal DNA contamination. Nuclease inhibitors, including diethyl pyrocarbonate, polyvinyl sulfate, and bentonite were used in the initial disruption of the tissue, which was accomplished by blender, Dounce homogenizer, or preparation of a cell suspension. Seven buffer systems, varying with respect to pH, detergent, and NaCl concentration, were used in the initial extraction with phenol, and the temperature of extraction was also varied. Protocols involving the selective use of naphthalene 1.5-disulfonic acid and sodium dodecyl sulfate were developed to provide an initial RNA extract with minimal DNA content. Dounce homogenization, followed by separate treatment of nuclear and cytosol fractions, was found to be the most effective technique, both in terms of RNA yield (averaging 76%) and the quality of RNA recovered (as judged by gel electrophoresis). RNA from blender preparations contained larger amounts of DNA and RNA yield was decreased to 54%. RNA extracted from spleen cell suspensions was of poor quality and gave very poor yield (27%).

  12. Fully automated synthesis of 11C-acetate as tumor PET tracer by simple modified solid-phase extraction purification

    International Nuclear Information System (INIS)

    Tang, Xiaolan; Tang, Ganghua; Nie, Dahong

    2013-01-01

    Introduction: Automated synthesis of 11 C-acetate ( 11 C-AC) as the most commonly used radioactive fatty acid tracer is performed by a simple, rapid, and modified solid-phase extraction (SPE) purification. Methods: Automated synthesis of 11 C-AC was implemented by carboxylation reaction of MeMgBr on a polyethylene Teflon loop ring with 11 C-CO 2 , followed by acidic hydrolysis with acid and SCX cartridge, and purification on SCX, AG11A8 and C18 SPE cartridges using a commercially available 11 C-tracer synthesizer. Quality control test and animals positron emission tomography (PET) imaging were also carried out. Results: A high and reproducible decay-uncorrected radiochemical yield of (41.0±4.6)% (n=10) was obtained from 11 C-CO 2 within the whole synthesis time about 8 min. The radiochemical purity of 11 C-AC was over 95% by high-performance liquid chromatography (HPLC) analysis. Quality control test and PET imaging showed that 11 C-AC injection produced by the simple SPE procedure was safe and efficient, and was in agreement with the current Chinese radiopharmaceutical quality control guidelines. Conclusion: The novel, simple, and rapid method is readily adapted to the fully automated synthesis of 11 C-AC on several existing commercial synthesis module. The method can be used routinely to produce 11 C-AC for preclinical and clinical studies with PET imaging. - Highlights: • A fully automated synthesis of 11 C-acetate by simple modified solid-phase extraction purification has been developed. • Typical non-decay-corrected yields were (41.0±4.6)% (n=10) • Radiochemical purity was determined by radio-HPLC analysis on a C18 column using the gradient program, instead of expensive organic acid column or anion column. • QC testing (RCP>99%)

  13. Aqueous-gas phase partitioning and hydrolysis of organic iodides

    International Nuclear Information System (INIS)

    Glowa, G.A.; Wren, J.C.

    2003-01-01

    The volatility and decomposition of organic iodides in a reactor containment building are important parameters to consider when assessing the potential consequences of a nuclear reactor accident. However, there are few experimental data available for the volatilities (often reported as partition coefficients) or few rate constants regarding the decomposition (via hydrolysis) of organic iodides. The partition coefficients and hydrolysis rate constants of eight organic iodides, having a range of molecular structures, have been measured in the current studies. This data, and data accumulated in the literature, have been reviewed and discussed to provide guidelines for appropriate organization of organic iodides for the purpose of modelling iodine behaviour under postulated nuclear reactor accident conditions. After assessment of the partition coefficients and their temperature dependences of many classes of organic compounds, it was found that organic iodides could be divided into two categories based upon their volatility relative to molecular iodine. Similarly, hydrolysis rates and their temperature dependences are assigned to the two categories of organic iodides. (author)

  14. Degradation of the organic phase of bone by osteoclasts

    DEFF Research Database (Denmark)

    Henriksen, Kim; Sørensen, Mette G; Nielsen, Rasmus H

    2006-01-01

    Osteoclasts degrade bone matrix by secretion of hydrochloric acid and proteases. We studied the processes involved in the degradation of the organic matrix of bone in detail and found that lysosomal acidification is involved in this process and that MMPs are capable of degrading the organic matrix...

  15. 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)

  16. Correction of 157-nm lens based on phase ring aberration extraction method

    Science.gov (United States)

    Meute, Jeff; Rich, Georgia K.; Conley, Will; Smith, Bruce W.; Zavyalova, Lena V.; Cashmore, Julian S.; Ashworth, Dominic; Webb, James E.; Rich, Lisa

    2004-05-01

    Early manufacture and use of 157nm high NA lenses has presented significant challenges including: intrinsic birefringence correction, control of optical surface contamination, and the use of relatively unproven materials, coatings, and metrology. Many of these issues were addressed during the manufacture and use of International SEMATECH"s 0.85NA lens. Most significantly, we were the first to employ 157nm phase measurement interferometry (PMI) and birefringence modeling software for lens optimization. These efforts yielded significant wavefront improvement and produced one of the best wavefront-corrected 157nm lenses to date. After applying the best practices to the manufacture of the lens, we still had to overcome the difficulties of integrating the lens into the tool platform at International SEMATECH instead of at the supplier facility. After lens integration, alignment, and field optimization were complete, conventional lithography and phase ring aberration extraction techniques were used to characterize system performance. These techniques suggested a wavefront error of approximately 0.05 waves RMS--much larger than the 0.03 waves RMS predicted by 157nm PMI. In-situ wavefront correction was planned for in the early stages of this project to mitigate risks introduced by the use of development materials and techniques and field integration of the lens. In this publication, we document the development and use of a phase ring aberration extraction method for characterizing imaging performance and a technique for correcting aberrations with the addition of an optical compensation plate. Imaging results before and after the lens correction are presented and differences between actual and predicted results are discussed.

  17. An absorbing microwave micro-solid-phase extraction device used in non-polar solvent microwave-assisted extraction for the determination of organophosphorus pesticides

    International Nuclear Information System (INIS)

    Wang Ziming; Zhao Xin; Xu Xu; Wu Lijie; Su Rui; Zhao Yajing; Jiang Chengfei; Zhang Hanqi; Ma Qiang; Lu Chunmei; Dong Deming

    2013-01-01

    Highlights: ► An absorbing microwave μ-SPE device packed with activated carbon was used. ► Absorbing microwave μ-SPE device was made and used to enrich the analytes. ► Absorbing microwave μ-SPE device was made and used to heat samples directly. ► MAE-μ-SPE was applied to the extraction of OPPs with non-polar solvent only. - Abstract: A single-step extraction-cleanup method, including microwave-assisted extraction (MAE) and micro-solid-phase extraction (μ-SPE), was developed for the extraction of ten organophosphorus pesticides in vegetable and fruit samples. Without adding any polar solvent, only one kind of non-polar solvent (hexane) was used as extraction solvent in the whole extraction step. Absorbing microwave μ-SPE device, was prepared by packing activated carbon with microporous polypropylene membrane envelope, and used as not only the sorbent in μ-SPE, but also the microwave absorption medium. Some experimental parameters effecting on extraction efficiency was investigated and optimized. 1.0 g of sample, 8 mL of hexane and three absorbing microwave μ-SPE devices were added in the microwave extraction vessel, the extraction was carried out under 400 W irradiation power at 60 °C for 10 min. The extracts obtained by MAE-μ-SPE were directly analyzed by GC–MS without any clean-up process. The recoveries were in the range of 93.5–104.6%, and the relative standard deviations were lower than 8.7%.

  18. An absorbing microwave micro-solid-phase extraction device used in non-polar solvent microwave-assisted extraction for the determination of organophosphorus pesticides

    Energy Technology Data Exchange (ETDEWEB)

    Wang Ziming, E-mail: wangziming@jlu.edu.cn [College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012 (China); College of Environment and Resources, Jilin University, 2699 Qianjin Street, Changchun 130012 (China); Zhao Xin; Xu Xu; Wu Lijie; Su Rui; Zhao Yajing; Jiang Chengfei; Zhang Hanqi [College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012 (China); Ma Qiang [Chinese Academy of Inspection and Quarantine, Beijing 100123 (China); Lu Chunmei [College of Technology Center, Jilin Entry-Exit Inspection and Quarantine Bureau, Changchun 130062 (China); Dong Deming [College of Environment and Resources, Jilin University, 2699 Qianjin Street, Changchun 130012 (China)

    2013-01-14

    Highlights: Black-Right-Pointing-Pointer An absorbing microwave {mu}-SPE device packed with activated carbon was used. Black-Right-Pointing-Pointer Absorbing microwave {mu}-SPE device was made and used to enrich the analytes. Black-Right-Pointing-Pointer Absorbing microwave {mu}-SPE device was made and used to heat samples directly. Black-Right-Pointing-Pointer MAE-{mu}-SPE was applied to the extraction of OPPs with non-polar solvent only. - Abstract: A single-step extraction-cleanup method, including microwave-assisted extraction (MAE) and micro-solid-phase extraction ({mu}-SPE), was developed for the extraction of ten organophosphorus pesticides in vegetable and fruit samples. Without adding any polar solvent, only one kind of non-polar solvent (hexane) was used as extraction solvent in the whole extraction step. Absorbing microwave {mu}-SPE device, was prepared by packing activated carbon with microporous polypropylene membrane envelope, and used as not only the sorbent in {mu}-SPE, but also the microwave absorption medium. Some experimental parameters effecting on extraction efficiency was investigated and optimized. 1.0 g of sample, 8 mL of hexane and three absorbing microwave {mu}-SPE devices were added in the microwave extraction vessel, the extraction was carried out under 400 W irradiation power at 60 Degree-Sign C for 10 min. The extracts obtained by MAE-{mu}-SPE were directly analyzed by GC-MS without any clean-up process. The recoveries were in the range of 93.5-104.6%, and the relative standard deviations were lower than 8.7%.

  19. Extraction of actinide and lanthanide complexonates in two-phase aqueous system potassium carbonate-polyethylene glycol-water

    International Nuclear Information System (INIS)

    Molochnikova, N.P.; Shkinev, V.M.; Spivakov, B.Ya.; Zolotov, Yu.A.; Myasoedov, B.F.

    1988-01-01

    Extraction system on the basis of polyethylene glycol for the concentration, isolation and separation of actinides is suggested. Extraction of actinides and lanthanides in two-phase aqueous system: potassium carbonate - polyethylene glycol - water in the presence of different complexones is investigated. Trivalent actinides are extracted quantitatively by polyethylene glycol from potassium carbonate solutions in the system with xylenol orange and alizarin-complexone. Under the conditions uranium (6) and plutonium (4) are extracted into the phase, enriched by polyethylene glycol, quite insignificantly, which permits to separate them from trivalent actinides with the separation factor of 10 2 - 10 3 . For actinide and lanthanide separation two complexones were introduced into the system, one of them being extractant, the other one - camouflaging reactant. The best results are obtained for the mixture of xylenol orange and hydroxyethylenediphosphonic acid. Separation coefficients for americium and europium constitute 4.5 - 5.6

  20. A comparison of sample preparation methods for extracting volatile organic compounds (VOCs) from equine faeces using HS-SPME.

    Science.gov (United States)

    Hough, Rachael; Archer, Debra; Probert, Christopher

    2018-01-01

    Disturbance to the hindgut microbiota can be detrimental to equine health. Metabolomics provides a robust approach to studying the functional aspect of hindgut microorganisms. Sample preparation is an important step towards achieving optimal results in the later stages of analysis. The preparation of samples is unique depending on the technique employed and the sample matrix to be analysed. Gas chromatography mass spectrometry (GCMS) is one of the most widely used platforms for the study of metabolomics and until now an optimised method has not been developed for equine faeces. To compare a sample preparation method for extracting volatile organic compounds (VOCs) from equine faeces. Volatile organic compounds were determined by headspace solid phase microextraction gas chromatography mass spectrometry (HS-SPME-GCMS). Factors investigated were the mass of equine faeces, type of SPME fibre coating, vial volume and storage conditions. The resultant method was unique to those developed for other species. Aliquots of 1000 or 2000 mg in 10 ml or 20 ml SPME headspace were optimal. From those tested, the extraction of VOCs should ideally be performed using a divinylbenzene-carboxen-polydimethysiloxane (DVB-CAR-PDMS) SPME fibre. Storage of faeces for up to 12 months at - 80 °C shared a greater percentage of VOCs with a fresh sample than the equivalent stored at - 20 °C. An optimised method for extracting VOCs from equine faeces using HS-SPME-GCMS has been developed and will act as a standard to enable comparisons between studies. This work has also highlighted storage conditions as an important factor to consider in experimental design for faecal metabolomics studies.

  1. Assimilable organic carbon (AOC) in soil water extracts using Vibrio harveyi BB721 and its implication for microbial biomass.

    Science.gov (United States)

    Ma, Jincai; Ibekwe, A Mark; Wang, Haizhen; Xu, Jianming; Leddy, Menu; Yang, Ching-Hong; Crowley, David E

    2012-01-01

    Assimilable organic carbon (AOC) is commonly used to measure the growth potential of microorganisms in water, but has not yet been investigated for measuring microbial growth potential in soils. In this study, a simple, rapid, and non-growth based assay to determine AOC in soil was developed using a naturally occurring luminous strain Vibrio harveyi BB721 to determine the fraction of low molecular weight organic carbon in soil water extract. Calibration of the assay was achieved by measuring the luminescence intensity of starved V. harveyi BB721 cells in the late exponential phase with a concentration range from 0 to 800 µg l(-1) glucose (equivalent to 0-16.0 mg glucose C kg(-1) soil) with the detection limit of 10 µg l(-1) equivalent to 0.20 mg glucose C kg(-1) soil. Results showed that bioluminescence was proportional to the concentration of glucose added to soil. The luminescence intensity of the cells was highly pH dependent and the optimal pH was about 7.0. The average AOC concentration in 32 soils tested was 2.9±2.2 mg glucose C kg(-1). Our data showed that AOC levels in soil water extracts were significantly correlated (Pgrowth bioluminescence based assay. Understanding the levels of AOC in soil water extract provides new insights into our ability to estimate the most available carbon pool to bacteria in soil that may be easily assimilated into cells for many metabolic processes and suggest possible the links between AOC, microbial regrowth potential, and microbial biomass in soils.

  2. Assimilable organic carbon (AOC in soil water extracts using Vibrio harveyi BB721 and its implication for microbial biomass.

    Directory of Open Access Journals (Sweden)

    Jincai Ma

    Full Text Available Assimilable organic carbon (AOC is commonly used to measure the growth potential of microorganisms in water, but has not yet been investigated for measuring microbial growth potential in soils. In this study, a simple, rapid, and non-growth based assay to determine AOC in soil was developed using a naturally occurring luminous strain Vibrio harveyi BB721 to determine the fraction of low molecular weight organic carbon in soil water extract. Calibration of the assay was achieved by measuring the luminescence intensity of starved V. harveyi BB721 cells in the late exponential phase with a concentration range from 0 to 800 µg l(-1 glucose (equivalent to 0-16.0 mg glucose C kg(-1 soil with the detection limit of 10 µg l(-1 equivalent to 0.20 mg glucose C kg(-1 soil. Results showed that bioluminescence was proportional to the concentration of glucose added to soil. The luminescence intensity of the cells was highly pH dependent and the optimal pH was about 7.0. The average AOC concentration in 32 soils tested was 2.9±2.2 mg glucose C kg(-1. Our data showed that AOC levels in soil water extracts were significantly correlated (P<0.05 with microbial biomass determined as microbial biomass carbon, indicating that the AOC concentrations determined by the method developed might be a good indicator of soil microbial biomass. Our findings provide a new approach that may be used to determine AOC in environmental samples using a non-growth bioluminescence based assay. Understanding the levels of AOC in soil water extract provides new insights into our ability to estimate the most available carbon pool to bacteria in soil that may be easily assimilated into cells for many metabolic processes and suggest possible the links between AOC, microbial regrowth potential, and microbial biomass in soils.

  3. Ginseng Berry Extract Prevents Atherogenesis via Anti-Inflammatory Action by Upregulating Phase II Gene Expression

    Directory of Open Access Journals (Sweden)

    Chun-Ki Kim

    2012-01-01

    Full Text Available Ginseng berry possesses higher ginsenoside content than its root, which has been traditionally used in herbal medicine for many human diseases, including atherosclerosis. We here examined the antiatherogenic effects of the Korean ginseng berry extract (KGBE and investigated its underlying mechanism of action in vitro and in vivo. Administration of KGBE decreased atherosclerotic lesions, which was inversely correlated with the expression levels of phase II genes to include heme oxygenase-1 (HO-1 and glutamine-cysteine ligase (GCL. Furthermore, KGBE administration suppressed NF-κB-mediated expression of atherogenic inflammatory genes (TNF-α, IL-1β, iNOS, COX-2, ICAM-1, and VCAM-1, without altering serum cholesterol levels, in ApoE-/- mice fed a high fat-diet. Treatment with KGBE increased phase II gene expression and suppressed lipopolysaccharide-induced reactive oxygen species production, NF-κB activation, and inflammatory gene expression in primary macrophages. Importantly, these cellular events were blocked by selective inhibitors of HO-1 and GCL. In addition, these inhibitors reversed the suppressive effect of KGBE on TNF-α-mediated induction of ICAM-1 and VCAM-1, resulting in decreased interaction between endothelial cells and monocytes. These results suggest that KGBE ameliorates atherosclerosis by inhibiting NF-κB-mediated expression of atherogenic genes via upregulation of phase II enzymes and thus has therapeutic or preventive potential for atherosclerosis.

  4. Enantioseparation of Racemic Flurbiprofen by Aqueous Two-Phase Extraction With Binary Chiral Selectors of L-dioctyl Tartrate and L-tryptophan.

    Science.gov (United States)

    Chen, Zhi; Zhang, Wei; Wang, Liping; Fan, Huajun; Wan, Qiang; Wu, Xuehao; Tang, Xunyou; Tang, James Z

    2015-09-01

    A novel method for chiral separation of flurbiprofen enantiomers was developed using aqueous two-phase extraction (ATPE) coupled with biphasic recognition chiral extraction (BRCE). An aqueous two-phase system (ATPS) was used as an extracting solvent which was composed of ethanol (35.0% w/w) and ammonium sulfate (18.0% w/w). The chiral selectors in ATPS for BRCE consideration were L-dioctyl tartrate and L-tryptophan, which were screened from amino acids, β-cyclodextrin derivatives, and L-tartrate esters. Factors such as the amounts of L-dioctyl tartrate and L-tryptophan, pH, flurbiprofen concentration, and the operation temperature were investigated in terms of chiral separation of flurbiprofen enantiomers. The optimum conditions were as follows: L-dioctyl tartrate, 80 mg; L-tryptophan, 40 mg; pH, 4.0; flurbiprofen concentration, 0.10 mmol/L; and temperature, 25 °C. The maximum separation factor α for flurbiprofen enantiomers could reach 2.34. The mechanism of chiral separation of flurbiprofen enantiomers is discussed and studied. The results showed that synergistic extraction has been established by L-dioctyl tartrate and L-tryptophan, which enantioselectively recognized R- and S-enantiomers in top and bottom phases, respectively. Compared to conventional liquid-liquid extraction, ATPE coupled with BRCE possessed higher separation efficiency and enantioselectivity without the use of any other organic solvents. The proposed method is a potential and powerful alternative to conventional extraction for separation of various enantiomers. © 2015 Wiley Periodicals, Inc.

  5. A phase model of intergenerational learning in organizations

    NARCIS (Netherlands)

    Gerpott, F.H.; Lehmann-Willenbrock, N.; Voelpel, S.C.

    Demographic changes challenge organizations to qualify employees across all career stages and to ensure the transfer of company-specific knowledge between experienced and young workers. Human resource development programs for employees from different generations may help address these challenges.

  6. Application of cation-exchange solid-phase extraction for the analysis of amino alcohols from water and human plasma for verification of Chemical Weapons Convention.

    Science.gov (United States)

    Kanaujia, Pankaj K; Tak, Vijay; Pardasani, Deepak; Gupta, A K; Dubey, D K

    2008-03-28

    The analysis of nitrogen containing amino alcohols, which are the precursors and degradation products of nitrogen mustards and nerve agent VX, constitutes an important aspect for verifying the compliance to the CWC (Chemical Weapons Convention). This work devotes on the development of solid-phase extraction method using silica- and polymer-based SCX (strong cation-exchange) and MCX (mixed-mode strong cation-exchange) cartridges for N,N-dialkylaminoethane-2-ols and alkyl N,N-diethanolamines, from water. The extracted analytes were analyzed by GC-MS (gas chromatography-mass spectrometry) in the full scan and selected ion monitoring modes. The extraction efficiencies of SCX and MCX cartridges were compared, and results revealed that SCX performed better. Extraction parameters, such as loading capacity, extraction solvent, its volume, and washing solvent were optimized. Best recoveries were obtained using 2 mL methanol containing 10% NH(4)OH and limits of detection could be achieved up to 5 x 10(-3) microg mL(-1) in the selected ion monitoring mode and 0.01 microg mL(-1) in full scan mode. The method was successfully employed for the detection and identification of amino alcohol present in water sample sent by Organization for Prohibition of Chemical Weapons (OPCW) in the official proficiency tests. The method was also applied to extract the analytes from human plasma. The SCX cartridge showed good recoveries of amino alcohols from human plasma after protein precipitation.

  7. Inorganic-Organic hybrid materials for uranium extraction from phosphoric acid

    International Nuclear Information System (INIS)

    El-Mourabit, Sabah

    2013-01-01

    Phosphate rocks are industrially processed in large quantities to produce phosphoric acid and fertilisers. These rocks contain significant concentration of uranium (50 to 300 ppm) which could be interesting for nuclear industry. This work deals with the valorisation of uranium as a by-product from fertiliser industry. The aim of this study is to develop a hybrid material, constituted of an inorganic solid support grafted with an extractant (complexing molecule), which can extract selectively uranium from phosphoric acid medium. The first step of our approach was to identify an inorganic support which is stable under these particular conditions (strong acidity and complexing medium). The chemical and mechanical stability of different meso-porous materials, such as silica, glass and carbon was studied. In a second phase, we focused on the identification and the optimisation of complexing molecules, specific of uranium in phosphoric acid. These ligands were then grafted on the most stable solids. Finally, the efficiency of these hybrid systems was evaluated through different tests of extraction, selectivity and de-extraction. (author) [fr

  8. Sensor-Based Auto-Focusing System Using Multi-Scale Feature Extraction and Phase Correlation Matching

    Directory of Open Access Journals (Sweden)

    Jinbeum Jang

    2015-03-01

    Full Text Available This paper presents a novel auto-focusing system based on a CMOS sensor containing pixels with different phases. Robust extraction of features in a severely defocused image is the fundamental problem of a phase-difference auto-focusing system. In order to solve this problem, a multi-resolution feature extraction algorithm is proposed. Given the extracted features, the proposed auto-focusing system can provide the ideal focusing position using phase correlation matching. The proposed auto-focusing (AF algorithm consists of four steps: (i acquisition of left and right images using AF points in the region-of-interest; (ii feature extraction in the left image under low illumination and out-of-focus blur; (iii the generation of two feature images using the phase difference between the left and right images; and (iv estimation of the phase shifting vector using phase correlation matching. Since the proposed system accurately estimates the phase difference in the out-of-focus blurred image under low illumination, it can provide faster, more robust auto focusing than existing systems.

  9. Biological activities of organic extracts of four Aureobasidium pullulans varieties isolated from extreme marine and terrestrial habitats.

    Science.gov (United States)

    Botić, Tanja; Kralj-Kunčič, Marjetka; Sepčić, Kristina; Batista, Urška; Zalar, Polona; Knez, Željko; Gunde-Cimerman, Nina

    2014-01-01

    We report on the screening for biological activities of organic extracts from seven strains that represent four varieties of the fungus Aureobasidium pullulans, that is A. pullulans var. melanogenum, A. pullulans var. pullulans, A. pullulans var. subglaciale and A. pullulans var. namibiae. We monitored haemolysis, cytotoxicity, antioxidant capacity and growth inhibition against three bacterial species. The haemolytic activity of A. pullulans var. pullulans EXF-150 strain was due to five different haemolytically active fractions. Extracts from all of the other varieties contained at least one haemolytically active fraction. Short-term exposure of cell lines to these haemolytically active organic extracts resulted in more than 95% cytotoxicity. Strong antioxidant capacity, corresponding to 163.88 μg ascorbic acid equivalent per gram of total solid, was measured in the organic extract of the strain EXF-3382, obtained from A. pullulans var. melanogenum, isolated from the deep sea. Organic extracts from selected varieties of A. pullulans exhibited weak antibacterial activities.

  10. The variability of standard artificial soils: Behaviour, extractability and bioavailability of organic pollutants

    International Nuclear Information System (INIS)

    Hofman, Jakub; Hovorková, Ivana; Semple, Kirk T.

    2014-01-01

    Highlights: • Artificial soils from different laboratories revealed different fates, behaviour and bioavailability of lindane and phenanthrene. • Lindane behaviour was related to organic carbon. • Phenanthrene behaviour was significantly affected by degrading microorganisms from peat. • Sterilization of artificial soils might reduce unwanted variability. -- Abstract: Artificial soil is an important standard medium and reference material for soil ecotoxicity bioassays. Recent studies have documented the significant variability of their basic properties among different laboratories. Our study investigated (i) the variability of ten artificial soils from different laboratories by means of the fate, extractability and bioavailability of phenanthrene and lindane, and (ii) the relationships of these results to soil properties and ageing. Soils were spiked with 14 C-phenanthrene and 14 C-lindane, and the total residues, fractions extractable by hydroxypropyl-β-cyclodextrin, and the fractions of phenanthrene mineralizable by bacteria were determined after 1, 14, 28 and 56 days. Significant temporal changes in total residues and extractable and mineralizable fractions were observed for phenanthrene, resulting in large differences between soils after 56 days. Phenanthrene mineralization by indigenous peat microorganisms was suggested as the main driver of that, outweighing the effects of organic matter. Lindane total residues and extractability displayed much smaller changes over time and smaller differences between soils related to organic matter. Roughly estimated, the variability between the artificial soils was comparable to natural soils. The implications of such variability for the results of toxicity tests and risk assessment decisions should be identified. We also suggested that the sterilization of artificial soils might reduce unwanted variability

  11. The variability of standard artificial soils: Behaviour, extractability and bioavailability of organic pollutants

    Energy Technology Data Exchange (ETDEWEB)

    Hofman, Jakub, E-mail: hofman@recetox.muni.cz [Research Centre for Toxic Compounds in the Environment (RECETOX), Faculty of Science, Masaryk University, Kamenice 753/5, Brno CZ-62500 (Czech Republic); Hovorková, Ivana [Research Centre for Toxic Compounds in the Environment (RECETOX), Faculty of Science, Masaryk University, Kamenice 753/5, Brno CZ-62500 (Czech Republic); Semple, Kirk T. [Lancaster Environment Centre, Lancaster University, Lancaster LA1 4YQ (United Kingdom)

    2014-01-15

    Highlights: • Artificial soils from different laboratories revealed different fates, behaviour and bioavailability of lindane and phenanthrene. • Lindane behaviour was related to organic carbon. • Phenanthrene behaviour was significantly affected by degrading microorganisms from peat. • Sterilization of artificial soils might reduce unwanted variability. -- Abstract: Artificial soil is an important standard medium and reference material for soil ecotoxicity bioassays. Recent studies have documented the significant variability of their basic properties among different laboratories. Our study investigated (i) the variability of ten artificial soils from different laboratories by means of the fate, extractability and bioavailability of phenanthrene and lindane, and (ii) the relationships of these results to soil properties and ageing. Soils were spiked with {sup 14}C-phenanthrene and {sup 14}C-lindane, and the total residues, fractions extractable by hydroxypropyl-β-cyclodextrin, and the fractions of phenanthrene mineralizable by bacteria were determined after 1, 14, 28 and 56 days. Significant temporal changes in total residues and extractable and mineralizable fractions were observed for phenanthrene, resulting in large differences between soils after 56 days. Phenanthrene mineralization by indigenous peat microorganisms was suggested as the main driver of that, outweighing the effects of organic matter. Lindane total residues and extractability displayed much smaller changes over time and smaller differences between soils related to organic matter. Roughly estimated, the variability between the artificial soils was comparable to natural soils. The implications of such variability for the results of toxicity tests and risk assessment decisions should be identified. We also suggested that the sterilization of artificial soils might reduce unwanted variability.

  12. Antiperoxidative Activity of Tetracarpidium conophorum Leaf Extract in Reproductive Organs of Male Rats