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Sample records for on-line sorbent extraction

  1. Miniaturized DNA aptamer-based monolithic sorbent for selective extraction of a target analyte coupled on-line to nanoLC.

    Science.gov (United States)

    Brothier, Fabien; Pichon, Valérie

    2014-12-01

    A complete characterization of a novel target-specific DNA aptamer-based miniaturized solid phase extraction (SPE)-sorbent coupled on-line to nanoLC is presented. A miniaturized oligosorbent (mOS) was prepared via the in situ sol-gel synthesis of a hybrid organic-inorganic monolith in 100 μm i.d. capillary columns using tetraethoxysilane and 3-aminopropyltriethoxysilane as precursors, followed by covalent binding of a 5'-amino-modified DNA aptamer with a C12 spacer arm specific for a molecule of small molecular weight. Ochratoxin A (OTA), one of the most abundant naturally occurring mycotoxins, was chosen as model analyte to demonstrate the principle of such an approach. The mOS was coupled on-line to RP-nanoLC-LIF. Selective extraction of OTA on several mOSs was demonstrated with an average extraction recovery above 80 % when percolating spiked binding buffer and a low recovery on control monoliths grafted with a non-specific aptamer. Reproducibility of mOSs preparation was highlighted by comparing extraction yields. Otherwise, the mOSs demonstrated no cross-reactivity towards an OTA structural analogue, i.e., ochratoxin B. Due to the high specific surface area of the hybrid silica-based monolith, the coverage density of DNA aptamers covalently immobilized in the capillaries was very high and reached 6.27 nmol μL(-1), thus leading to a capacity above 5 ng of OTA. This miniaturized device was then applied to the selective extraction of OTA from beer samples. It revealed to be effective in isolating OTA from this complex matrix, thus improving the reliability of its analysis at the trace level.

  2. Molecularly imprinted polymers for on-line extraction techniques.

    Science.gov (United States)

    Moein, Mohammad M; Abdel-Rehim, Mohamed

    2015-01-01

    Recent years have seen an increasing interest in the use of molecularly imprinted polymers (MIPs) as a sorbent for different extraction methods and this is due to its high selectivity. The MIP is designed to show specificity for the analyte of interest. Moreover, MIPs show physical robustness, resistance to high temperatures and pressures, and stability in the presence of acids, bases and a wide range of organic solvents. In the present article, various novel sample preparation techniques which MIPs applied as sorbent and on-line connected with analytical instruments were highlighted and discussed. The future aspects of MIPs as well were described.

  3. Automated on-line preconcentration of palladium on different sorbents and its determination in environmental samples.

    Science.gov (United States)

    Sánchez Rojas, Fuensanta; Bosch Ojeda, Catalina; Cano Pavón, José Manuel

    2007-01-01

    The determination of noble metals in environmental samples is of increasing importance. Palladium is often employed as a catalyst in chemical industry and is also used with platinum and rhodium in motor car catalytic converters which might cause environmental pollution problems. Two different sorbents for palladium preconcentration in different samples were investigated: silica gel functionalized with 1,5-bis(di-2-pyridyl)methylene tbiocarbohydrazide (DPTH-gel) and [1,5-Bis(2-pyridyl)-3-sulphophenyI methylene thiocarbonohydrazide (PSTH) immobilised on an anion-exchange resin (Dowex lx8-200)]. The sorbents were tested in a micro-column, placed in the auto-sampler arm, at the flow rate 2.8 mL min(-1). Elution was performed with 4 M HCl and 4 M HNO3, respectively. Satisfactory results were obtained for two sorbents.

  4. Amberlite XAD-2 functionalized with 2-aminothiophenol as a new sorbent for on-line preconcentration of cadmium and copper.

    Science.gov (United States)

    Lemos, Valfredo Azevedo; Baliza, Patrícia Xavier

    2005-09-15

    A new functionalized resin has been applied in an on-line preconcentration system for copper and cadmium determination. Amberlite XAD-2 was functionalized by coupling it to 2-aminothiophenol (AT-XAD) by means of an NN spacer. This resin was packed in a minicolumn and used as sorbent in the on-line system. Metal ions were sorbed in the minicolumn, from which it could be eluted directly to the nebulizer-burner system of the flame atomic absorption spectrometer (FAAS). Elution of Cd(II) and Cu(II) from minicolumn can be made with 0.50moll(-1) HCl or HNO(3). The enrichment factors obtained were 28 (Cd) and 14 (Cu), for 60s preconcentration time, and 74 (Cd) and 35 (Cu), if used 180 s preconcentration time. The proposed procedure allowed the determination of cadmium and copper with detection limits of 0.14 and 0.54mugl(-1), respectively, when used preconcentration periods of 180s. The effects of foreign ions on the adsorption of these metal ions are reported. The validation of the procedure was carried out by analysis of certified reference material. This procedure was applied to cadmium and copper determination in natural, drink and tap water samples.

  5. Development of Novel Sorbents for Uranium Extraction from Seawater

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Wenbin; Taylor-Pashow, Kathryn

    2014-01-08

    As the uranium resource in terrestrial ores is limited, it is difficult to ensure a long-term sustainable nuclear energy technology. The oceans contain approximately 4.5 billion tons of uranium, which is one thousand times the amount of uranium in terrestrial ores. Development of technologies to recover the uranium from seawater would greatly improve the uranium resource availability, sustaining the fuel supply for nuclear energy. Several methods have been previously evaluated including solvent extraction, ion exchange, flotation, biomass collection, and adsorption; however, none have been found to be suitable for reasons such as cost effectiveness, long term stability, and selectivity. Recent research has focused on the amidoxime functional group as a promising candidate for uranium sorption. Polymer beads and fibers have been functionalized with amidoxime functional groups, and uranium adsorption capacities as high as 1.5 g U/kg adsorbent have recently been reported with these types of materials. As uranium concentration in seawater is only ~3 ppb, great improvements to uranium collection systems must be made in order to make uranium extraction from seawater economically feasible. This proposed research intends to develop transformative technologies for economic uranium extraction from seawater. The Lin group will design advanced porous supports by taking advantage of recent breakthroughs in nanoscience and nanotechnology and incorporate high densities of well-designed chelators into such nanoporous supports to allow selective and efficient binding of uranyl ions from seawater. Several classes of nanoporous materials, including mesoporous silica nanoparticles (MSNs), mesoporous carbon nanoparticles (MCNs), meta-organic frameworks (MOFs), and covalent-organic frameworks (COFs), will be synthesized. Selective uranium-binding liagnds such as amidoxime will be incorporated into the nanoporous materials to afford a new generation of sorbent materials that will be

  6. Transport extraction for trace element separation and preconcentration. Pt. 3; Polyurethane foam sorbent supported transport extraction

    Energy Technology Data Exchange (ETDEWEB)

    Palagyi, S. (Inst. of Inorganic and Analytical Chemistry, Eoetvoes Univ., Budapest (Hungary)); Braun, T. (Inst. of Inorganic and Analytical Chemistry, Eoetvoes Univ., Budapest (Hungary))

    1994-01-01

    A new method of sorbent supported transport extraction based on the use of open-cell polyurethane foam sorbents in solvent sublation separation has been developed. The method has been shown to be effective for the separation and preconcentration of radioiodine and/or stable iodine from 4 l of deionized, drinking (tap) and surface (river) waters using N-cetylpyridinium chloride as the cationic surfactant and N[sub 2] carrier gas as the bubbling medium. A transport extraction efficiency of about 94% was obtained in 60 to 90 min; a 300-fold preconcentration was found for radioiodine as measured by direct radioactivity counting. Both radioiodine and stable iodine can be back-extracted from the polyurethane foam support (e.g. into acetone with an efficiency of almost 95%). (orig.)

  7. Selective extraction of nitroaromatic explosives by using molecularly imprinted silica sorbents.

    Science.gov (United States)

    Lordel, Sonia; Chapuis-Hugon, Florence; Eudes, Véronique; Pichon, Valérie

    2011-01-01

    Two molecularly imprinted silicas (MISs) were synthesized and used as selective sorbents for the extraction of nitroaromatic explosives in post-blast samples. The synthesis of the MISs was carried out with phenyltrimethoxysilane as monomer, 2,4-dinitrotoluene (2,4-DNT) as template and triethoxysilane as cross-linker by a sol-gel approach in two molar ratios: 1/4/20 and 1/4/30 (template/monomer/cross-linker). Non-imprinted silica sorbents were also prepared following the same procedures without introducing the template. An optimized procedure dedicated to the selective treatment of aqueous samples was developed for both MISs for the simultaneous extraction of the template and other nitroaromatic compounds commonly used as explosives. The capacity of the MISs was measured by the extraction of increasing amounts of 2,4-DNT in pure water and is higher than 3.2 mg/g of sorbent for each MIS. For the first time, four nitroaromatic compounds were selectively extracted and determined simultaneously with extraction recoveries higher than 79%. The potential of these sorbents was then highlighted by their use for the clean-up of post-blast samples (motor oil, post-mortem blood, calcined fragments, etc.). The results were compared to those obtained using a conventional sorbent, thus demonstrating the interest of the use of these MISs as selective sorbents.

  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. Extraction of trace nitrophenols in environmental water samples using boronate affinity sorbent

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yong; Mei, Meng; Huang, Xiaojia, E-mail: hxj@xmu.edu.cn; Yuan, Dongxing

    2015-10-29

    In this research, the applicability of a new sorbent based on boronate affinity material is demonstrated. For this purpose, six strong polar nitrophenols were selected as models which are difficult to be extracted in neutral form (only based on hydrophobic interactions). The extracted nitrophenols were separated and determined by high-performance liquid chromatography with diode array detection. The sorbent was synthesized by in situ copolymerization of 3-acrylamidophenylboronic acid and divinylbenzene using dimethyl sulfoxide and azobisisobutyronitrile as porogen solvent and initiator, respectively. The effect of the preparation parameters in the polymerization mixture on extraction performance was investigated in detail. The size and morphology of the sorbent have been characterized via different techniques such as infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. The important parameters influencing the extraction efficiency were studied and optimized thoroughly. Under the optimum extraction conditions, the limits of detection (S/N = 3) and limits of quantification (S/N = 10) for the target nitrophenols were 0.097–0.28 and 0.32–0.92 μg/L, respectively. The precision of the proposed method was evaluated in terms of intra- and inter-assay variability calculated as RSD, and it was found that the RSDs were all below 9%. Finally, the developed method was successfully applied for environmental water samples such as wastewater, tap, lake and river water. The recoveries varied within the range of 71.2–115% with RSD below 11% in all cases. The results well demonstrate that the new boronate affinity sorbent can extract nitrophenols effectively through multi-interactions including boron–nitrogen coordination, hydrogen-bond and hydrophobic interactions between sorbent and analytes. - Highlights: • A new boronate affinity sorbent (BAS) was prepared. • The BAS was used as the extractive medium of stir

  10. Polypyrrole/silica/magnetite nanoparticles as a sorbent for the extraction of sulfonamides from water samples.

    Science.gov (United States)

    Sukchuay, Thanyaporn; Kanatharana, Proespichaya; Wannapob, Rodtichoti; Thavarungkul, Panote; Bunkoed, Opas

    2015-09-08

    A magnetic solid-phase extraction sorbent of polypyrrole/silica/magnetite nanoparticles was successfully synthesized and applied for the extraction and preconcentration of sulfonamides in water samples. The magnetite nanoparticles provided a simple and fast separation method for the analytes in water samples. The silica coating increased the surface area that helped to increase the polypyrrole layer. The polypyrrole-coated silica provided a high extraction efficiency due to the π-π and hydrophobic interactions between the polypyrrole and sulfonamides. Several parameters that affected the extraction efficiencies, i.e. the amount of sorbent, pH of the sample, extraction time, extraction temperature, ionic strength, and desorption conditions were investigated. Under the optimal conditions, the method was linear over the range of 0.30-200 μg/L for sulfadiazine and sulfamerazine, and 1.0-200 μg/L for sulfamethazine and sulfamonomethoxine. The limit of detection was 0.30 μg/L for sulfadiazine and sulfamerazine and 1.0 μg/L for sulfamethazine and sulfamonomethoxine. This simple and rapid method was successfully applied to efficiently extract sulfonamides from water samples. It showed a high extraction efficiency for all tested sulfonamides, and the recoveries were in the range of 86.7-99.7% with relative standard deviations of < 6%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Determination of polar aromatic amines using newly synthesized sol-gel titanium (IV) butoxide cyanopropyltriethoxysilane as solid phase extraction sorbent.

    Science.gov (United States)

    Miskam, Mazidatulakmam; Abu Bakar, Nor Kartini; Mohamad, Sharifah

    2014-03-01

    A solid phase extraction (SPE) method has been developed using a newly synthesized titanium (IV) butoxide-cyanopropyltriethoxysilane (Ti-CNPrTEOS) sorbent for polar selective extraction of aromatic amines in river water sample. The effect of different parameters on the extraction recovery was studied using the SPE method. The applicability of the sorbents for the extraction of polar aromatic amines by the SPE was extensively studied and evaluated as a function of pH, conditioning solvent, sample loading volume, elution solvent and elution solvent volume. The optimum experimental conditions were sample at pH 7, dichloromethane as conditioning solvent, 10 mL sample loading volume and 5 mL of acetonitrile as the eluting solvent. Under the optimum conditions, the limit of detection (LOD) and limit of quantification (LOQ) for solid phase extraction using Ti-CNPrTEOS SPE sorbent (0.01-0.2; 0.03-0.61 µg L(-1)) were lower compared with those achieved using Si-CN SPE sorbent (0.25-1.50; 1.96-3.59 µg L(-1)) and C18 SPE sorbent (0.37-0.98; 1.87-2.87 µg L(-1)) with higher selectivity towards the extraction of polar aromatic amines. The optimized procedure was successfully applied for the solid phase extraction method of selected aromatic amines in river water, waste water and tap water samples prior to the gas chromatography-flame ionization detector separation.

  12. Solid-phase extraction of flavonoids in honey samples using carbamate-embedded triacontyl-modified silica sorbent.

    Science.gov (United States)

    Liu, Houmei; Zhang, Mingliang; Guo, Yong; Qiu, Hongdeng

    2016-08-01

    In this study, carbamate-embedded triacontyl-modified silica (Sil-CBM-C30) is successfully prepared and used as an efficient sorbent for solid-phase extraction. The extraction performance of the resultant sorbent is evaluated with five flavonoids including myricetin, quercetin, luteolin, kaempferol and isorhamnetin. Main parameters, which affect extraction efficiencies, are carefully investigated and optimized. Comparative experiments between Sil-CBM-C30 and commercial C18 sorbents indicate that the extraction efficiencies of the former one surpass the latter one. The modification of carbamate-embedded triacontyl group on surface of silica causes analytes extracted by hydrophobic, hydrogen bonding and π-π interactions. Under optimal conditions, good linearities and satisfied LODs and LOQs are achieved. The SPE-HPLC-DAD method is successfully developed and applied for the honey sample analysis. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. Application of dissolvable layered double hydroxides as sorbent in dispersive solid-phase extraction and extraction by co-precipitation for the determination of aromatic acid anions.

    Science.gov (United States)

    Tang, Sheng; Lee, Hian Kee

    2013-08-06

    Three types of magnesium-aluminum layered double hydroxides were synthesized and employed as solid-phase extraction (SPE) sorbents to extract several aromatic acids (protocatechuic acid, mandelic acid, phthalic acid, benzoic acid, and salicylic acid) from aqueous samples. An interesting feature of these sorbents is that they dissolve when the pH of the solution is lower than 4. Thus, the analyte elution step, as needed in conventional sorbent-based extraction, was obviated by dissolving the sorbent in acid after extraction and separation from the sample solution. The extract was then directly injected into a high-performance liquid chromatography-ultraviolet detection system for analysis. In the key adsorption process, both dispersive SPE and co-precipitation extraction with the sorbents were conducted and experimental parameters such as pH, temperature, and extraction time were optimized. The results showed that both extraction methods provided low limits of detection (0.03-1.47 μg/L) and good linearity (r(2) > 0.9903). The optimized extraction conditions were applied to human urine and sports drink samples. This new and interesting extraction approach was demonstrated to be a fast and efficient procedure for the extraction of organic anions from aqueous samples.

  14. Extractive fixed-site polymer sorbent for selective boron removal from natural water.

    Science.gov (United States)

    Thakur, Neha; Kumar, Sanjukta A; Shinde, Rakesh N; Pandey, Ashok K; Kumar, Sangita D; Reddy, A V R

    2013-09-15

    Water contamination by boron is a widespread environmental problem. The World Health Organization (WHO) recommends maximum boron concentration of 2.4 mg L(-1) for drinking water. The paper presents a simple method for preparation of functionalized sheet sorbent for selective extraction of boron from natural water. The pores of commercially available poly(propylene) membrane were functionalized by room temperature in situ crosslinking of poly(vinylbenzyl chloride) with a cyclic diamine piperazine. The precursor membranes were chemically modified with N-methyl D-glucamine which is selective for boron. Characterization of membrane was carried out using scanning electron microscopy (SEM) and attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR) techniques. The functionalized membrane has been characterized in terms of parameters that influence the sorption of boron from aqueous streams like pH, uptake capacity, contact time, effects of competing ions and reusability. The maximum boron sorption capacity determined experimentally was 28 mg g(-1). The studies showed that trace concentrations of boron were quantitatively removed from water at neutral pH. The developed fixed site polymer sorbent exhibited high sorption capacity and fast kinetics as compared to various sorbents reported in literature. It was successfully applied for the removal of boron from ground water and seawater samples in presence of high concentration of interfering ions.

  15. Facile fabrication of reduced graphene oxide-encapsulated silica: a sorbent for solid-phase extraction.

    Science.gov (United States)

    Luo, Yan-Bo; Zhu, Gang-Tian; Li, Xiao-Shui; Yuan, Bi-Feng; Feng, Yu-Qi

    2013-07-19

    In this study, a facile hydrothermal reduction strategy was developed for the preparation of reduced graphene oxide-encapsulated silica (SiO2@rGO). Compared with other conventional methods for the synthesis of SiO2@rGO, the proposed strategy endowed the obtained SiO2@rGO with larger amount of immobilized rGO. The prepared functionalized silica shows remarkable adsorption capacity toward chlorophenols (CPs) and peptides. When it was used as solid-phase extraction (SPE) sorbent, a superior recovery could be obtained compared to commercial sorbents, such as C18 silica, graphitized carbon black and carbon nanotubes. Based on these, the prepared material was used as SPE sorbent for the enrichment of CPs, and a method for the analysis of CPs in water samples was established by coupling SPE with high performance liquid chromatography-ultra violet detection (SPE-HPLC/UV). In addition, the obtained SiO2@rGO was further successfully extended to the enrichment of peptides in bovine serum albumin (BSA) digests.

  16. On-line high speed lipid extraction for nanoflow liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Lee, Ju Yong; Yang, Joon Seon; Park, Se Mi; Byeon, Seul Kee; Moon, Myeong Hee

    2016-09-16

    An on-line lipid extraction method is introduced by utilizing a short capillary extraction column using HILIC and C4 particles prior to nanoflow liquid chromatography-tandem mass spectrometry (nLC-MS/MS). The on-line extraction using a urine sample spiked with PL standards showed similar or slightly higher recovery values (86%-96%) of phospholipids (PLs) compared to those obtained by the conventional off-line extraction based on the Folch method with or without using the air-exposed drying process. In this study, we demonstrated that PL oxidation can occur during the air-exposed drying process of lipid extracts in standard liquid-liquid extraction procedures, which was confirmed by the oxidized PL (OxPL) molecules that were generated from an off-line extraction using a few PL standards. Quantitative comparison of these OxPL species between on- and off-line extraction followed by nLC-MS/MS with multiple reaction monitoring (MRM) analysis showed a significant decrease (2-10 fold) in unwanted OxPL species when on-line extraction was employed. While the number of identified PLs from a urine sample was somewhat lower than those by off-line extraction, the number of OxPLs was significantly reduced (from 70 to 22) with on-line extraction. The new method offers high speed (∼5min) automated extraction of PLs with nLC-MS/MS analysis and presents the possibility of handling a biological sample with a very limited amount of lipids.

  17. Novel D2EHPA-polysiloxane-based sorbent for titanium (IV) extraction and separation

    Energy Technology Data Exchange (ETDEWEB)

    Mendoza R, L. G.; Rodriguez de San Miguel, E.; Pardo G, D. Y.; De Gyves, J. [UNAM, Facultad de Quimica, Departamento de Quimica Analitica, Ciudad Universitaria, 04510 Mexico D. F. (Mexico); Sanchez G, J. P., E-mail: degyves@unam.mx [Instituto Mexicano del Petroleo, Laboratorio de Evaluacion Molecular, Eje Central Norte Lazaro Cardenas No. 152, Apdo. Postal 14-805, 07730 Mexico D. F. (Mexico)

    2011-07-01

    In this work the synthesis, characterization and evaluation of a novel sorbent material used for the solid-phase extraction of titanium (IV) from hydrochloric acid medium is described. The material was prepared by the sol-gel route incorporating bis(2-ethylhexyl phosporic acid) (D2EHPA) as extractant within a polymeric matrix based on polysiloxanes and characterized through Ftir-Atr, XRD, {sup 29}Si and {sup 31}P NMR, TGA and DSC. In studies of titanium sorption and desorption in batch mode several factors related with the extraction and back-extraction operations were evaluated, such as: contact time, titanium concentration, nature and composition of the aqueous media, and extractant concentration in the sorbent. The maximum sorption was observed at 30 min of contact time in a 1 mol L{sup -1} HCl + 0.1% KCl medium, while the maximum desorption was observed at 60 min in a 1.5 mol L{sup -1} H{sub 2}SO{sub 4} + 20% v/v H{sub 2}O{sub 2} medium when titanium concentration was 70 mg L{sup -1}. Under optimal conditions the recovered percent of titanium was nearly 90%. In addition, the characterization of the extraction equilibrium was performed. The selectivity of the method was studied adding Al(III), Fe(III) and V(v) to the extraction medium. A high selectivity for Ti over Al and Fe was observed, even at high concentrations of the interferences; 50% of Ti, only 7% of Fe, 3% of Al and less than 1% of V were recovered under the established conditions. The method was finally applied for titanium recovery from a certified fly ash sample generated from a municipal incineration plant. (Author)

  18. On-line coupling of supercritical fluid extraction and chromatographic techniques.

    Science.gov (United States)

    Sánchez-Camargo, Andrea Del Pilar; Parada-Alfonso, Fabián; Ibáñez, Elena; Cifuentes, Alejandro

    2017-01-01

    This review summarizes and discusses recent advances and applications of on-line supercritical fluid extraction coupled to liquid chromatography, gas chromatography, and supercritical fluid chromatographic techniques. Supercritical fluids, due to their exceptional physical properties, provide unique opportunities not only during the extraction step but also in the separation process. Although supercritical fluid extraction is especially suitable for recovery of non-polar organic compounds, this technique can also be successfully applied to the extraction of polar analytes by the aid of modifiers. Supercritical fluid extraction process can be performed following "off-line" or "on-line" approaches and their main features are contrasted herein. Besides, the parameters affecting the supercritical fluid extraction process are explained and a "decision tree" is for the first time presented in this review work as a guide tool for method development. The general principles (instrumental and methodological) of the different on-line couplings of supercritical fluid extraction with chromatographic techniques are described. Advantages and shortcomings of supercritical fluid extraction as hyphenated technique are discussed. Besides, an update of the most recent applications (from 2005 up to now) of the mentioned couplings is also presented in this review.

  19. 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.

  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. Development of a selective solid phase extraction method for nitro musk compounds in environmental waters using a molecularly imprinted sorbent.

    Science.gov (United States)

    Lopez-Nogueroles, Marina; Lordel-Madeleine, Sonia; Chisvert, Alberto; Salvador, Amparo; Pichon, Valérie

    2013-06-15

    A powerful analytical method for the determination of the family of the nitro musk compounds at trace level in environmental waters-river, sea, and water from a treatment plant-is presented. The method is based on the use of molecularly imprinted silica (MIS) as sorbent for solid phase extraction (SPE) used for the clean-up and the concentration step of the target analytes previous to their determination by gas chromatography-mass spectrometry. The optimized extraction procedure allowed extraction recoveries between 61% and 87% using the MIS. The comparison with a non-imprinted silica (NIS) sorbent, for which extraction recoveries between 8% and 26% were obtained, showed the high selectivity of the MIS for the nitro musks. Moreover, high enrichment factors, ranging between 580 and 827, were achieved. The imprinted sorbent was compared to a conventional polymeric SPE sorbent for the extraction of the target compounds from environmental waters, showing high selectivity of the MIS and its clean-up potential. For the first time, the five nitro musk compounds were selectively extracted with an imprinted material.

  2. Surface modified magnetic Fe{sub 3}O{sub 4} nanoparticles as a selective sorbent for solid phase extraction of uranyl ions from water samples

    Energy Technology Data Exchange (ETDEWEB)

    Sadeghi, Susan, E-mail: ssadeghi@birjand.ac.ir [Department of Chemistry, Faculty of Science, University of Birjand, P.O. Box. 97175/615, Birjand (Iran, Islamic Republic of); Azhdari, Hoda [Department of Chemistry, Faculty of Science, University of Birjand, P.O. Box. 97175/615, Birjand (Iran, Islamic Republic of); Arabi, Hadi [Magnetism and Superconducting Research Lab, Department of Physics, Faculty of Science, University of Birjand, P.O. Box. 97175/615, Birjand (Iran, Islamic Republic of); Moghaddam, Ali Zeraatkar [Department of Chemistry, Faculty of Science, University of Birjand, P.O. Box. 97175/615, Birjand (Iran, Islamic Republic of)

    2012-05-15

    Highlights: Black-Right-Pointing-Pointer A new sorbent based on functionalized magnetite nanoparticles with quercetin is reported. Black-Right-Pointing-Pointer The quercetin based magnetic nanoparticles could be used as a sorbent to remove toxic uranyl ions from water samples. Black-Right-Pointing-Pointer The sorbent provides a rapidly and easy separation of uranyl ions only by using a permanent magnet. Black-Right-Pointing-Pointer This technique is considered more efficient separation compared to conventional filtering or centrifuging methods for the removing of the sorbent. - Abstract: In this study, silica-coated magnetic nanoparticles modified with quercetin were synthesized by a sol-gel method. These magnetic nanoparticles were assessed as a new solid phase sorbent for extraction of uranyl ions from aqueous solutions. The crystal and chemical structures and magnetic property of the new sorbent were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectrophotometer (FT-IR), and vibration sample magnetometer (VSM). The experimental parameters affecting the extraction efficiency of uranyl ions from aqueous solutions using the synthesized sorbent were optimized by means of the response surface methodology. The adsorption equilibrium of uranyl ions onto the sorbent was explained by Langmuir isotherm and maximum monolayer adsorption capacity was found 12.33 mg/g. The synthesized sorbent was applied to extraction of uranyl ions from different water samples.

  3. Insight into the extraction mechanism of polymeric ionic liquid sorbent coatings in solid-phase microextraction.

    Science.gov (United States)

    Ho, Tien D; Cole, William T S; Augusto, Fabio; Anderson, Jared L

    2013-07-12

    An investigation into the mechanism of extraction for polymeric ionic liquid (PIL)-based solid phase microextraction sorbent coatings is described. Four PIL-based coatings, namely, a poly(1-4-vinylbenzyl)-3-hexadecylimidazolium bis[(trifluoromethyl)sulfonyl] imide (poly([VBHDIM][NTf2])) PIL produced through 2,2'-azo-bis(isobutyronitrile) (AIBN) initiated free-radical polymerization, a UV-initiated poly(1-vinyl-3-hexylimidazolium) chloride (poly([VHIM][Cl])) PIL, and two crosslinked PILs containing the same IL monomers copolymerized with dicationic IL crosslinkers, were investigated. Calibration curves of 1-octanol were plotted in the presence of naphthalene, a model interfering compound, to observe changes in the linear range, sensitivity, and amount of analytes extracted. Results were compared with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) coating and a polyacrylate (PA) coating which are known to extract analytes primarily through adsorption and partitioning mechanisms, respectively. All PIL-based coatings extracted analytes via a non-competitive partitioning mechanism regardless of the extent of crosslinking.

  4. Electromembrane extraction of tartrazine from food samples: Effects of nano-sorbents on membrane performance.

    Science.gov (United States)

    Yaripour, Saeid; Mohammadi, Ali; Nojavan, Saeed

    2016-07-01

    In the present study, for the first time electromembrane extraction followed by high-performance liquid chromatography coupled with ultraviolet detection was developed and validated for the determination of tartrazine in some food samples. The parameters influencing electromembrane extraction were evaluated and optimized. The membrane consists of 1-octanol immobilized in the pores of a hollow fiber. As a driving force, a 30 V electrical field was applied to make the analyte migrate from sample solution with pH 3, through the supported liquid membrane into an acceptor solution with pH 10. Best preconcentration (enrichment factor >21) was obtained in extraction duration of 15 min. Effects of some solid nano-sorbents like carbon nanotubes and molecularly imprinted polymers on membrane performance and electromembrane extraction efficiency were evaluated. The method provided the linearity in the range 25-1000 ng/mL for tartrazine (R(2) > 0.9996) with repeatability range (RSD) between 3.8 and 8.5% (n = 3). The limits of detection and quantitation were 7.5 and 25 ng/mL, respectively. Finally, the method was applied to the determination and quantification of tartrazine from some food samples with relative recoveries in the range between 90 and 98%.

  5. On-line immunoaffinity solid-phase extraction capillary electrophoresis mass spectrometry for the analysis of large biomolecules: a preliminary report.

    Science.gov (United States)

    Medina-Casanellas, Silvia; Benavente, Fernando; Giménez, Estela; Barbosa, José; Sanz-Nebot, Victoria

    2014-08-01

    The analysis of large biomolecules by on-line immunoaffinity solid-phase extraction capillary electrophoresis mass spectrometry (IA-SPE-CE-MS) remains unexplored because of the complex issues that need to be addressed. In this preliminary study, we used the human glycoprotein transferrin (Tf) as a model of a large biomolecule. First, we established by CE-UV a novel method compatible with IA-SPE-CE-MS, based on the use of a fused silica capillary coated with an anionic derivative of polyacrylamide (UltraTrol(TM) Dynamic Pre-Coat High Normal, HN) to prevent protein adsorption. The methodology allowed the detection of the most abundant Tf sialoforms. Repeatability studies demonstrated high stability of the coated capillaries, which was required for on-line immunoextraction and MS detection. IA-SPE-CE-UV and IA-SPE-CE-MS methods were optimized for the analysis of Tf standards and human serum samples using a laboratory-made IA sorbent. Three peaks corresponding to Tf were detected with UV detection when on-line immunoextraction was applied to the standards. The use of MS detection, however, reduced the resolution of the electrophoretic separation. Finally, we demonstrated that it was possible to detect Tf in human serum samples, after off-line serum sample de-salting by centrifugal filtration.

  6. Sol-gel methyl coating in capillary microextraction hyphenated on-line with high-performance liquid chromatography Counterintuitive extraction behavior for polar analytes.

    Science.gov (United States)

    Segro, Scott S; Malik, Abdul

    2008-07-18

    A sol-gel coating with anchored methyl groups was developed for capillary microextraction hyphenated on-line with high-performance liquid chromatography (HPLC). This was accomplished by using methyltrimethoxysilane as the sol-gel precursor. The methyl group on the sol-gel precursor ultimately turned into a pendant group on the created sol-gel coating and was primarily responsible for the extraction of nonpolar analytes. A 40-cm segment of 0.25mm I.D. fused silica capillary containing the sol-gel methyl coating on the inner surface was installed as a sampling loop in an HPLC injection port. The analytes were extracted by the coating when an aqueous sample containing the analytes was passed through this capillary. The extracted analytes were then transferred to the HPLC column using isocratic elution with an acetonitrile/water mobile phase. This capillary demonstrated excellent extraction capability for polycyclic aromatic hydrocarbons and ketones. Unexpectedly, this coating also provided good extraction for polar analytes, including aromatic phenols, alcohols, and amines. Considering the fact that the methyl group is nonpolar in nature, such an extraction behavior of sol-gel methyl coating toward polar analytes is counterintuitive. Thus, sol-gel sorbents with short alkyl side chains have the potential to offer a polymer-free alternative to traditional sol-gel capillary microextraction (CME) media commonly prepared with the use of polymers in the sol solution. Elimination of polymers from the sol-gel coating solution is conducive to improving thermal stability and solvent tolerance of the created sol-gel extracting phase. This also makes the preparation of sol-gel coatings facile and cost-effective. Possessing excellent solvent stability, such sol-gel coatings offer the opportunity for effective on-line hyphenation of capillary microextraction with HPLC and other liquid-phase separation techniques that employ organo-aqueous mobile phases.

  7. New extraction sorbent based on aptamers for the determination of ochratoxin A in red wine.

    Science.gov (United States)

    Chapuis-Hugon, Florence; du Boisbaudry, Aude; Madru, Benjamin; Pichon, Valérie

    2011-05-01

    A new solid phase extraction method based on aptamers, an oligosorbent, was developed and applied to the determination of ochratoxin A (OTA) from red wine. Two solid supports were chosen to immobilize OTA aptamer by covalent binding (cyanogen bromide-activated sepharose) or noncovalent binding (streptavidin-activated agarose). The resulting oligosorbents were evaluated in terms of retention, selectivity, and capacity. To assess the selectivity of the resulting oligosorbents, control supports made only of a solid support without immobilized aptamers were simultaneously studied. After optimization of the selective extraction procedure, extraction recoveries close to 100% were obtained on both materials. No retention was observed on the control supports. A similar capacity was also found for both oligosorbents. However, the immobilization by covalent bonding appeared more robust for the determination of OTA in the wine. A conventional sorbent and an immunoaffinity column were also applied to the determination of OTA in red wine to compare the potential of the various approaches for the treatment of such complex samples.

  8. Polyaniline/Graphene Nanocomposite as a Promising Sorbent for Dispersive Solid Phase Extraction of Avermectins from Citrus Fruit Juice

    Directory of Open Access Journals (Sweden)

    Faezeh Khalilian

    2017-06-01

    Full Text Available A solid phase extraction sorbent based on polyaniline/graphene nanocomposite is presented. The structure and morphology of synthesized nanocomposite were investigated by Fourier transform infrared spectroscopy, field emission scanning electron microscopy, X-ray diffraction and thermal gravimetric analysis. The dispersive solid phase extraction was employed to the isolation and preconcentration of avermectins insecticide (mixture of B1a and B1b. The extraction procedure was investigated by high performance liquid chromatography-UV detection. The sorbent demonstrated a favorable analytical performance for avermectins detection with reasonable linear ranges (1.5-1000 μg L-1 and 5.0-1000 μg L-1 for B1a and B1b in order and acceptable detection limits (0.5 μg L-1 for B1a and 2.5 μg L-1 for B1b under optimized conditions. The extraction efficiency of polyaniline/graphene nanocomposite in the extraction of avermectins was compared with graphene, polyaniline, carbon nanotube and C18 sorbents. Moreover, the applicability of proposed method was assessed for the extraction of analyte from citrus fruit juice.

  9. Spectrophotometric detection of arsenic using flow-injection hydride generation following sorbent extraction preconcentration.

    Science.gov (United States)

    Neto, J A; Montes, R; Cardoso, A A

    1999-12-06

    An automated system with a C(18) bonded silica gel packed minicolumn is proposed for spectrophotometric detection of arsenic using flow-injection hydride generation following sorbent extraction preconcentration. Complexes formed between arsenic(III) and ammonium diethyl dithiophosphate (ADDP) are retained on a C(18) sorbent. The eluted As-DDP complexes are merged with a 1.5% (w/v) NaBH(4) and the resulting solution is thereafter injected into the hydride generator/gas-liquid separator. The arsine generated is carried out by a stream of N(2) and trapped in an alkaline iodine solution in which the analyte is determined by the arsenomolybdenum blue method. With preconcentration time of 120 s, calibration in the 5.00-50.0 mug As l(-1) range and sampling rate of about 20 samples h(-1) are achieved, corresponding to 36 mg ADDP plus 36 mg ammonium heptamolybdate plus 7 mg hydrazine sulfate plus 0.7 mg stannous chloride and about 7 ml sample consumed per determination. The detection limit is 0.06 mug l(-1) and the relative standard deviation (n=12) for a typical 17.0 mug As l(-1) sample is ca. 6%. The accuracy was checked for arsenic determination in plant materials from the NIST (1572 citrus leaves; 1573 tomato leaves) and the results were in agreement with the certified values at 95% confidence level. Good recoveries (94-104%) of spiked tap waters, sugars and synthetic mixtures of trivalent and pentavalent arsenic were also found.

  10. Determination of Hg(II) in waters by on-line preconcentration using Cyanex 923 as a sorbent — Cold vapor atomic absorption spectrometry

    Science.gov (United States)

    Duan, Taicheng; Song, Xuejie; Xu, Jingwei; Guo, Pengran; Chen, Hangting; Li, Hongfei

    2006-09-01

    Using a solid phase extraction mini-column home-made from a neutral extractant Cyanex 923, inorganic Hg could be on-line preconcentrated and simultaneously separated from methyl mercury. The preconcentrated Hg (II) was then eluted with 10% HNO 3 and subsequently reduced by NaBH 4 to form Hg vapor before determination by cold vapor atomic absorption spectrometry (CVAAS). Optimal conditions for and interferences on the Hg preconcentration and measurement were at 1% HCl, for a 25 mL sample uptake volume and a 10 mL min - 1 sample loading rate. The detection limit was 0.2 ng L - 1 and much lower than that of conventional method (around 15.8 ng L - 1 ). The relative standard deviation (RSD) is 1.8% for measurements of 40 ng L - 1 of Hg and the linear working curve is from 20 to 2000 ng L - 1 (with a correlation coefficient of 0.9996). The method was applied in determination of inorganic Hg in city lake and deep well water (from Changchun, Jilin, China), and recovery test results for both samples were satisfactory.

  11. Determination of Hg(II) in waters by on-line preconcentration using Cyanex 923 as a sorbent - Cold vapor atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Duan Taicheng [State Key Laboratory of Electroanalytical Chemistry, National Research Center of Electroanalytical and Spectroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Song Xuejie [State Key Laboratory of Electroanalytical Chemistry, National Research Center of Electroanalytical and Spectroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Xu Jingwei [State Key Laboratory of Electroanalytical Chemistry, National Research Center of Electroanalytical and Spectroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Guo Pengran [State Key Laboratory of Electroanalytical Chemistry, National Research Center of Electroanalytical and Spectroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Chen Hangting [State Key Laboratory of Electroanalytical Chemistry, National Research Center of Electroanalytical and Spectroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China)]. E-mail: htchen@ciac.jl.cn; Li Hongfei [Laboratory of Rare Earth Chemistry and Physics, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China)

    2006-09-15

    Using a solid phase extraction mini-column home-made from a neutral extractant Cyanex 923, inorganic Hg could be on-line preconcentrated and simultaneously separated from methyl mercury. The preconcentrated Hg (II) was then eluted with 10% HNO{sub 3} and subsequently reduced by NaBH{sub 4} to form Hg vapor before determination by cold vapor atomic absorption spectrometry (CVAAS). Optimal conditions for and interferences on the Hg preconcentration and measurement were at 1% HCl, for a 25 mL sample uptake volume and a 10 mL min{sup -1} sample loading rate. The detection limit was 0.2 ng L{sup -1} and much lower than that of conventional method (around 15.8 ng L{sup -1}). The relative standard deviation (RSD) is 1.8% for measurements of 40 ng L{sup -1} of Hg and the linear working curve is from 20 to 2000 ng L{sup -1} (with a correlation coefficient of 0.9996). The method was applied in determination of inorganic Hg in city lake and deep well water (from Changchun, Jilin, China), and recovery test results for both samples were satisfactory.

  12. Rubidium extraction using an organic polymer encapsulated potassium copper hexacyanoferrate sorbent

    KAUST Repository

    Naidu, Gayathri

    2016-07-11

    Sea water reverse osmosis (SWRO) brine contains significant quantity of Rb. As an economically valuable metal, extracting Rb using a suitable and selective extraction method would be beneficial. An inorganic sorbent, copper based potassium hexacyanoferrate (KCuFC), exhibited high selectivity to extract Rb compared to potassium hexacyanoferrate consisting of other transition metal combinations such as Ni, Co and Fe. An organic polymer (polyacrylonitrile, PAN) encapsulated KCuFC (KCuFC-PAN) achieved a Langmuir maximum Rb sorption capacity of 1.23 mmol/g at pH 7.0 ± 0.5. KCuFC-PAN showed Rb selectivity over a wide concentration range of co-existing ions and salinity of SWRO brine. High salinity (0.5-2.5 M NaCl) resulted in 12-30% sorption capacity reduction. At a molar ratio of Li:Rb (21:1), Cs:Rb (0.001:1) and Ca:Rb (14,700:1) commonly found in SWRO brine, sorption reduction of only 18% occurred. Nevertheless, at a very high K:Rb molar ratio (7700:1), KCuFC-PAN sorption capacity of Rb reduced significantly by 65-70%. KCuFC-PAN was well suited for column operation. In a fixed-bed KCuFC-PAN column (influent concentration 0.06 mmol Rb/L, flow velocity 2 m/h), two sorption/desorption cycles were successfully achieved with a maximum Rb sorption capacity of 1.01 (closely similar to the batch study) and 0.85 mmol/g in the first and second cycles, respectively. Around 95% of Rb was desorbed from the column with 0.2 M KCl. Resorcinol formaldehyde (RF) resin showed promising results of separating Rb from K/Rb mixed solution in effluents from a fixed-bed column, and a subsequent sequential acid desorption, producing 68% purified Rb.

  13. Integrating Multiple On-line Knowledge Bases for Disease-Lab Test Relation Extraction

    Science.gov (United States)

    Zhang, Yaoyun; Soysal, Ergin; Moon, Sungrim; Wang, Jingqi; Tao, Cui; Xu, Hua

    2015-01-01

    A computable knowledge base containing relations between diseases and lab tests would be a great resource for many biomedical informatics applications. This paper describes our initial step towards establishing a comprehensive knowledge base of disease and lab tests relations utilizing three public on-line resources. LabTestsOnline, MedlinePlus and Wikipedia are integrated to create a freely available, computable disease-lab test knowledgebase. Disease and lab test concepts are identified using MetaMap and relations between diseases and lab tests are determined based on source-specific rules. Experimental results demonstrate a high precision for relation extraction, with Wikipedia achieving the highest precision of 87%. Combining the three sources reached a recall of 51.40%, when compared with a subset of disease-lab test relations extracted from a reference book. Moreover, we found additional disease-lab test relations from on-line resources, indicating they are complementary to existing reference books for building a comprehensive disease and lab test relation knowledge base. PMID:26306271

  14. Preparation of an aminopropyl imidazole-modified silica gel as a sorbent for solid-phase extraction of carboxylic acid compounds and polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Wang, Na; Guo, Yong; Wang, Licheng; Liang, Xiaojing; Liu, Shujuan; Jiang, Shengxiang

    2014-05-21

    In this paper, a kind of aminopropyl imidazole-modified silica sorbent was synthesized and used as a solid-phase extraction (SPE) sorbent for the determination of carboxylic acid compounds and polycyclic aromatic hydrocarbons (PAHs). The resultant aminopropyl imidazole-modified silica sorbent was characterized by Fourier transform infrared spectroscopy (FT-IR) and elemental analysis (EA) to ensure the successful binding of aminopropyl imidazole on the surface of silica gel. Then the aminopropyl imidazole-modified silica sorbent served as a SPE sorbent for the enrichment of carboxylic acid compounds and PAHs. The new sorbent exhibited high extraction efficiency towards the tested compounds and the results show that such a sorbent can offer multiple intermolecular interactions: electrostatic, π-π, and hydrophobic interactions. Several parameters affecting the extraction recovery, such as the pH of sample solution, the pH of eluent, the solubility of eluent, the volume of eluent, and sample loading, were also investigated. Under the optimized conditions, the proposed method was applied to the analysis of four carboxylic acid compounds and four PAHs in environmental water samples. Good linearities were obtained for all the tested compounds with R(2) larger than 0.9903. The limits of detection were found to be in the range of 0.0065-0.5 μg L(-1). The recovery values of spiked river water samples were from 63.2% to 112.3% with relative standard deviations (RSDs) less than 10.1% (n = 4).

  15. Metal-organic framework templated inorganic sorbents for rapid and efficient extraction of heavy metals.

    Science.gov (United States)

    Abney, C W; Gilhula, J C; Lu, K; Lin, W

    2014-12-17

    An innovative wet-treatment with Na2 S transforms two indium metal-organic frameworks (MOFs) into a series of porous inorganic sorbents. These MOF-templated materials display remarkable affinity for heavy metals with saturation occurring in less than 1 h. The saturation capacity for Hg(II) exceeds 2 g g(-1) , more than doubling the best thiol-functionalized sorbents in the literature.

  16. Ampholine-functionalized hybrid organic-inorganic silica material as sorbent for solid-phase extraction of acidic and basic compounds.

    Science.gov (United States)

    Wang, Tingting; Chen, Yihui; Ma, Junfeng; Chen, Mingliang; Nie, Chenggang; Hu, Minjie; Li, Ying; Jia, Zhijian; Fang, Jianghua; Gao, Haoqi

    2013-09-20

    A novel sorbent for solid-phase extraction (SPE) was synthesized by chemical immobilization of ampholine on hybrid organic-inorganic silica material. The ampholine-functionalized hybrid organic-inorganic silica sorbent is consisted of aliphatic amine groups, carboxyl groups and long carbon chains, allowing for extraction of both acidic and basic compounds. The retention properties of the developed sorbent were evaluated for 1-hydroxy-2-naphthoic acid (HNA), 1-naphthoic acid (NA), 3-hydroxybenzoic acid (HBA), benzoic acid (BA), sorbic acid (SA), vanillic aldehyde (VA), butyl 4-hydroxybenzoate (BHB), propyl 4-hydroxybenzoate (PHB), ethyl 4-hydroxybenzoate (EHB), and methyl 4-hydroxybenzoate (MHB). The results show that such a sorbent has three types of interaction, i.e., electrostatic interaction, hydrophobic interaction, and hydrogen bonding, exhibiting high extraction efficiency towards the compounds tested. The adsorption capacities of the analytes ranged from 0.61 to 6.54μgmg(-1). The reproducibility of the sorbent preparation was evaluated at three spiking concentration levels, with relative standard deviations (RSDs) of 1.0-10.5%. The recoveries of ten acidic and basic compounds spiked in beverage Coca-Cola(®) sample ranged from 82.5% to 98.2% with RSDs less than 5.8%. Under optimum conditions, the ampholine-functionalized hybrid organic-inorganic silica sorbent rendered higher extraction efficiency for acidic compounds than that of the commercially available ampholine-functionalized silica particles, and was comparable to that of the commercial Oasis WAX and Oasis WCX.

  17. Magnetic nanocomposite of self-doped polyaniline-graphene as a novel sorbent for solid-phase extraction.

    Science.gov (United States)

    Mehdinia, Ali; Esfandiarnejad, Reyhaneh; Jabbari, Ali

    2015-01-01

    This work is the first study on the extraction efficiency of self-doped polyaniline that is immobilized on the graphene-modified magnetic nanoparticles. The new material was used as a sorbent for the magnetic solid-phase extraction of methyl-, propyl-, and butylparabens. The use of graphene provides a high surface area and prevents aggregation of the nanoparticles. The self-doped polyaniline also provides multifunctionality, high extraction capacity, and chemical stability even in the basic medium. The parabens were acetylated for determination by gas chromatography with flame ionization detection. The effects of monomer ratio, extraction solvent, sorbent amount, sample volume, desorption solvent volume, adsorption and desorption times, and sample ionic strength were optimized. Preconcentration factors obtained were from 190 to 310. The detection limits of the method were <2.8 μg/L. Linear ranges of the method were 5-2000 μg/L for propyl and butyl parabens, and 10-2000 μg/L for methyl paraben. The method was applied for the determination of the parabens in cosmetic products and extraction recoveries were 89-101% with RSDs ≤7.9%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. On-line anion exchange solid-phase extraction coupled to liquid chromatography with fluorescence detection to determine quinolones in water and human urine.

    Science.gov (United States)

    Lara, Francisco J; Del Olmo-Iruela, Monsalud; García-Campaña, Ana M

    2013-10-04

    An analytical method based on on-line solid-phase extraction coupled to liquid chromatography with fluorescence detection has been developed to determine quinolones in tap water and human urine. A home-made setup was used to percolate 10 mL of sample through a solid-phase extraction column. Analytes were retained onto the sorbent by an anion exchange mechanism which ensures an optimum compatibility with the subsequent chromatographic separation. A C-18 column containing core-shell particles (2.6 μm) was used to achieve peak efficiencies up to 200,000 plates/m, at a flow rate of 1.2 mL/min and without the need for special pumps. The method allowed the determination of 11 quinolones directly in tap water samples in less than 20 min and with limits of detection ranging between 7 and 110 ng/L. The sensitivity achieved made possible the direct determination of 9 quinolones in human urine without any sample treatment, just dilution with water. Relative recoveries between 94 and 109% were obtained meaning that the matrix effect in human urine is negligible after dilution. Satisfactory results were also obtained in terms of precision since relative standard deviations were always below 13%.

  19. Matrix molecularly imprinted mesoporous sol-gel sorbent for efficient solid-phase extraction of chloramphenicol from milk.

    Science.gov (United States)

    Samanidou, Victoria; Kehagia, Maria; Kabir, Abuzar; Furton, Kenneth G

    2016-03-31

    Highly selective and efficient chloramphenicol imprinted sol-gel silica based inorganic polymeric sorbent (sol-gel MIP) was synthesized via matrix imprinting approach for the extraction of chloramphenicol in milk. Chloramphenicol was used as the template molecule, 3-aminopropyltriethoxysilane (3-APTES) and triethoxyphenylsilane (TEPS) as the functional precursors, tetramethyl orthosilicate (TMOS) as the cross-linker, isopropanol as the solvent/porogen, and HCl as the sol-gel catalyst. Non-imprinted sol-gel polymer (sol-gel NIP) was synthesized under identical conditions in absence of template molecules for comparison purpose. Both synthesized materials were characterized by Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FT-IR) and nitrogen adsorption porosimetry, which unambiguously confirmed their significant structural and morphological differences. The synthesized MIP and NIP materials were evaluated as sorbents for molecularly imprinted solid phase extraction (MISPE) of chloramphenicol in milk. The effect of critical extraction parameters (flow rate, elution solvent, sample and eluent volume, selectivity coefficient, retention capacity) was studied in terms of retention and desorption of chloramphenicol. Competition and cross reactivity tests have proved that sol-gel MIP sorbent possesses significantly higher specific retention and enrichment capacity for chloramphenicol compared to its non-imprinted analogue. The maximum imprinting factor (IF) was found as 9.7, whereas the highest adsorption capacity of chloramphenicol by sol-gel MIP was 23 mg/g. The sol-gel MIP was found to be adequately selective towards chloramphenicol to provide the necessary minimum required performance limit (MRPL) of 0.3 μg/kg set forth by European Commission after analysis by LC-MS even without requiring time consuming solvent evaporation and sample reconstitution step, often considered as an integral part in solid phase extraction work-flow. Intra and

  20. Micro-solid-phase extraction of organochlorine pesticides using porous metal-organic framework MIL-101 as sorbent.

    Science.gov (United States)

    Huang, Zhenzhen; Lee, Hian Kee

    2015-07-03

    In this study, a metal-organic framework material, MIL-101, used as a micro-solid-phase extraction (μ-SPE) sorbent for efficient enrichment of five organochlorine pesticides (OCPs), including α-HCH, Aldrin, α-Chlordane, Dieldrin and p,p'-DDD from water samples, followed by gas chromatography-mass spectrometry, is reported. This study demonstrated a new application of MIL-101 using μ-SPE, an advantage of the latter being its ability to process complex aqueous matrices, due to the protection of the sorbent afforded by the hollow fiber membrane bag. Key factors affecting extraction efficiency were studied, including elution solvent, extraction and desorption time. Under the optimal extraction conditions, the calibration plots were linear from 0.05 to 50 ng/mL for α-HCH and p,p'-DDD, and 0.1 to 50 ng/mL for the other three analytes. The limits of detection were between 0.0025 and 0.016 ng/mL. The relative recoveries of the OCPs spiked into real water samples (at 5 ng/mL of each analyte) ranged from 87.6 to 98.6% with relative standard deviations of <10%.

  1. Biochar as a sorbent for chlorinated hydrocarbons - sorption and extraction experiments in single and bi-solute systems

    Science.gov (United States)

    Schreiter, Inga J.; Wefer-Roehl, Annette; Graber, Ellen R.; Schüth, Christoph

    2017-04-01

    Biochar (BC) is increasingly deemed a potential sorbent for contaminants in soil and water remediation, and brownfield restoration. In this study, sorption and extraction experiments were performed to assess the potential of three different BCs to sorb and retain the chlorinated hydrocarbons trichloroethylene (TCE) and tetrachloroethylene (PCE). BCs studied were produced from wood chips, grain husk, and cattle manure at 450 °C. A commercially available activated carbon (AC) served as a reference. The sorption behaviour was studied in batch experiments in single solute and bi-solute systems. Resulting isotherms were fitted to the Freundlich model. To assess the desorption behaviour, a five-step extraction scheme (water at 40°C, water at 80°C, methanol at 50°C, toluene at 50°C, and n-hexane at 50°) was developed, utilizing Accelerated Solvent Extraction. Isotherms revealed distinct differences in sorption behaviour depending on BC feedstock. Sorption capacity ranked as follows: wood chip BC > grain husk BC > cattle manure BC for both contaminants. This sequence could be attributable to an increasing specific surface area, an increasing amount of carbon, and a decreasing ash content of the sorbents. It is noteworthy that all three BCs were more effective in adsorbing TCE, which is surprising, given the higher logKow of PCE. The reverse was observed for the AC. Here, sorption is purely driven by the hydrophobicity of the compound rather than sorbent properties. In bi-solute experiments, PCE sorbed as good as or stronger than TCE, yet the total mass of sorbed compounds increased slightly. In contrast, AC showed a significant decrease of TCE sorption and no significant changes in the total mass sorbed. Extraction experiments revealed that for all BCs a large fraction of the contaminants could not be readily desorbed. In all cases, water remobilized < 5 % of the total contaminant mass and up to 70 % could not be extracted by any of the solvents. The findings suggest

  2. Rotating disk sorbent extraction for pre-concentration of chromogenic organic compounds and direct determination by solid phase spectrophotometry.

    Science.gov (United States)

    Richter, Pablo; Cañas, Alejandro; Muñoz, Carlos; Leiva, Claudio; Ahumada, Inés

    2011-06-10

    A novel and very simple microextraction approach for pre-concentration and direct solid phase spectrophotometric measurement has been developed for the determination of chromogenic analytes. The model analyte to assess this approach was the chromophore malachite green (MG). The analyte was extracted from water samples onto a small rotating disk made of Teflon containing a sorbent phase of polydimethylsiloxane (PDMS) on one of its surfaces. We refer to the extraction procedure as rotating disk sorptive extraction (RDSE). After extraction, the sorbent phase with the concentrated analyte was separated from the Teflon disk and used directly for MG determination by solid phase spectrophotometry at 624 nm, without the necessity of a desorption step. Chemical and extraction variables such as concentration of sodium sulfate, pH, disk rotational velocity, extraction time, and temperature were studied in order to establish the best conditions for extraction. Under optimum conditions, the extraction of MG was carried out in 18 min and 90 min, for sample volumes of 100mL or 1000 mL, respectively. The detection limit, based on three times the standard deviation of the blank phase (3σ(b)), was 1.4 μg L⁻¹ and the repeatability, expressed as relative standard deviation (RSD), for 20 μg L⁻¹ MG was 8.1%. This study also applied the method to real samples, obtaining quantitative recovery (mean recovery of 99.3%). The PDMS phases could be reused after desorbing the MG into methanol for 3h. Replacement of the PDMS film onto the disk is very easy and low cost.

  3. Hybrid organic-inorganic silica monolith with hydrophobic/strong cation-exchange functional groups as a sorbent for micro-solid phase extraction.

    Science.gov (United States)

    Zheng, Ming-Ming; Ruan, Ge-Deng; Feng, Yu-Qi

    2009-11-06

    A hybrid organic-inorganic silica monolith with hydrophobic and strong cation-exchange functional groups was prepared and used as a sorbent for micro-solid phase extraction (micro-SPE). The hybrid silica monolith functionalized with octyl and thiol groups was conveniently synthesized by hydrolysis and polycondensation of a mixture of tetraethoxysilane (TEOS), n-octyltriethoxysilane (C8-TEOS) and 3-mercaptopropyltrimethoxysilane (MPTMS) via a two-step catalytic sol-gel process. Due to the favorable chemical reactivity of mercapto pendant moieties, the obtained hybrid monolith was oxidized using hydrogen peroxide (30%, w/w) to yield sulfonic acid groups, which provided strong cation-exchange sites. The obtained hybrid monolith was characterized by diffused infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. The results show that the resulting monolith contains much higher carbon (31.6%) and sulfur (4.8%) contents than traditionally bonded silica materials. The extraction performance of the hybrid monolith was evaluated using sulfonamides as testing analytes by micro-SPE on-line coupled to HPLC. The results show that the hybrid monolith with hydrophobic and strong cation-exchange functional groups exhibits high extraction efficiency towards the testing analytes. The column-to-column RSD values were 1.3-9.8% for the extraction of SAs investigated. The extraction performance of the hybrid silica monolith remained practically unchanged after treated with acid (pH 1.0) and basic solutions (pH 10.5). Finally, the application of the hybrid monolith was demonstrated by micro-SPE of sulfonamide residues from milk followed by HPLC-UV analysis. The limits of detection (S/N=3) for eight SAs were found to be 1.0-3.0ng/mL in milk. The recoveries of eight SAs spiked in milk sample ranged from 80.2% to 115.6%, with relative standard deviations less than 11.8%.

  4. Graphene oxide as a micro-solid-phase extraction sorbent for the enrichment of parabens from water and vinegar samples.

    Science.gov (United States)

    Wang, Lu; Zang, Xiaohuan; Wang, Chun; Wang, Zhi

    2014-07-01

    A simple hydrophilic polyamide organic membrane protected micro-solid-phase extraction method with graphene oxide as the sorbent was developed for the enrichment of some parabens from water and vinegar samples prior to gas chromatography with mass spectrometry detection. The main experimental parameters affecting the extraction efficiencies, such as the type and amount of the sorbent, extraction time, stirring rate, salt addition, sample solution pH and desorption conditions, were investigated. Under the optimized experimental conditions, the method showed a good linearity in the range of 0.1-100.0 ng/mL for water samples and 0.5-100.0 ng/mL for vinegar samples, with the correlation coefficients varying from 0.9978 to 0.9997. The limits of detection (S/N = 3) of the method were in the range of 0.005-0.010 ng/mL for water samples and 0.01-0.05 ng/mL for vinegar samples, respectively. The recoveries of the method for the analytes at spiking levels of 5.0 and 70.0 ng/mL were between 84.6 and 106.4% with the relative standard deviations varying from 4.2 to 9.5%. The results indicated that the developed method could be a practical approach for the determination of paraben residues in water and vinegar samples.

  5. A multisyringe flow-through sequential extraction system for on-line monitoring of orthophosphate in soils and sediments

    DEFF Research Database (Denmark)

    Buanuam, Janya; Miró, Manuel; Hansen, Elo Harald

    2007-01-01

    A fully automated flow-through microcolumn fractionation system with on-line post-extraction derivatization is proposed for monitoring of orthophosphate in solid samples of environmental relevance. The system integrates dynamic sequential extraction using 1.0 mol l-1 NH4Cl, 0.1 mol l-1 NaOH and 0.......5 mol l-1 HCl as extractants according to the Hietjles-Lijklema (HL) scheme for fractionation of phosphorus associated with different geological phases, and on-line processing of the extracts via the Molybdenum Blue (MB) reaction by exploiting multisyringe flow injection as the interface between...... the solid containing microcolumn and the flow-through detector. The proposed flow assembly, capitalizing on the features of the multicommutation concept, implies several advantages as compared to fractionation analysis in the batch mode in terms of saving of extractants and MB reagents, shortening...

  6. On-line SPE-UHPLC method using fused core columns for extraction and separation of nine illegal dyes in chilli-containing spices.

    Science.gov (United States)

    Khalikova, Maria A; Satínský, Dalibor; Smidrkalová, Tereza; Solich, Petr

    2014-12-01

    The presented work describes the development of a simple, fast and effective on-line SPE-UHPLC-UV/vis method using fused core particle columns for extraction, separation and quantitative analysis of the nine illegal dyes, most frequently found in chilli-containing spices. The red dyes Sudan I-IV, Sudan Red 7B, Sudan Red G, Sudan Orange G, Para Red, and Methyl Red were separated and analyzed in less than 9 min without labor-consuming pretreatment procedure. The chromatographic separation was performed on Ascentis Express RP-Amide column with gradient elution using mixture of acetonitrile and water, as a mobile phase at a flow rate of 1.0 mL min(-1) and 55°C of temperature. As SPE sorbent for cleanup and pre-concentration of illegal dyes short guard fused core column Ascentis Express F5 was used. The applicability of proposed method was proven for three different chilli-containing commercial samples. Recoveries for all compounds were between 90% and 108% and relative standard deviation ranged from 1% to 4% for within- and from 2% to 6% for between-day. Limits of detection showed lower values than required by European Union regulations and were in the range of 3.3-10.3 µg L(-1) for standard solutions, 5.6-235.6 µg kg(-1) for chilli-containing spices.

  7. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    Energy Technology Data Exchange (ETDEWEB)

    Herrero Latorre, C., E-mail: carlos.herrero@usc.es [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain); Alvarez Mendez, J.; Barciela Garcia, J.; Garcia Martin, S.; Pena Crecente, R.M. [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain)

    2012-10-24

    Highlights: Black-Right-Pointing-Pointer The use of CNTs as sorbent for metal species in solid phase extraction has been described. Black-Right-Pointing-Pointer Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. Black-Right-Pointing-Pointer Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes - due to their high adsorption and desorption capacities - have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

  8. Flame AAS determination of lead in water with flow-injection preconcentration and speciation using functionalized cellulose sorbent.

    Science.gov (United States)

    Naghmush, A M; Pyrzyńska, K; Trojanowicz, M

    1995-06-01

    The on-line solid phase extraction of trace amount of lead in flow-injection system with flame AAS detection was investigated using cellulose sorbents with phosphonic acid and carboxymethyl groups, C(18) sorbent non-modified and modified with Pyrocatechol Violet or 8-quinolinol, commercial chelating sorbents Chelex 100 and Spheron Oxin 1000, non-polar sorbent Amberlite XAD-2 modified with Pyrocatechol Violet and several cation-exchange resins. The best dynamic characteristics of retention were observed for functionalized cellulose sorbents. For Cellex P assumed as optimum sorbent, elution with a separate fractions of nitric acid and ethanol allows the differentiation between tetraalkyllead and sum of inorganic lead and organolead species of smaller number of alkyl groups. The detection limit for the determination of inorganic Pb(II) was estimated as 0.17 microg/l. at preconcentration from 50 ml sample at a flow rate of 7 ml/min.

  9. [Determination of five avermectins in bovine liver by on-line solid-phase extraction with hydrophobic monolithic column coupled with high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Li, Xin; Zhang, Yaoqin; Ai, Lianfeng; Wang, Xuesheng; Wang, Manman; Xu, Houjun; Hao, Yulan

    2015-06-01

    A method based on on-line solid-phase extraction (SPE) with hydrophobic monolithic column coupled with high performance liquid chromatography-tandem mass spectrometry was developed for the simultaneous determination of five avermectins in bovine liver. A poly(butyl methacrylate-co-ethylene dimethacrylate) monolithic column was used as the sorbent. The parameters influenced on on-line SPE and separation process such as the loading mobile phase, the eluting flow rate and the solvent for the separation were investigated in detail. Blank samples, spiked samples, matrix effect and recovery experiments were investigated to evaluate the extraction efficiency and potential interfering compounds originating from the matrix. Under the optimized conditions, the method showed a linear range of 1-100 µg/L and the quantification limit of 5 µg/kg for each analyte. The presented method gave recoveries of 77.4%-98.4%. The relative standard deviations of intra-day and inter-day were 4.46%-8.03% and 4.79%-8.68%, respectively. Moreover, no significant changes were found in the extraction performance after more than 400 usages on one monolithic column, and even on the monoliths with various batches. The feasibility of the developed poly (butyl methacrylate-coethylene dimethacrylate) monolithic column based on the on-line SPE method for the determination of avermectins was further demonstrated by the analysis of real samples.

  10. Double-bed-type extraction needle packed with activated-carbon-based sorbents for very volatile organic compounds.

    Science.gov (United States)

    Ueta, Ikuo; Samsudin, Emi Liana; Mizuguchi, Ayako; Takeuchi, Hayato; Shinki, Takumi; Kawakubo, Susumu; Saito, Yoshihiro

    2014-01-01

    A novel needle-type sample preparation device was developed for the determination of very volatile organic compounds (VVOCs) in gaseous samples by gas chromatography-mass spectrometry (GC-MS). Two types of activated-carbon-based sorbents, Carbopack X and a carbon molecular sieve (CMS), were investigated as the extraction medium. A double-bed-type extraction needle showed successful extraction and desorption performance for all investigated VVOCs, including acetaldehyde, isoprene, pentane, acetone, and ethanol. Sensitive and reliable determination of VVOCs was achieved by systematically optimizing several desorption conditions. In addition, the effects of sample humidity on the extraction and desorption of analytes were investigated with the needle-type extraction devices. Only the CMS packed extraction needle was adversely affected by sample humidity during the desorption process; on the other hand the double-bed-type extraction needle was unaffected by sample humidity. Finally, the developed double-bed-type extraction needle was successfully applied to the analysis of breath VVOCs of healthy subjects.

  11. Feature Extraction in Sequential Multimedia Images: with Applications in Satellite Images and On-line Videos

    Science.gov (United States)

    Liang, Yu-Li

    Multimedia data is increasingly important in scientific discovery and people's daily lives. Content of massive multimedia is often diverse and noisy, and motion between frames is sometimes crucial in analyzing those data. Among all, still images and videos are commonly used formats. Images are compact in size but do not contain motion information. Videos record motion but are sometimes too big to be analyzed. Sequential images, which are a set of continuous images with low frame rate, stand out because they are smaller than videos and still maintain motion information. This thesis investigates features in different types of noisy sequential images, and the proposed solutions that intelligently combined multiple features to successfully retrieve visual information from on-line videos and cloudy satellite images. The first task is detecting supraglacial lakes above ice sheet in sequential satellite images. The dynamics of supraglacial lakes on the Greenland ice sheet deeply affect glacier movement, which is directly related to sea level rise and global environment change. Detecting lakes above ice is suffering from diverse image qualities and unexpected clouds. A new method is proposed to efficiently extract prominent lake candidates with irregular shapes, heterogeneous backgrounds, and in cloudy images. The proposed system fully automatize the procedure that track lakes with high accuracy. We further cooperated with geoscientists to examine the tracked lakes and found new scientific findings. The second one is detecting obscene content in on-line video chat services, such as Chatroulette, that randomly match pairs of users in video chat sessions. A big problem encountered in such systems is the presence of flashers and obscene content. Because of various obscene content and unstable qualities of videos capture by home web-camera, detecting misbehaving users is a highly challenging task. We propose SafeVchat, which is the first solution that achieves satisfactory

  12. Multivariate detection limits of on-line NIR model for extraction process of chlorogenic acid from Lonicera japonica.

    Science.gov (United States)

    Wu, Zhisheng; Sui, Chenglin; Xu, Bing; Ai, Lu; Ma, Qun; Shi, Xinyuan; Qiao, Yanjiang

    2013-04-15

    A methodology is proposed to estimate the multivariate detection limits (MDL) of on-line near-infrared (NIR) model in Chinese Herbal Medicines (CHM) system. In this paper, Lonicera japonica was used as an example, and its extraction process was monitored by on-line NIR spectroscopy. Spectra of on-line NIR could be collected by two fiber optic probes designed to transmit NIR radiation by a 2mm-flange. High performance liquid chromatography (HPLC) was used as a reference method to determine the content of chlorogenic acid in the extract solution. Multivariate calibration models were carried out including partial least squares regression (PLS) and interval partial least-squares (iPLS). The result showed improvement of model performance: compared with PLS model, the root mean square errors of prediction (RMSEP) of iPLS model decreased from 0.111mg to 0.068mg, and the R(2) parameter increased from 0.9434 to 0.9801. Furthermore, MDL values were determined by a multivariate method using the type of errors and concentration ranges. The MDL of iPLS model was about 14ppm, which confirmed that on-line NIR spectroscopy had the ability to detect trace amounts of chlorogenic acid in L. japonica. As a result, the application of on-line NIR spectroscopy for monitoring extraction process in CHM could be very encouraging and reliable.

  13. Preparation a new sorbent based on polymeric ionic liquid for stir cake sorptive extraction of organic compounds and inorganic anions.

    Science.gov (United States)

    Huang, Xiaojia; Wang, Yulei; Hong, Qiuyun; Liu, Yi; Yuan, Dongxing

    2013-11-01

    A new multi-interaction sorbent (MIS) based on polymeric ionic liquid was prepared and used as extractive medium of stir cake sorptive extraction (SCSE). In the presence of dimethyl sulfoxide, an ionic liquid, 1-vinylbenzyl-3-methylimidazolium chloride was used as monomer to copolymerize in situ with divinylbenzene to form the MIS. The influences of the content of monomer and the porogen solvent in the polymerization mixture on the extraction performance were investigated thoroughly. The MIS was characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. Parabens and aromatic amines were used to investigate the extraction performance of MIS-SCSE for apolar and strongly polar analytes, respectively. The extraction parameters for parabens and aromatic amines were optimized. At the same time, simple and sensitive analytical methods for parabens and aromatic amines in real samples were developed by the combination of MIS-SCSE and HPLC/DAD. Some inorganic anions, such as F(-), Br(-), NO3(-), PO4(3-) and SO4(2-), were used to test the extraction performance of MIS-SCSE for anions. Results indicated that mechanism involved in the extraction of MIS is the multi-interaction modes including π-π, hydrophobic, hydrogen-bonding, dipole-dipole and anion-exchange interactions.

  14. Development, comparison and application of sorbent-assisted accelerated solvent extraction, microwave-assisted extraction and ultrasonic-assisted extraction for the determination of polybrominated diphenyl ethers in sediments.

    Science.gov (United States)

    Song, Shanjun; Shao, Mingwu; Tang, Hua; He, Yajuan; Wang, Weihua; Liu, Liliang; Wu, Jiajia

    2016-12-02

    Fast and selective analytical methods were developed based on sorbent-assisted mechanism and microwave-assisted extraction (SA-MAE), accelerate solvent extraction (SA-ASE) and ultrasonic-assisted extraction (SA-UAE) for the determination of polybrominated diphenyl ethers (PBDEs) in sediments. The experimental parameters, such as extraction conditions and sorbent amounts, were optimized according to Taguchi Orthogonal Arrays. The accuracy of developed SA-methods was a satisfactory ranging from 71% to 118%. The inter/intra-day RSDs were extraction intensity may produce various matrix effects. In addition, the developed SA-ASE method was successfully applied on real environmental samples collected from a typical polluted area. The data and calculation suggested local environmental contamination pattern and potential pollution source.

  15. Matrix molecularly imprinted mesoporous sol–gel sorbent for efficient solid-phase extraction of chloramphenicol from milk

    Energy Technology Data Exchange (ETDEWEB)

    Samanidou, Victoria, E-mail: samanidu@chem.auth.gr [Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki (Greece); Kehagia, Maria [Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki (Greece); Kabir, Abuzar, E-mail: akabir@fiu.edu [International Forensic Research Institute, Department of Chemistry and Biochemistry, Florida International University, Miami, FL (United States); Furton, Kenneth G. [International Forensic Research Institute, Department of Chemistry and Biochemistry, Florida International University, Miami, FL (United States)

    2016-03-31

    Highly selective and efficient chloramphenicol imprinted sol–gel silica based inorganic polymeric sorbent (sol–gel MIP) was synthesized via matrix imprinting approach for the extraction of chloramphenicol in milk. Chloramphenicol was used as the template molecule, 3-aminopropyltriethoxysilane (3-APTES) and triethoxyphenylsilane (TEPS) as the functional precursors, tetramethyl orthosilicate (TMOS) as the cross-linker, isopropanol as the solvent/porogen, and HCl as the sol–gel catalyst. Non-imprinted sol–gel polymer (sol–gel NIP) was synthesized under identical conditions in absence of template molecules for comparison purpose. Both synthesized materials were characterized by Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FT-IR) and nitrogen adsorption porosimetry, which unambiguously confirmed their significant structural and morphological differences. The synthesized MIP and NIP materials were evaluated as sorbents for molecularly imprinted solid phase extraction (MISPE) of chloramphenicol in milk. The effect of critical extraction parameters (flow rate, elution solvent, sample and eluent volume, selectivity coefficient, retention capacity) was studied in terms of retention and desorption of chloramphenicol. Competition and cross reactivity tests have proved that sol–gel MIP sorbent possesses significantly higher specific retention and enrichment capacity for chloramphenicol compared to its non-imprinted analogue. The maximum imprinting factor (IF) was found as 9.7, whereas the highest adsorption capacity of chloramphenicol by sol–gel MIP was 23 mg/g. The sol–gel MIP was found to be adequately selective towards chloramphenicol to provide the necessary minimum required performance limit (MRPL) of 0.3 μg/kg set forth by European Commission after analysis by LC-MS even without requiring time consuming solvent evaporation and sample reconstitution step, often considered as an integral part in solid phase extraction work

  16. Aerogel sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Begag, Redouane; Rhine, Wendell E; Dong, Wenting

    2016-04-05

    The current invention describes methods and compositions of various sorbents based on aerogels of various silanes and their use as sorbent for carbon dioxide. Methods further provide for optimizing the compositions to increase the stability of the sorbents for prolonged use as carbon dioxide capture matrices.

  17. 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

    2017-08-21

    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.

  18. Study of on-line analysis using energy dispersive X-ray fluorescence spectrometry for controlling lanthanum and neodymium extraction

    Energy Technology Data Exchange (ETDEWEB)

    Wenli, Li; Ascenzo, G.D`; Curini, R. [Department of Chemistry, University of Rome `La Sapienza`, Rome (Italy); Gasparini, G.M.; Casarci, M.; Mattia, B.; Traverso, D.M.; Bellisario, F. [ENEA, CRE Casaccia INN-NUMA (Italy)

    1998-05-04

    Many rare-earth extraction processes require frequent control over separation process quality. Ideally, an analysis method for this type should be simple, rapid and reliable. Energy dispersive X-ray fluorescence (EDXRF) spectrometry, due to its relative simplicity of instrumentation, speed of analysis, and non-destructive nature, is well suited to this on-line analysis application. In particular, since the radioisotope energy dispersive XRF method eliminates the need to transport samples to a laboratory which houses the X-ray spectrometry, it is most commonly used for on-line analysis of extraction systems. The present paper describes an attempt to type the radioisotope source {sup 241}Am XRF on-line analysis arrangement coupled with a personal computer for controlling a lanthanum and neodymium separation process. From the HpGe detector (high-purity germanium) response, a continuous spectral signal is observed during loading of the feed samples. The separation process using countercurrent extraction consists of a 16-stage laboratory mixer-settler, a switching valve, and a pumping system. The performance of this control system is illustrated by extracting La, Nd acidic solutions with 100% tributyl phosphate

  19. Solid phase extraction for evaluation of occupational exposure to Pb (II) using XAD-4 sorbent prior to atomic absorption spectroscopy.

    Science.gov (United States)

    Shahtaheri, Seyed Jamaleddin; Khadem, Monireh; Golbabaei, Farideh; Rahimi-Froushan, Abbas; Ganjali, Mohammad Reza; Norouzi, Parviz

    2007-01-01

    Lead is an important constituent widely used in different industrial processes. For evaluation of workers' exposure to trace toxic metal of Pb (II), solid-phase extraction (SPE) was optimized. SPE using mini columns filled with XAD-4 resin was developed with regard to sample pH, ligand concentration, loading flow rate, elution solvent, sample volume, elution volume, the amount of resins, and sample matrix interferences. Lead ions were retained on a solid sorbent and then eluted, followed by a simple determination of analytes with flame atomic absorption spectrometery. The obtained recoveries of metal ions were greater than 92%. This method was validated with 3 different pools of spiked urine samples; it showed a good reproducibility over 6 consecutive days as well as 6 within-day experiments. This optimized method can be considered successful in simplifying sample preparation for a trace residue analysis of lead in different matrices when evaluating occupational and environmental exposures is required.

  20. Novel surface dummy molecularly imprinted silica as sorbent for solid-phase extraction of bisphenol A from water samples.

    Science.gov (United States)

    Hu, Xiaolei; Wu, Xiao; Yang, Fanfan; Wang, Qiang; He, Chiyang; Liu, Shaorong

    2016-01-01

    A novel surface molecularly imprinted silica composite was prepared by a dummy-template imprinting strategy for the solid-phase extraction (SPE) of bisphenol A (BPA). 2,2-Bis(4-hydroxyphenyl) hexafluoropropane (BPAF) was chosen as the template molecule, and a hybrid technique was used for imprinting procedure. The imprinted silica was characterized by FT-IR spectroscopy, scanning electron microscope, thermo-gravimetric analysis, and nitrogen adsorption-desorption isotherms. The static binding test verified that the imprinted silica had much higher recognition ability for BPA than the non-imprinted silica, and the kinetic adsorption test presented the fast binding kinetics of the surface imprinted silica for BPA. When used as a SPE sorbent, the imprinted silica showed high extraction efficiencies and high enrichment factor for BPA. Based on the imprinted silica, a SPE-HPLC-UV method was developed and successfully applied to the detection of BPA in BPA-spiked lake water, tap water and drinking water samples with a high recovery of 97.3-106.0%, a RSD of 1.2-3.8% (n=3) and a limit of detection (S/N=3) of 0.3 ng/mL. The analysis results of a certified BPA sample also demonstrated the reliability of present method. The new surface dummy molecularly imprinted silica completely avoided the interference of the residual template molecules and greatly improved the binding kinetic of the target molecules. Therefore, it can be used as a good sorbent for SPE of BPA in environmental water samples.

  1. [Research on quality parameters of scutellariae radix (formula particles) using on-line NIR in pilot with different extraction process].

    Science.gov (United States)

    Li, Yang; Wu, Zhi-Sheng; Shi, Xin-Yuan; Pan, Xiao-Ning; Zhang, Qiao; Qiao, Yan-Jiang

    2014-10-01

    The on-line monitor for the changes in the content of baicalin in Scutellariae Radix formula particles during the extraction process was conducted by using near infrared spectroscopy (NIR). High performance liquid chromatography (HPLC) was used as a reference method. Kennard-Stone (KS) was used to divide sample sets, so as to compare different pretreatment methods. The synergy interval partial least squares (SiPLS) was used to screen out modeling wave band to establish partial least-squares models. The relative error method was applied to predict forecast set samples of Scutellariae Radix in three extraction phases. The results showed that the model established by Savitzky-Golay smoothing with 11 points (SG11 points) was the best, with the root mean square with cross validation (RMSECV), root mean square error of correction (RMSEC) and root mean square error of prediction (RMSEP) of baicalin of 0.092 7, 0.134 4 and 0.114 8, respectively, the determination coefficient R2 of greater than 0.99, and the relative error of baicalin content of less than 5%. This indicates that the on-line near infrared reflectance spectroscopy could be applied in on-line monitor and quality control of the extraction process of Scutellariae Radix formula particles.

  2. Preparation and evaluation of open tubular C18-silica monolithic microcartridges for preconcentration of peptides by on-line solid phase extraction capillary electrophoresis.

    Science.gov (United States)

    Ortiz-Villanueva, Elena; Benavente, Fernando; Giménez, Estela; Yilmaz, Fatma; Sanz-Nebot, Victoria

    2014-10-10

    In this study, C18-silica monoliths were synthesized as a porous layer in open tubular capillary columns, to be cut later into microcartridges for the analysis of neuropeptides by on-line solid-phase extraction capillary electrophoresis with UV and MS detection (SPE-CE-UV and SPE-CE-MS). First, several types of C18-silica monolithic (MtC18) microcartridges were used to analyse standard solutions of five neuropeptides (i.e. dynorphin A (1-7), substance P (7-11), endomorphin 1, methionine enkephalin and [Ala]-methionine enkephalin). The MtC18 sorbents were especially selective against endomorphin 1 and substance P (7-11)). The best results in terms of sensitivity and inter-microcartridge reproducibility were achieved with the microcartridges obtained from a 10-cm open tubular capillary column with a thin monolithic coating with large through-pores (1-5μm). Run-to-run repeatability, microcartridge durability, linearity ranges and LODs were studied by MtC18-SPE-CE-MS. As expected due to their greater selectivity, the best LOD enhancement was obtained for End1 and SP (7-11) (50 times with regard to CE-MS). Finally, the suitability of the methodology for analysing biological fluids was tested with plasma samples spiked with End1 and SP (7-11). Results obtained were promising because both neuropeptides could be detected at 0.05μgmL(-1), which was almost the same concentration level as for the standard solutions (0.01μgmL(-1)).

  3. Hybrid monolith sorbent of polypyrrole-coated graphene oxide incorporated into a polyvinyl alcohol cryogel for extraction and enrichment of sulfonamides from water samples.

    Science.gov (United States)

    Chullasat, Kochaporn; Nurerk, Piyaluk; Kanatharana, Proespichaya; Kueseng, Pamornrat; Sukchuay, Thanyaporn; Bunkoed, Opas

    2017-04-08

    A hybrid monolith sorbent of polypyrrole-coated graphene oxide embedded in polyvinyl alcohol cryogel was prepared and used as an effective solid phase extraction sorbent for the determination of trace sulfonamides. The large surface areas with many adsorption sites of polypyrrole and graphene oxide facilitated the high adsorption of sulfonamides via hydrogen bonding, π-π and hydrophobic interactions. The high porosity of the polyvinyl alcohol cryogel helped to reduce the back pressure that occurs in a conventional packed solid phase extraction cartridge. The effecting parameters on the extraction efficiency including the type of sorbent, the polymerization time, desorption conditions, the sample pH, the sample volume, the sample flow rate, and ionic strength were investigated and optimized. Under the optimum conditions, the developed method provided a wide linear range from 0.20 to 100.0 μg L(-1) for sulfadiazine, sulfathiazole and sulfamerazine; and from 0.10 to 100 μg L(-1) for sulfamethazine, sulfamonomethoxine and sulfadimethoxine. The limits of detection were 0.20 μg L(-1) for sulfadiazine, sulfathiazole and sulfamerazine; and 0.10 μg L(-1) for sulfamethazine, sulfamonomethoxine and sulfadimethoxine. The developed hybrid monolith polypyrrole-coated graphene oxide embedded in the polyvinyl alcohol cryogel sorbent provided good recoveries in the range of 85.5-99.0% with RSDs of less than 5.0%. The sorbent offered a good reproducibility, was robust and can be reused at least 10 times. It was successfully applied for the extraction and enrichment of sulfonamides from normal and supplemented water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Using pollen grains as novel hydrophilic solid-phase extraction sorbents for the simultaneous determination of 16 plant growth regulators.

    Science.gov (United States)

    Lu, Qian; Wu, Jian-Hong; Yu, Qiong-Wei; Feng, Yu-Qi

    2014-11-01

    In this article, pollen grains were for the first time used as a hydrophilic solid-phase extraction (HILIC-SPE) sorbent for the determination of 16 plant growth regulators (PGRs) in fruits and vegetables. Fourier transform infrared spectroscopy (FT-IR), scanning electronic microscopy (SEM) and nitrogen sorption porosimetry (NSP) were used to investigate the chemical structure and the surface properties of the pollen grains. Pollen grains exhibited an excellent adsorption capacity for some polar compounds due to their particular functional groups. Several parameters influencing extraction performance were investigated. A green and simple HILIC-SPE-method using pollen grain cartridge for purification of fruit and vegetable extractions, followed by ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry (UHPLC-MS/MS) was established. Good linear relationships were obtained for 16 PGRs with correlation coefficients (R) above 0.9980. The limits of detection (LODs) of 16 PGRs in cucumber were in the range of 0.01-1.10 μg · kg(-1). Reproducibility of the method was evaluated by intra-day and inter-day precisions with relative standard deviations (RSDs), which were less than 14.4%. We successfully applied this methodology to analyze 16 PGRs in 8 different kinds of fruits and vegetables. The recoveries from samples spiked with 16 PGRs were from 80.5% to 119.2%, with relative standard deviations less than 15.0%.

  5. A novel dispersive micro solid phase extraction using zein nanoparticles as the sorbent combined with headspace solid phase micro-extraction to determine chlorophenols in water and honey samples by GC-ECD.

    Science.gov (United States)

    Farhadi, Khalil; Matin, Amir Abbas; Amanzadeh, Hatam; Biparva, Pourya; Tajik, Hossein; Farshid, Amir Abbas; Pirkharrati, Hossein

    2014-10-01

    This study presents a new technique, dispersive micro solid phase extraction (DMSPE) combined with headspace solid phase micro-extraction (HS-SPME) for extraction and determination of chlorophenols (CPs) in water and honey samples using a Gas Chromatography-Electron Capture Detector (GC-ECD). Zein nanoparticles were made by liquid-liquid dispersion and applied for the first time as the sorbent phase in DMSPE. In the proposed DMSPE-HS-SPME method, 1% w/v of ethanolic zein solution was added to an aqueous sample and then a dose of the in-situ generated zein nanoparticles was applied to a pre-concentration of target analytes. Thermal desorption of analytes was performed after the isolating sorbent phase, and then HS-SPME was applied for enrichment prior to introducing to gas chromatography. All the important parameters influencing efficiency of the extraction process such effects of salt, pH, sorbent concentration, temperature, sorbent solution volume in DMSPE procedure, extraction temperature, extraction time, desorption temperature and time in the HS-SPME procedure were investigated and optimized. Results showed that under optimum extraction conditions, detection limits (signal to noise ratio=3) were in the range of 0.08-0.6 ng mL(-1) and evaluations for relative standard deviations (RSDs %) were between 6.62% and 8.36%.

  6. Simultaneous extraction and HPLC determination of 3-indole butyric acid and 3-indole acetic acid in pea plant by using ionic liquid-modified silica as sorbent.

    Science.gov (United States)

    Sheikhian, Leila; Bina, Sedigheh

    2016-01-15

    In this study, ionic liquid-modified silica was used as sorbent for simultaneous extraction and preconcentration of 3-indole butyric acid and 3-indole acetic acid in pea plants. The effect of some parameters such as pH and ionic strength of sample solution, amount of sorbent, flow rate of aqueous sample solution and eluent solution, concentration of eluent solution, and temperature were studied for each hormone solution. Percent extraction of 3-indole butyric acid and 3-indole acetic acid was strongly affected by pH of aqueous sample solution. Ionic strength of aqueous phase and temperature showed no serious effects on extraction efficiency of studied plant hormones. Obtained breakthrough volume was 200mL for each of studied hormones. Preconcentration factor for spectroscopic and chromatographic determination of studied hormones was 100 and 4.0×10(3) respectively. Each solid sorbent phase was reusable for almost 10 times of extraction/stripping procedure. Relative standard deviations of extraction/stripping processes of 3-indole butyric acid and 3-indole acetic acid were 2.79% and 3.66% respectively. The calculated limit of detections for IBA and IAA were 9.1×10(-2)mgL(-1) and 1.6×10(-1)mgL(-1) respectively.

  7. Selective solid-phase extraction using molecularly imprinted polymer as a sorbent for the analysis of fenarimol in food samples.

    Science.gov (United States)

    Khan, Shagufta; Bhatia, Tejasvi; Trivedi, Purushottam; Satyanarayana, G N V; Mandrah, Kapil; Saxena, Prem Narayan; Mudiam, Mohana Krishna Reddy; Roy, Somendu Kumar

    2016-05-15

    In the present communication, a non-covalent fenarimol-imprinted polymer was synthesized by precipitation polymerization technique using methacrylic acid (MAA) as a functional monomer, ethylene glycol dimethacrylate (EGDMA) as a cross-linker, and azobisisobutyronitrile (AIBN) as an initiator in different porogenic solvent. Binding study of molecularly imprinted and non-imprinted polymer (MIP and NIP) showed that MIP possesses a higher affinity towards this analyte compared to NIP. The binding affinity of MIP was calculated by static and kinetic adsorption study. Further, a MIP based cartridge was designed to use in extraction process, necessary for specific determination and quantification of the fungicide in food matrices. Under the optimum conditions, developed method was found to be linear (R(2)=0.9999-0.9994). Limit of detection (LOD) and limit of quantitation (LOQ) in samples were 0.03-0.06 and 0.12-0.21 μg mL(-1), respectively. The rate of recovery of fenarimol was 91.16-99.52% on MIPs. The validated method of molecularly imprinted solid-phase extraction (MISPE) cartridge was successfully applied to the food matrices and compared with commercial sorbent (RP18 and Oasis HLB). However we feel, this method has promising applications in the routine analysis of food samples in industry.

  8. SEMIAUTOMATIC BUILDING EXTRACTION FROM STEREOIMAGE PAIR BASED ON LINES GROUPING AND LEAST SQUARES MATCHING

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    The paper presents a general paradigm of semiautomatic building extrac tion from aerial stereo image pair.In the semiautomatic extraction system,the building model is defined by selected roof type through human-machine interface and input the approximation of area where the extracted building exists.Then un der the knowledge of the roof type,low-level and mid-level processing including edge detection,straight line segments extraction and line segments grouping ar e used to establish the initial geometrical model of the roof-top.However,the initial geometrical model is not so accurate in geometry.To attain accurate res ults,a general least squares adjustment integrating the linear templates matchin g model with geometrical constraints in object-space is applied to refine the ini tial geometrical model.The adjustment model integrating the straight edge pat tern and 3D constraints together is a well-studied optimal and ant i-noise method.After gaining proper initial values,this adjustment model can f lexibly process extraction of kinds of roof types by changing or assembling the geometrical constraints in object-space.

  9. A hybrid material as a sorbent phase for the disposable pipette extraction technique enhances efficiency in the determination of phenolic endocrine-disrupting compounds.

    Science.gov (United States)

    Corazza, Gabriela; Merib, Josias; Magosso, Hérica A; Bittencourt, Otávio R; Carasek, Eduardo

    2017-09-01

    In this study, the hybrid material 3-n-propyl(3-methylpyridinium) silsesquioxane chloride (Si3Py(+)Cl(-)) was synthesized and investigated as a novel sorbent phase for the disposable pipette extraction (DPX) technique coupled to high-performance liquid chromatography-florescence detection. This sorbent phase was characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). Aqueous samples containing the phenolic endocrine-disrupting compounds bisphenol A (BPA), 17α-ethynylestradiol (EE2), 4-tert-octylphenol (4-t-OP), 4-octylphenol (4-OP) and 4-nonylphenol (4-NP) were subjected to DPX procedures and a series of optimizations was performed to determine the ideal extraction conditions using this approach. The proposed sorbent phase exhibited higher extraction efficiency than DPX-RP (reversed phase tips containing styrene-divinylbenzene), commonly used for the determination of the phenolic endocrine- disrupting-compounds under study. Satisfactory analytical performance was achieved with linear ranges from 2 to 100μgL(-1) for 4-t-OP and 1-100μgL(-1) for the other analytes. Limits of detection of 0.60μgL(-1) for 4-t-OP and 0.30μgL(-1) for other analytes, RSDs ranging from 1 to 20% and relative recoveries of 83-116% were obtained. Based on these satisfactory results, this sorbent phase represents a valuable alternative for the extraction of compounds with polar moieties in their structure. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Specific mercury(II) adsorption by thymine-based sorbent.

    Science.gov (United States)

    Liu, Xiangjun; Qi, Cui; Bing, Tao; Cheng, Xiaohong; Shangguan, Dihua

    2009-04-15

    A new kind of polymer sorbent based on the specific interaction of Hg(II) with nucleic acid base, thymine, is described for the selective adsorption of Hg(II) from aqueous solution. Two types of sorbents immobilized with thymine were prepared by one-step swelling and polymerization and graft polymerization, respectively. The maximum static adsorption capacity of the new polymer sorbents for Hg(II) is proportional to the density of thymine on their surface, up to 200mg/g. Moreover, the new kind polymer sorbent shows excellent selectivity for Hg(II) over other interfering ions, such as Cu(II), Cd(II), Zn(II), Co(II), Ca(II) and Mg(II), exhibits very fast kinetics for Hg(II) adsorption from aqueous solution, and can be easily regenerated by 1.0M HCl. It also has been successfully used for the selective adsorption of spiked Hg(II) from real tap water samples. This new thymine polymer sorbent holds a great promise in laboratory and industrial applications such as separation, on-line enrichment, solid-phase extraction, and removal of Hg(II) from pharmaceutical, food and environmental samples.

  11. One-pot synthesized functionalized mesoporous silica as a reversed-phase sorbent for solid-phase extraction of endocrine disrupting compounds in milks.

    Science.gov (United States)

    Gañán, Judith; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Marina, María Luisa; Sierra, Isabel

    2016-01-08

    A new procedure for the determination of 12 naturally occurring hormones and some related synthetic chemicals in milk, commonly used as growth promoters in cattle, is reported. The method is based on liquid-liquid extraction followed by solid-phase extraction (SPE) using a new one-pot synthesized ordered mesoporous silica (of the SBA-15 type) functionalized with octadecyl groups (denoted as SBA-15-C18-CO) as reversed-phase sorbent. The analytes were eluted with methanol and then submitted to HPLC with diode array detection. Under optimal conditions, the method quantification limit for the analytes ranged from 0.023 to 1.36μg/mL. The sorbent affored the extraction of estrone, 17β-estradiol, estriol, progesterone, hexestrol, diethylstilbestrol, 4-androstene-3,17-dione, ethinylestradiol, 17α-methyltestosterone, nandrolone, prednisolone and testosterone with mean recoveries ranging from 72% to 105% (except for diethylstilbestrol) with RSDextraction methods, therefore SBA-15-C18-CO mesoporous silica possess a high potential as a reversed-phase sorbent for SPE of the 12 mentioned endocrine disrupting compounds in milk samples.

  12. β-cyclodextrin-bonded silica particles as novel sorbent for stir bar sorptive extraction of phenolic compounds.

    Science.gov (United States)

    Faraji, Hakim; Husain, Syed Waqif; Helalizadeh, Masoumeh

    2011-01-01

    A stir bar coated with β-cyclodextrin-bonded-silica (CDS) as novel sorbent has been developed and used to analyze seven phenolic compounds in aqueous samples, followed by thermal desorption and gas chromatography-mass spectrometric detection. Significant parameters affecting sorption process such as the time and temperature of sorption and desorption, ionic strength, pH and stirring rate have been optimized and discussed. The coating has a high thermal stability up to 300°C and long application lifetime (80 times). The porous structure of CDS coating provides high surface area and allows high extraction efficiency. Under the selected conditions, linearity range of 0.1-400 μg/L, limit of quantifications of 0.08-3.3 μg/L and method detection limits of 0.02-1.00 μg/L have been obtained. A satisfactory repeatability (RSD ≤ 6.5, n = 7) with good linearity (0.9975 ≤ r(2) ≤ 0.9996) of results illustrated a good performance of the present method. The recovery of different natural water samples was higher than 81.5%.

  13. Automated Protein Biomarker Analysis: on-line extraction of clinical samples by Molecularly Imprinted Polymers

    Science.gov (United States)

    Rossetti, Cecilia; Świtnicka-Plak, Magdalena A.; Grønhaug Halvorsen, Trine; Cormack, Peter A. G.; Sellergren, Börje; Reubsaet, Léon

    2017-03-01

    Robust biomarker quantification is essential for the accurate diagnosis of diseases and is of great value in cancer management. In this paper, an innovative diagnostic platform is presented which provides automated molecularly imprinted solid-phase extraction (MISPE) followed by liquid chromatography-mass spectrometry (LC-MS) for biomarker determination using ProGastrin Releasing Peptide (ProGRP), a highly sensitive biomarker for Small Cell Lung Cancer, as a model. Molecularly imprinted polymer microspheres were synthesized by precipitation polymerization and analytical optimization of the most promising material led to the development of an automated quantification method for ProGRP. The method enabled analysis of patient serum samples with elevated ProGRP levels. Particularly low sample volumes were permitted using the automated extraction within a method which was time-efficient, thereby demonstrating the potential of such a strategy in a clinical setting.

  14. Automated Protein Biomarker Analysis: on-line extraction of clinical samples by Molecularly Imprinted Polymers

    Science.gov (United States)

    Rossetti, Cecilia; Świtnicka-Plak, Magdalena A.; Grønhaug Halvorsen, Trine; Cormack, Peter A.G.; Sellergren, Börje; Reubsaet, Léon

    2017-01-01

    Robust biomarker quantification is essential for the accurate diagnosis of diseases and is of great value in cancer management. In this paper, an innovative diagnostic platform is presented which provides automated molecularly imprinted solid-phase extraction (MISPE) followed by liquid chromatography-mass spectrometry (LC-MS) for biomarker determination using ProGastrin Releasing Peptide (ProGRP), a highly sensitive biomarker for Small Cell Lung Cancer, as a model. Molecularly imprinted polymer microspheres were synthesized by precipitation polymerization and analytical optimization of the most promising material led to the development of an automated quantification method for ProGRP. The method enabled analysis of patient serum samples with elevated ProGRP levels. Particularly low sample volumes were permitted using the automated extraction within a method which was time-efficient, thereby demonstrating the potential of such a strategy in a clinical setting. PMID:28303910

  15. FI/SI on-line solvent extraction/back extraction preconcentration coupled to direct injection nebulization inductively coupled plasma mass spectrometry for determination of copper and lead

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2002-01-01

    at a sample flow rate of 6.0 ml/min The precisions (RSD) at the 0.2 mug/1 level were 4.4% (Cu) and 4.8% (Pb), respectively. The applicability of the procedure is demonstrated for the determination of copper and lead in three certified reference materials and a urine sample.......An automated sequential injection on-line preconcentration procedure for determination of trace levels of copper and lead via solvent extraction/back extraction coupled to ICP-MS is described. In citrate buffer of pH 3, neutral complexes between the analytes and the chelating reagent, ammonium...

  16. Exploiting Sequential Injection on-line Solvent Extraction/Back Extraction with Detection by ETAAS or ICPMS

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    tolerances. With detection by ETAAS, separation/preconcentration by solvent extraction has enjoyed much use. However, this approach is not necessarily the optimal one since introduction of organic eluates directly into the graphite tube might lead to deteriorated reproducibility and lower sensitivity....... And for ICPMS, organics are prohibitive because they give rise to an unstable plasma, and excessive carbon deposited on the sampling and skimmer cones might result in a gradual loss of sensitivity. All of these difficulties can be readily overcome by using solvent extraction/back extraction. Surprisingly...

  17. Exploiting sequential injection on-line solvent extraction/back extraction with detection by ETAAS and ICPMS

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    . With detection by ETAAS, separation/preconcentration by solvent extraction has enjoyed much use. However, this approach is not necessarily the optimal one since introduction of organic eluates directly into the graphite tube might lead to deteriorated reproducibility and lower sensitivity. And for ICPMS......, organics are prohibitive because they give rise to an unstable plasma, and excessive carbon deposited on the sampling and skimmer cones might result in a gradual loss of sensitivity. All of these difficulties can be readily overcome by using solvent extraction/back extraction. Surprisingly, this approach...

  18. On-line lab-in-syringe cloud point extraction for the spectrophotometric determination of antimony.

    Science.gov (United States)

    Frizzarin, Rejane M; Portugal, Lindomar A; Estela, José M; Rocha, Fábio R P; Cerdà, Victor

    2016-02-01

    Most of the procedures for antimony determination require time-consuming sample preparation (e.g. liquid-liquid extraction with organic solvents), which are harmful to the environment. Because of the high antimony toxicity, a rapid, sensitive and greener procedure for its determination becomes necessary. The goal of this work was to develop an analytical procedure exploiting for the first time the cloud point extraction on a lab-in-syringe flow system aiming at the spectrophotometric determination of antimony. The procedure was based on formation of an ion-pair between the antimony-iodide complex and H(+) followed by extraction with Triton X-114. The factorial design showed that the concentrations of ascorbic acid, H2SO4 and Triton X-114, as well as second and third order interactions were significant at the 95% confidence level. A Box-Behnken design was applied to obtain the response surfaces and to identify the critical values. System is robust at the 95% confidence level. A linear response was observed from 5 to 50 µg L(-1), described by the equation A=0.137+0.050C(Sb) (r=0.998). The detection limit (99.7% confidence level), the coefficient of variation (n=5; 15 µg L(-1)) and the sampling rate was estimated at 1.8 µg L(-1), 1.6% and 16 h(-1), respectively. The procedure allows quantification of antimony in the concentrations established by environmental legislation (6 µg L(-1)) and it was successfully applied to the determination of antimony in freshwater samples and antileishmanial drugs, yielding results in agreement with those obtained by HGFAAS at the 95% confidence level.

  19. Automatic Building Extraction and Roof Reconstruction in 3k Imagery Based on Line Segments

    Science.gov (United States)

    Köhn, A.; Tian, J.; Kurz, F.

    2016-06-01

    We propose an image processing workflow to extract rectangular building footprints using georeferenced stereo-imagery and a derivative digital surface model (DSM) product. The approach applies a line segment detection procedure to the imagery and subsequently verifies identified line segments individually to create a footprint on the basis of the DSM. The footprint is further optimized by morphological filtering. Towards the realization of 3D models, we decompose the produced footprint and generate a 3D point cloud from DSM height information. By utilizing the robust RANSAC plane fitting algorithm, the roof structure can be correctly reconstructed. In an experimental part, the proposed approach has been performed on 3K aerial imagery.

  20. Electrospun composite of polypyrrole-polyamide as a micro-solid phase extraction sorbent.

    Science.gov (United States)

    Bagheri, Habib; Aghakhani, Ali; Akbari, Maryam; Ayazi, Zahra

    2011-07-01

    A micro-solid phase extraction technique was developed using a novel polypyrrole-polyamide nanofiber sheet, fabricated by electrospinning method. The applicability of the new nanofiber sheet was examined as an extracting medium to isolate malathion as a model pesticide from aqueous samples. Solvent desorption was subsequently performed in a microvial, and an aliquot of extractant was injected into gas chromatography-mass spectrometry. Various parameters affecting the electrospinning process including monomer concentration, polyamide content, applied voltage, and electrospinning time were examined. After fabricating the most suitable preparation conditions, influential parameters on the extraction and desorption processes were optimized. The developed method proved to be rather convenient and offers sufficient sensitivity and good reproducibility. The limit of detection (S/N = 3) and limit of quantification (S/N = 10) of the method under optimized conditions were 50 and 100 ng L(-1), respectively. The relative standard deviation at concentration level of 1 ng mL(-1) was 2% (n = 3). The calibration curve of analyte showed linearity in the range of 0.1-1 ng mL(-1) (R (2) = 0.9975). The developed method was successfully applied to tap and Zayanderood river water samples, while the relative recovery percentages of 98% and 96% were obtained, respectively. The whole procedure showed to be conveniently applicable and quite easy to be manipulated.

  1. Polypyrrole/magnetic nanoparticles composite as an efficient sorbent for dispersive micro-solid-phase extraction of antidepressant drugs from biological fluids.

    Science.gov (United States)

    Asgharinezhad, Ali Akbar; Karami, Sara; Ebrahimzadeh, Homeira; Shekari, Nafiseh; Jalilian, Niloofar

    2015-10-15

    In this study, polypyrrole/magnetic nanoparticles composites in the presence of two different dopants were synthesized with the aid of chemical oxidative polymerization process for dispersive-μ-solid phase extraction (D-μ-SPE). The synthesized magnetic sorbents were characterized by various techniques. The results exhibited that the nanocomposite modified by polypyrrole with sodium perchlorate as a dopant demonstrated higher extraction efficiency for citalopram (CIT) and sertraline (STR) as the model compounds. This nanosorbent in combination with high performance liquid chromatography-UV detection was applied for extraction, preconcentration and determination of CIT and STR in urine and plasma samples. The effect of various parameters on the extraction efficiency including: sample pH, amount of sorbent, sorption time, eluent and its volume, salt content, and elution time were investigated and optimized. The opted conditions were: sample pH, 9.0; sorbent dosage, 10mg; sorption time, 7 min; elution solvent and its volume, 0.06 mol L(-1) HCl in methanol, 120 μL; elution time, 2 min and without addition of salt to the sample. The calibration curves were linear in the concentration range of 1-800 μg L(-1). The limits of detection (LODs) were obtained in the range of 0.2-1.0 μg L(-1) for CIT and 0.3-0.7 μg L(-1) for STR, respectively. The percent of extraction recoveries and relative standard deviations (n=5) were in the range of 93.4-99, 4.8-8.4 for CIT and 94-98.4, 4.3-9.2 for STR, respectively. Finally, the applicability of the method was successfully confirmed by the extraction and determination of CIT and STR in human urine and plasma samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Vortex-Assisted Dispersive Micro-Solid Phase Extraction Using CTAB-Modified Zeolite NaY Sorbent Coupled with HPLC for the Determination of Carbamate Insecticides.

    Science.gov (United States)

    Salisaeng, Pawina; Arnnok, Prapha; Patdhanagul, Nopbhasinthu; Burakham, Rodjana

    2016-03-16

    A vortex-assisted dispersive micro-solid phase extraction (VA-D-μ-SPE) based on cetyltrimethylammonium bromide (CTAB)-modified zeolite NaY was developed for preconcentration of carbamate pesticides in fruits, vegetables, and natural surface water prior to analysis by high performance liquid chromatography with photodiode array detection. The small amounts of solid sorbent were dispersed in a sample solution, and extraction occurred by adsorption in a short time, which was accelerated by vortex agitation. Finally, the sorbents were filtered from the solution, and the analytes were subsequently desorbed using an appropriate solvent. Parameters affecting the VA-D-μ-SPE performance including sorbent amount, sample volume, desorption solvent ,and vortex time were optimized. Under the optimum condition, linear dynamic ranges were achieved between 0.004-24.000 mg kg(-1) (R(2) > 0.9946). The limits of detection (LODs) ranged from 0.004-4.000 mg kg(-1). The applicability of the developed procedure was successfully evaluated by the determination of the carbamate residues in fruits (dragon fruit, rambutan, and watermelon), vegetables (cabbage, cauliflower, and cucumber), and natural surface water.

  3. The determination of organochlorine pesticides based on dynamic microwave-assisted extraction coupled with on-line solid-phase extraction of high-performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Chen Ligang [College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012 (China); Ding Lan [College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012 (China)]. E-mail: analchem@jlu.edu.cn; Jin Haiyan [College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012 (China); Song Daqian [College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012 (China); Zhang Huarong [College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012 (China); Li Jiantao [College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012 (China); Zhang Kun [College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012 (China); Wang Yutang [College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012 (China); Zhang Hanqi [College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012 (China)

    2007-04-25

    A rapid technique based on dynamic microwave-assisted extraction coupled with on-line solid-phase extraction of high-performance liquid chromatography (DMAE-SPE-HPLC) has been developed. A TM{sub 010} microwave resonance cavity built in the laboratory was applied to concentrate the microwave energy. The sample placed in the zone of microwave irradiation was extracted with 95% acetonitrile (ACN) aqueous solution which was driven by a peristaltic pump at a flow rate of 1.0 mL min{sup -1}. The extraction can be completed in a recirculating system in 10 min. When a number of extraction cycles were completed, the extract (1 mL) was diluted on-line with water. Then the extract was loaded into an SPE column where the analytes were retained while the unretained matrix components were washed away. Subsequently, the analytes were automatically transferred from the SPE column to the analytical column and determined by UV detector at 238 nm. The technique was used for determination of organochlorine pesticides (OCPs) in grains, including wheat, rice, corn and bean. The limits of detection of OCPs are in the range of 19-37 ng g{sup -1}. The recoveries obtained by analyzing the four spiked grain samples are in the range of 86-105%, whereas the relative standard deviation (R.S.D.) values are <8.7% ranging from 1.2 to 8.7%. Our method was demonstrated to be fast, accurate, and precise. In addition, only small quantities of solvent and sample were required.

  4. Solid-phase extraction of galloyl- and caffeoylquinic acids from natural sources (Galphimia glauca and Arnicae flos) using pure zirconium silicate and bismuth citrate powders as sorbents inside micro spin columns.

    Science.gov (United States)

    Hussain, Shah; Schönbichler, Stefan A; Güzel, Yüksel; Sonderegger, Harald; Abel, Gudrun; Rainer, Matthias; Huck, Christian W; Bonn, Günther K

    2013-10-01

    Galloyl- and caffeoylquinic acids are among the most important pharmacological active groups of natural compounds. This study describes a pre-step in isolation of some selected representatives of these groups from biological samples. A selective solid-phase extraction (SPE) method for these compounds may help assign classes and isomer designations within complex mixtures. Pure zirconium silicate and bismuth citrate powders (325 mesh) were employed as two new sorbents for optimized SPE of phenolic acids. These sorbents possess electrostatic interaction sites which accounts for additional interactions for carbon acid moieties as compared to hydrophilic and hydrophobic sorbents alone. Based on this principle, a selective SPE method for 1,3,4,5-tetragalloylquinic acid (an anti-HIV and anti-asthamatic agent) as a starting compound was developed and then deployed upon other phenolic acids with success. The recoveries and selectivities of both sorbents were compared to most commonly applied and commercially available sorbents by using high performance liquid chromatography. The nature of interaction between the carrier sorbent and the acidic target molecules was investigated by studying hydrophilic (silica), hydrophobic (C18), mixed-mode (ionic and hydrophobic: Oasis(®) MAX) and predominantly electrostatic (zirconium silicate) materials. The newly developed zirconium silicate and bismuth citrate stationary phases revealed promising results for the selective extraction of galloyl- and caffeoylquinic acids from natural sources. It was observed that zirconium silicate exhibited maximum recovery and selectivity for tetragalloylquinic acid (84%), chlorogenic acid (82%) and dicaffeoylquinic acid (94%) among all the tested sorbents.

  5. On-line Identification of chiral ofloxacin in milk with an extraction/ionization device coupled to Electrospray Mass Spectrometry.

    Science.gov (United States)

    Wang, Jiang; Jiang, Xiao-Xiao; Zhao, Wei; Hu, Jun; Guan, Qi-Yuan; Xu, Jing-Juan; Chen, Hong-Yuan

    2017-08-15

    The direct separation and analysis of chiral drugs in the complex matrix systems are meaningful and challenging. As the most common broad-spectrum antibiotic, levofloxacin has a strong antibacterial ability, but its enantiomer, dextrofloxacin can cause serious harm to human health. In this work, we reported a rapid on-line extraction/ionization device coupled with Electrospray Mass Spectrometry (ESI-MS) for chiral analysis of ofloxacin enantiomers in complex matrix of milk. Since ofloxacin is difficult to dissolve in water and most organic solvents, the procedure of separating ofloxacin in complex system is often complicated. Using the homemade apparatus, the sample pretreatment process was greatly simplified. Milk sample was directly injected and chiral ofloxacin in the sample was extracted at PTFE membrane for further ionization. It took less than 10s to finish all the procedures including sampling, extraction, reagents mixing, ionization and mass analysis. Utilizing reaction thermodynamics method, trimeric cluster ion [Ni(ΙΙ)(ref)2Ofloxacin-H](+) was formed and collisionally dissociated to get chiral resolution of levofloxacin and dextrofloxacin due to the different relative stabilities of the two diastereomeric clusters produced through the dissociation of Ni(ΙΙ) bound trimeric clusters. With the proposed method, qualitative and quantitative chiral analysis of ofloxacin in milk was successfully achieved in a simple and fast way. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Comparative study of different fabric phase sorptive extraction sorbents to determine emerging contaminants from environmental water using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Lakade, Sameer S; Borrull, Francesc; Furton, Kenneth G; Kabir, Abuzar; Fontanals, Núria; Marcé, Rosa Maria

    2015-11-01

    A new sorptive extraction technique, fabric phase sorptive extraction (FPSE), using different coating chemistries: non-polar sol-gel poly(dimethyldiphenylsiloxane) (PDMDPS), medium polar sol-gel poly(tetrahydrofuran) (PTHF), and polar sol-gel poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) (PEG-PPG-PEG triblock) and sol-gel Carbowax 20 M were evaluated to extract a group of pharmaceuticals and personal care products (PPCPs) with wide range of polarity from environmental aqueous samples. Different parameters affecting FPSE such as sample pH, stirring speed, addition of salt, extraction time, sample volume, elution solvent and desorption time were optimized for each sorbent coated FPSE media. Under optimum conditions, FPSE media coated with sol-gel Carbowax 20 M provided the highest absolute recoveries (77-85%) for majority of the analytes with the exception of the most polar ones. Nevertheless, all four sorbents offered better recovery compared to the commercially available coating for stir-bar sorptive extraction based on Ethylene Glycol/Silicone (EG/Silicone). The method based on FPSE with sol-gel Carbowax 20 M media and liquid chromatography-(electrospray ionization) tandem mass spectrometry (LC-(ESI) MS/MS) was developed and validated for environmental water samples. Good apparent recoveries (41-80%), detection limits (1-50 ng L(-1)), repeatability (%RSD<15%, n=5) and reproducibility (%RSD<18%, n=5) were achieved.

  7. Carboxylated graphene oxide/polyvinyl chloride as solid-phase extraction sorbent combined with ion chromatography for the determination of sulfonamides in cosmetics.

    Science.gov (United States)

    Zhong, Zhixiong; Li, Gongke; Luo, Zhibin; Liu, Zhe; Shao, Yijuan; He, Wanwen; Deng, Jianchao; Luo, Xingling

    2015-08-12

    A carboxylated graphene oxide/polyvinyl chloride (CGO/PVC) material was prepared as a sorbent for the selective extraction of sulphonamides from complex sample. After being dispersed in buffer solution, sample was transferred into the prefabricated solid-phase extraction (SPE) column, which integrated extraction and cleanup into one single-step. A multi-response optimization based on the Box-Behnken design was used to optimize factors affecting extraction efficiency. Compared with the commonly commercial sorbents including MCX, WCX and C18, CGO/PVC hybrid material had higher extraction selectivity and capacity to sulphonamides. The limits of detection and quantification for seven target compounds were in the range of 3.4-7.1 μg/L and 11.4-23.7 μg/L, respectively. The self-assembly SPE cartridge was successfully used to enrich seven analytes in anti-acne cosmetics prior to ion chromatography detection with good recoveries of 87.8-102.0% and relative standard deviations of 1.2-6.4%, implying that this method was suitable for routine analysis of cosmetics. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. Development of Novel Porous Sorbents for Extraction of Uranium from Seawater

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Wenbin [Univ. of Chicago, IL (United States)

    2017-05-25

    Climate disruption is one of the greatest crises the global community faces in the 21st century. Alarming increases in CO2, NO, SO2 and particulate matter levels will have catastrophic consequences on the environment, food supplies, and human health if no action is taken to lessen their worldwide prevalence. Nuclear energy remains the only mature technology capable of continuous base-load power generation with ultralow carbon dioxide, nitric oxide, and sulfur dioxide emissions. Over the lifetime of the technology, nuclear energy outputs less than 1.5% the carbon dioxide emissions per gigawatt hour relative to coal—about as much as onshore wind power.1 However, in order for nuclear energy to be considered a viable option in the future, a stable supply of uranium must be secured. Current estimates suggest there is less than 100 years’ worth of uranium left in terrestrial ores (6.3 million tons) if current consumption levels remain unchanged.2 It is likely, however, that demand for nuclear fuel will rise as a direct consequence of the ratification of global climate accords. The oceans, containing approximately 4.5 billion tons of uranium (U) at a uniform concentration of ~3 ppb, represent a virtually limitless supply of this resource.3 Development of technologies to recover uranium from seawater would greatly improve the U resource availability, providing a U price ceiling for the current generation and sustaining the nuclear fuel supply for future generations. Several methods have been previously evaluated for uranium sequestration including solvent extraction, ion exchange, flotation, biomass collection, and adsorption; however, none have been found to be suitable for reasons including cost effectiveness, long term stability, and selectivity.4,5 While polymer beads and fibers have been functionalized with amidoxime functional groups to afford U adsorption capacities as high as 1.5 g U/kg,6 further discoveries are needed to make uranium

  9. On-line Ultrasound-Assisted Dispersive Micro-Solid-Phase Extraction Based on Amino Bimodal Mesoporous Silica Nanoparticles for the Preconcentration and Determination of Cadmium in Human Biological Samples.

    Science.gov (United States)

    Shirkhanloo, H; Falahnejad, M; Zavvar Mousavi, H

    2016-06-01

    On-line ultrasound-assisted dispersive micro-solid-phase extraction (USA-DμSPE) has been developed for preconcentration and separation of trace amounts of Cd(II) ions in 0.5 mL of human biological samples. In a syringe with a nylon membrane, new synthetic bulky amino bimodal mesoporous silica nanoparticles (NH2-UVM7) were dispersed as a nanoadsorbent in 5 mL of diluted serum sample (1:10), and after ultrasonic shaking, the liquid phase was separated from the solid phase. At the optimized pH, the chemical and physical adsorption of cadmium ions occurred, respectively, based on complexation with amine groups of UVM7 (Cd:NH2-UVM7) and silica nanoparticles. The analyte was then back-extracted from the sorbent with nitric acid solution (0.2 M), and its concentration was determined by electrothermal atomic absorption spectrometry (ETAAS). Under the optimized conditions, the linear range, limit of detection (LOD), and preconcentration factor (PF) were obtained as 0.01-0.56 μg L(-1), 0.002 μg L(-1), and 25, respectively. The adsorption capacity of NH2-UVM7 was found to be 108.6 mg g(-1) of cadmium. The validation of the methodology was performed by the human standard reference material (HSRM).

  10. Evaluation of magnetic nanoparticles to serve as solid-phase extraction sorbents for the determination of endocrine disruptors in milk samples by gas chromatography mass spectrometry.

    Science.gov (United States)

    Synaridou, Maria-Evangelia S; Sakkas, Vasilios A; Stalikas, Constantine D; Albanis, Triantafyllos A

    2014-06-27

    A rapid magnetic solid-phase extraction (MSPE) is proposed based on C18-functionalized magnetic silica nanoparticles as sorbents, for the determination of endocrine disruptors - 20 organochlorine pesticides and 6 polychlorinated biphenyls - in milk samples. Magnetic nanoparticles are characterized by several techniques, such as Scanning Electron Microscopy, X-Ray diffraction, Brunauer-Emmett-Teller and Fourier transform-infrared. The MSPE is performed by dispersion of the Fe3O4@SiO2@C18 nanoparticles in milk samples with sonication, after protein precipitation. Then, the sorbent is collected by applying an external magnetic field and the analytes are desorbed by n-hexane. Several parameters affecting the extraction efficiency of target analytes by the magnetic nanoparticles are investigated, including washing and elution solvents, amount of sorbents, time of extraction and elution, sample and elution solvent volume. The proposed method is optimized by means of experimental design and response surface methodology. When coupled with gas chromatography-mass spectrometry detection and under optimum extraction conditions, average recoveries of target analytes are found to be in the range of 79% to 116%. The proposed MSPE-GC-MS analytical method has a linear calibration curve for all target analytes with coefficients of determination to range from 0.9950 to 0.9999. The limits of quantification are found to be between 0.2 and 1μg/L ensuring compliance with the maximum residue limits established by European Commission and Codex Alimentarius, for OCPs and PCBs residues in milk. The proposed method is applied to the determination of target analytes in milk samples from local markets.

  11. The selective cleanup of complex matrices and simultaneous separation of benzo[a]pyrene by solid-phase extraction with MgO microspheres as sorbents.

    Science.gov (United States)

    Jin, Jing; Li, Yun; Zhang, Zhiping; Su, Fan; Qi, Peipei; Lu, Xianbo; Chen, Jiping

    2011-12-23

    A new method for the selective cleanup of complex matrices and simultaneous separation of benzo[a]pyrene (BaP) was developed in this study. This method was based on solid-phase extraction (SPE) using magnesium oxide microspheres as sorbents, and it eliminated interferences from various impurities, such as lipids, sulphur, pigments, halobenzenes, polychlorodibenzo-p-dioxins and polychlorodibenzofurans. Several parameters, including the volume of rinsing and eluting solvents, the type of loading solvents and SPE sorbents, were optimized systematically. The capability for impurity removal was verified by gel permeation chromatography, gas chromatography, and liquid chromatography. Compared to commercial sorbents (silica gel, florisil and alumina), MgO microspheres exhibited excellent performance in the selective isolation of BaP and removal of impurities. The proposed method was applied to detect BaP in complex samples (sediments, soils, fish, and porcine liver). The limit of quantification (LOQ) was 1.04 ngL(-1), and the resulting regression coefficient (r(2)) was greater than 0.999 over a broad concentration range (9.5-7600 ngL(-1)). In contrast to traditional methods, the proposed method can give rise to higher recovery (85.1-100.8%) and better selectivity with simpler operation and less consumption of organic solvents (20-40 mL).

  12. Single "click" synthesis of a mixed-mode silica sorbent and application in matrix solid-phase dispersion extraction of β-agonists from porcine liver.

    Science.gov (United States)

    Zhu, Yuling; Yang, Siwen; Chen, Gang; Xing, Jun

    2014-08-08

    A single "click" strategy is proposed for the preparation of a reversed-phase/weak cation-exchange mixed-mode silica-based sorbent (silica-WCX). Upon this strategy, both 1-dodecyne and 5-hexynoic acid were simultaneously immobilized onto azide-silica in varied ratio via Cu (I)-catalyzed azide-alkyne cycloaddition click reaction. The chemical compositions of silica-WCXs were characterized by elemental analysis, acid-base titration and Fourier transform-infrared spectroscopy. The results indicated that the actual mole ratio of n-dodecyl to carboxylic group on the sorbent is almost the same as the reactant ratio of 1-dodecyne to 5-hexynoic acid, and the repeatability of synthesis method is good. After that, two β-agonists, clenbuterol and ractopamine, were selected as model drug residues to evaluate the applicability of silica-WCX in matrix solid-phase dispersion extraction for the determination of basic drug residues in porcine liver by HPLC/UV. In comparison with some commercial sorbents, silica-WCX exhibited higher recoveries and better purification capability. Under the optimized conditions, linearity ranges were between 0.04 and 8.0μg/g for both analytes with coefficients of determination (R(2)) higher than 0.9997. The average recoveries at three spiked levels ranged from 92.5% to 105.0% with RSDs less than 6.6%.

  13. Development of an on-line high performance liquid chromatography detection system for human cytochrome P450 1A2 inhibitors in extracts of natural products

    NARCIS (Netherlands)

    Jeurissen, S.M.F.; Claassen, F.W.; Havlik, J.; Bouwmans, E.E.; Cnubben, N.H.P.; Sudhölter, E.J.R.; Rietjens, I.M.C.M.; Beek, T.A. van

    2007-01-01

    An on-line HPLC screening method for detection of inhibitors of human cytochrome P450 1A2 in extracts was developed. HPLC separation of extracts is connected to a continuous methoxyresorufin-O-demethylation (MROD) assay in which recombinant human P450 1A2 converts methoxyresorufin to its fluorescent

  14. Developing qualitative extraction profiles of coffee aromas utilizing polymeric ionic liquid sorbent coatings in headspace solid-phase microextraction gas chromatography-mass spectrometry.

    Science.gov (United States)

    López-Darias, Jessica; Anderson, Jared L; Pino, Verónica; Afonso, Ana M

    2011-11-01

    Two solid-phase microextraction (SPME) sorbent coatings based on polymeric ionic liquids (PILs) have been utilized for the analysis of complex coffee aroma samples. The PIL-based SPME coatings examined, namely, poly(1-(4-vinylbenzyl)-3-hexadecylimidazolium bis[(trifluoromethyl)sulfonyl]imide) [poly(VBHDIm(+) NTf(2)(-))], with ~14-μm thickness, and poly(1-vinyl-3-hexylimidazolium chloride) [poly(ViHIm(+)Cl(-))], with ~8-μm thickness, were employed for the headspace determination of up to 49 analytes from four different coffee beans: two French roast coffees of different brands, Sumatra coffee, and decaffeinated Sumatra coffee. The analysis was conducted using gas chromatography coupled to mass spectrometry. For comparative purposes, the commercial polyacrylate (PA, 85-μm film thickness) SPME coating was utilized under the same extraction conditions. The three SPME coatings tested behaved quite differently as a function of the families of compounds extracted. Thus, the poly(VBHDIm(+) NTf(2)(-) ) coating was extremely selective for aldehydes while also exhibiting good extraction efficiencies for acids. The poly-(ViHIm(+) Cl(-)) coating exhibited superior performance for aromatic alcohols, and the PA coating worked better for heterocyclic aromatics. Both PIL-based SPME sorbent coatings demonstrated exceptional selectivity and extraction efficiency when dealing with complex coffee aromas in spite of their small film thicknesses.

  15. Microextraction by packed sorbent and salting-out-assisted liquid-liquid extraction for the determination of aromatic amines formed from azo dyes in textiles.

    Science.gov (United States)

    Sánchez, Miguel del Nogal; Santos, Patricia Martín; Sappó, Cristina Pérez; Pavón, José Luis Pérez; Cordero, Bernardo Moreno

    2014-02-01

    EU legislation prohibits the use of certain azo dyes which, on reduction, form any of 22 aromatic amines listed in Regulation (EC) 1907/2006 at concentrations above the threshold limit of 30 mg Kg(-1). Two different extraction techniques for the determination of aromatic amines formed from azo dyes in textiles in combination with gas chromatography-mass spectrometry (GC-MS) are described. The first one is based on microextraction by packed sorbent (MEPS) and the other approach involves salting-out-assisted liquid-liquid extraction (SALLE). The influence of several parameters on the efficiency of the extraction using MEPS (sorbent material, sample volume, elution solvent, elution volume and washing steps, among others) and SALLE (extraction volume and amount of salt) were investigated. In addition, chromatographic separation was optimized and quadrupole mass spectrometry was evaluated using the synchronous SIM/scan data acquisition mode. The repeatability (n=8, S/N=3) of the methods, calculated as the relative standard deviation (RSD) was below 15 and 11% for all compounds when MEPS and SALLE were used, respectively. Standard additions procedure was used to quantify the aromatic amines in the textil samples. The detection limits in the samples for both methods were lower than the maximum value allowed by legislation. The results obtained in the analysis of textiles revealed the presence of o-anisidine, p-chloroaniline, 4-chloro-o-toluidine, 2-naphthylamine and 3,3'-dimethoxybenzidine in some of them. © 2013 Elsevier B.V. All rights reserved.

  16. Polyimide-coated magnetic nanoparticles as a sorbent in the solid-phase extraction of polycyclic aromatic hydrocarbons in seawater samples.

    Science.gov (United States)

    Mehdinia, Ali; Haddad, Hosein; Mozaffari, Shahla

    2016-09-01

    Magnetic polyimide poly(4,4'-oxydiphenylene-pyromellitimide) nanoparticles were successfully synthesized and developed for the solid-phase extraction of polycyclic aromatic hydrocarbons in seawater samples. The aromatic rings of polyimide coating provided a good adsorption capacity (28.3-42.5 mg/g) for polycyclic aromatic hydrocarbons because of the π-π stacking interaction. The developed method was used as a simple, fast, and efficient extraction and preconcentration technique for the trace analysis of polycyclic aromatic hydrocarbons. The high chemical, physical and thermal stability, excellent reusability, and good magnetic properties are the merits of the sorbent. High preconcentration factors (41-63) were obtained. The sorbent was also characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, energy dispersive X-ray spectrometry, transmission electron microscopy, and vibrating sample magnetometry. After optimizing several appropriate extraction parameters, the results indicated that the extraction recoveries of polycyclic aromatic hydrocarbons were in the range of 61.6-94.7%, with relative standard deviations between 2.9 and 5.4%, the calibration graph was linear in the concentration range of 1-100 μg/L (r > 0.9991) with limit of detection in the range of 0.15-0.19 μg/L (n = 3). Seawater samples were analyzed as real samples and good recoveries (68.5-99.5%) were obtained at different spiked values.

  17. Accelerated solvent extraction followed by on-line solid-phase extraction coupled to ion trap LC/MS/MS for analysis of benzalkonium chlorides in sediment samples

    Science.gov (United States)

    Ferrer, I.; Furlong, E.T.

    2002-01-01

    Benzalkonium chlorides (BACs) were successfully extracted from sediment samples using a new methodology based on accelerated solvent extraction (ASE) followed by an on-line cleanup step. The BACs were detected by liquid chromatography/ion trap mass spectrometry (LC/MS) or tandem mass spectrometry (MS/MS) using an electrospray interface operated in the positive ion mode. This methodology combines the high efficiency of extraction provided by a pressurized fluid and the high sensitivity offered by the ion trap MS/MS. The effects of solvent type and ASE operational variables, such as temperature and pressure, were evaluated. After optimization, a mixture of acetonitrile/water (6:4 or 7:3) was found to be most efficient for extracting BACs from the sediment samples. Extraction recoveries ranged from 95 to 105% for C12 and C14 homologues, respectively. Total method recoveries from fortified sediment samples, using a cleanup step followed by ASE, were 85% for C12BAC and 79% for C14-BAC. The methodology developed in this work provides detection limits in the subnanogram per gram range. Concentrations of BAC homologues ranged from 22 to 206 ??g/kg in sediment samples from different river sites downstream from wastewater treatment plants. The high affinity of BACs for soil suggests that BACs preferentially concentrate in sediment rather than in water.

  18. [Determination of tris (2-chloroethyl) phosphate in leather by gas chromatography-mass spectrometry coupled with mixed-mode sorbent solid phase extraction].

    Science.gov (United States)

    Zhang, Weiya; Zhu, Yuling; Wang, Chengyun; Li, Lixia; Zhang, Junqing; Xing, Jun

    2014-10-01

    Leather is one of the important exporting products to European Union (EU), and tris(2-chloroethyl) phosphate (TCEP) is a commonly used flame retardant in leather and leather products. Recently, TCEP has been classified as a kind of substance of very high concern (SVHC) by EU for its carcinogenicity and reproductive toxicity. But to date, there is not a recognized method for the determination of TCEP in leather and leather products due to the serious matrix interferences and relatively low recovery of TCEP. In this work, a home-made mixed-mode sorbent (Silica-WCX) with carboxyl and alkyl groups was tested as the sorbent of solid phase extraction (SPE) to extract TECP from leather. The results demonstrated that, making the carboxyl groups protonized under acidic condition, Silica-WCX exhibited better extraction performance towards TCEP over some frequently used commercial sorbents tested. After the optimization of the SPE conditions based on Silica-WCX, a method of gas chromatography/mass spectrometry (GC-MS) was established for the determination of TCEP in leather samples. The linear range for TCEP ranged from 0.10 to 100.0 μg/L and the limit of quantification (LOQ, S/N = 10) was 44.46 ng/kg. The recoveries of TCEP spiked in samples at varied levels were in the range of 91.45%-99.98% with the relative standard deviations (RSDs) of 4.33%-5.97%. The method is simple, sensitive and reliable for the analysis of TCEP in leather and leather products.

  19. 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

  20. Dispersive micro-solid-phase extraction of benzoylurea insecticides in honey samples with a β-cyclodextrin-modified attapulgite composite as sorbent.

    Science.gov (United States)

    Zhang, Panjie; Cui, Xiangqian; Yang, Xiaoling; Zhang, Sanbing; Zhou, Wenfeng; Gao, Haixiang; Lu, Runhua

    2016-01-01

    A β-cyclodextrin-modified attapulgite composite was prepared and used as a dispersive micro-solid-phase extraction sorbent for the determination of benzoylurea insecticides in honey samples. Parameters that may influence the extraction efficiency, such as the type and volume of the eluent, the amount of the sorbent, the extraction time and the ionic strength were investigated and optimized using batch and column procedures. Under optimized conditions, good linearity was obtained for all of the tested compounds, with R(2) values of at least 0.9834. The limits of detection were determined in the range of 0.2-1.0 μg/L. The recoveries of the four benzoylurea insecticides in vitex honey and acacia honey increased from 15.2 to 81.4% and from 14.2 to 82.0%, respectively. Although the β-cyclodextrin-modified attapulgite composite did not show a brilliant adsorption capacity for the selected benzoylurea insecticides, it exhibited a higher adsorption capacity toward relatively hydrophobic compounds, such as chlorfluazuron and hexaflumuron (recoveries in vitex honey samples ranged from 70.0 to 81.4% with a precision of 1.0-3.7%). It seemed that the logPow of the benzoylurea insecticides is related to their recoveries. The results confirmed the possibility of using cyclodextrin-modified palygorskite in the determination of relatively hydrophobic trace pharmaceutical residues. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Determination of trace acrylamide in starchy foodstuffs by HPLC using a novel mixed-mode functionalized calixarene sorbent for solid-phase extraction cleanup.

    Science.gov (United States)

    Zhang, Wenfen; Deng, Zhifen; Zhao, Wenjie; Guo, Ling; Tang, Wei; Du, Huifang; Lin, Lin; Jiang, Qiong; Yu, Ajuan; He, Lijun; Zhang, Shusheng

    2014-07-01

    In this paper, a rapid and effective HPLC method, using tetraazacalix[2]arene[2]triazine-modified silica gel (NCSi) as solid-phase extraction (SPE) sorbent, was developed for the purification and determination of trace acrylamide in starchy foodstuffs. The main influence factors of SPE including amount of NCSi sorbent, sample flow rate, and volume and composition of washing solution were investigated and evaluated in the sample pretreatment step. The optimized purification effect was achieved at the sample flow rate of 3 mL/min with 100 mg of NCSi and 2 mL of washing solution (water, 100%). The HPLC separation was carried out on a C18 column (250×4.6 mm i.d., 5 μm) with a mobile phase of methanol/water (10:90, v/v). The linear range of the calibration curve was 4-4000 ng/mL with s correlation coefficient of >0.9999. The intraday and interday RSDs (n=5) of peak areas of acrylamide were 0.22 and 0.90% and the intraday and interday RSDs (n=5) of retention times were 0.50 and 1.63%, respectively. In addition, overall recoveries through the extraction and NCSi-SPE purification ranged from 73.13 to 98%. Compared with the commercial SPE sorbents, NCSi featured excellent selectivity to retain polar and nonpolar interferences in the sample matrices. The improved method was simple, rapid, accurate, and promising for the determination of trace acrylamide in starchy foods with a complex matrix.

  2. Synthesis and application of multi-walled carbon nanotubes-molecularly imprinted sol-gel composite material for on-line solid-phase extraction and high-performance liquid chromatography determination of trace Sudan IV

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Zhaohui, E-mail: zhaohuizhang77@hotmail.com [College of Chemistry and Chemical Engineering, Jishou University, Jishou 416000 (China); State Key Laboratory of Chemo/Biosensing and Chemometrics, Hunan University, Changsha 410082 (China); Zhang Huabin; Hu Yufang [College of Chemistry and Chemical Engineering, Jishou University, Jishou 416000 (China); Yao Shouzhuo [State Key Laboratory of Chemo/Biosensing and Chemometrics, Hunan University, Changsha 410082 (China)

    2010-02-28

    A novel composite material of multi-walled carbon nanotubes (MWNTs)-Sudan IV molecularly imprinted polymers (MIPs) was prepared by surface molecular imprinting technique in combination with sol-gel technology. The MWNTs-MIPs were evaluated by scanning electron micrograph (SEM), Fourier transform infrared spectroscopy (FT-IR), and adsorption experiments. The results showed that the MWNTs-MIPs exhibited good selective recognition to Sudan IV. The maximum saturated binding capacity (Q{sub max}) is 63.2 {mu}mol g{sup -1}. Applied as sorbent, the MWNTs-MIPs were used for the determination of trace Sudan IV in chilli powder by on-line solid-phase extraction-high-performance liquid chromatography (SPE-HPLC). The results showed that an enrichment factor of 741 was achieved with a loading flow rate of 1.0 mL min{sup -1} for sampling 50 mL. The MWNTs-MIPs provided a fast and convenience determination platform for Sudan IV in real samples.

  3. Dispersive micro-solid phase extraction of aromatic amines based on an efficient sorbent made from poly(1,8-diaminonaphtalen) and magnetic multiwalled carbon nanotubes composite.

    Science.gov (United States)

    Jalilian, Niloofar; Ebrahimzadeh, Homeira; Asgharinezhad, Ali Akbar

    2017-05-26

    In this work, the extraction of aromatic amines with an efficient magnetic multiwalled carbon nanotubes/Fe3O4@Poly(1,8-diaminonaphtalen) (MWCNTs/Fe3O4@PDAN) composite followed by HPLC-DAD was presented. Imprimis, the comparison among different magnetic nanosorbents including Fe3O4, MWCNTs/Fe3O4, Fe3O4@PDAN and MWCNTs/Fe3O4@PDAN was conducted. The obtained results, exhibited that the MWCNTs/Fe3O4@PDAN composite has the highest extraction efficiency for target analytes (3-nitroaniline, 4-chloroaniline, 4-bromoaniline and 3,4-dichloroaniline). This sorbent was characterized by Fourier transform infrared spectroscopy, X-ray dispersive spectroscopy, thermogravimetry analysis, scanning electron microscopy, transition electron microscopy, vibrating sample magnetometry and X-ray diffraction. Design of experiment approach was applied to find out the optimal experimental conditions. The optimal extraction conditions were: pH of the sample, 10; sorbent amount, 10mg; sorption time, 15min; salt concentration, 10% w/w; type and volume of the eluent, 0.01molL(-1) HCl in acetonitrile, 145μL; elution time; 2min. Under the optimal extraction conditions detection limits and linear dynamic ranges were achieved in the range of 0.1-0.25μgL(-1) and 0.25-500μgL(-1), respectively. The percent of extraction recovery and relative standard deviations (n=5) were in the range of 31.2-82.8% and 3.4-5.6%, respectively. Finally, the applicability of the method was successfully confirmed by the extraction and determination of target analytes in various water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Fluorescence method using on-line sodium cholate coacervate surfactant mediated extraction for the flow injections analysis of Rhodamine B.

    Science.gov (United States)

    Acosta, Gimena; Talio, María C; Luconi, Marta O; Hinze, Willie L; Fernández, Liliana P

    2014-11-01

    An on-line surfactant mediated extraction method in a flow injection analysis format with fluorescence detection was developed for the determination of Rhodamine B (RhB) in food condiments. The sample was extracted using the phase separation behavior exhibited by the bile salt surfactant, sodium cholate (NaC), upon addition of sodium dodecylsulfate (SDS) in the presence of acid at room temperature. The RhB in the sample was incorporated into the NaC/SDS coacervate phase which was then collected on a glass-wool packed mini column from which it was subsequently eluted using a 1.00 mol L(-1) HCl solution. The inherent fluorescence (λex=555 nm; λem=575 nm) of RhB was employed for detection. Good linearity (r(2)=0.9933) was obtained over the concentration range 0.4-4794-479.0 µg L(-1) RhB. The detection (LOD) and quantification (LOQ) limits were 0.12 and 0.40 µg L(-1), respectively. The method was successfully applied for analysis of RhB in food condiments and spiked samples. The average recoveries ranged from 95.3% to 118.9% at spiked concentration levels of 1.19 and 2.39 µg L(-1). Under optimized conditions, a throughput of 50 samples per hour was achieved. The proposed method may be a valuable tool not only for quality control of food condiments and similar food confectioneries but for the analysis of a variety of other RhB-containing samples as well.

  5. Flow injection on-line solid phase extraction for ultra-trace lead screening with hydride generation atomic fluorescence spectrometry.

    Science.gov (United States)

    Wan, Zhuo; Xu, Zhangrun; Wang, Jianhua

    2006-01-01

    A flow injection (FI) on-line solid phase extraction (SPE) procedure for ultra-trace lead separation and preconcentration was developed, followed by hydride generation and atomic fluorescence spectrometric (AFS) detection. Lead is retained on an iminodiacetate chelating resin packed microcolumn, and is afterward eluted with 2.5% (v/v) hydrochloric acid to facilitate the hydride generation by reaction with alkaline tetrahydroborate solution with 1% (m/v) potassium ferricyanide as an oxidizing (or sensitizing) reagent. The hydride was separated from the reaction medium in the gas-liquid separator and swept into the atomizer for quantification. The chemical variables and the FI flow parameters were carefully optimized. With a sample loading volume of 4.8 ml, quantitative retention of lead was obtained, along with an enrichment factor of 11.3 and a sampling frequency of 50 h(-1). A detection limit of 4 ng l(-1), defined as 3 times the blank standard deviation (3 sigma), was achieved along with a RSD value of 1.6% at the 0.4 microg l(-1) level. The procedure was validated by determining lead contents in two certified reference materials, and its practical applicability was further demonstrated by analysing a variety of biological and environmental samples.

  6. Ultrasound-assisted ionic liquid-based micellar extraction combined with microcrystalline cellulose as sorbent in dispersive microextraction for the determination of phenolic compounds in propolis.

    Science.gov (United States)

    Cao, Jun; Peng, Li-Qing; Du, Li-Jing; Zhang, Qi-Dong; Xu, Jing-Jing

    2017-04-22

    An ionic liquid-(IL) based micellar extraction combined with microcrystalline cellulose- (MCC) assisted dispersive micro solid-phase extraction method was developed to extract phenolic compounds from propolis. A total of 20 target compounds were identified by ultra-high- performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry. The main extraction parameters were optimized and included the ultrasonic power, ultrasonic time, sample pH, type of IL, the concentration of [C12mim]Br, extraction time, concentration of MCC, type of sorbent and type of elution solvents. Under the optimum conditions, the proposed method exhibited good linearities (r(2) ≥ 0.999) for all plant phenolic compounds with the lower limits of detection in the range of 0.21-0.41 ng/mL. The recoveries ranged from 82.74% to 97.88% for pinocembrin, chrysin and galangin. Compared with conventional solvent extraction, the present method was simpler and more efficient and required less organic solvent and a shorter extraction time. Finally, the methodology was successfully used for the extraction and enrichment of phenolic compounds in propolis. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Automatic On-line Solid-phase Extraction-Electrothermal Atomic Absorption Spectrometry Exploiting Sequential Injection Analysis for Trace Vanadium, Cadmium and Lead Determination in Human Urine Samples.

    Science.gov (United States)

    Giakisikli, Georgia; Ayala Quezada, Alejandro; Tanaka, Junpei; Anthemidis, Aristidis N; Murakami, Hiroya; Teshima, Norio; Sakai, Tadao

    2015-01-01

    A fully automated sequential injection column preconcentration method for the on-line determination of trace vanadium, cadmium and lead in urine samples was successfully developed, utilizing electrothermal atomic absorption spectrometry (ETAAS). Polyamino-polycarboxylic acid chelating resin (Nobias chelate PA-1) packed into a handmade minicolumn was used as a sorbent material. Effective on-line retention of chelate complexes of analytes was achieved at pH 6.0, while the highest elution effectiveness was observed with 1.0 mol L(-1) HNO3 in the reverse phase. Several analytical parameters, like the sample acidity, concentration and volume of the eluent as well as the loading/elution flow rates, have been studied, regarding the efficiency of the method, providing appropriate conditions for the analysis of real samples. For a 4.5 mL sample volume, the sampling frequency was 27 h(-1). The detection limits were found to be 3.0, 0.06 and 2.0 ng L(-1) for V(V), Cd(II) and Pb(II), respectively, with the relative standard deviations ranging between 1.9 - 3.7%. The accuracy of the proposed method was evaluated by analyzing a certified reference material (Seronorm(TM) trace elements urine) and spiked urine samples.

  8. Data correlation in on-line solid-phase extraction-gas chromatography-atomic emission/mass spectrometric detection of unknown microcontaminants

    NARCIS (Netherlands)

    Hankemeier, Th.; Rozenbrand, J.; Abhadur, M.; Vreuls, J.J.; Brinkman, U.A.Th.

    1998-01-01

    A procedure is described for the (non-target) screening of hetero-atom-containing compounds in tap and waste water by correlating data obtained by gas chromatography (GC) using atomic emission (AED) and mass selective (MS) detection. Solid-phase extraction (SPE) was coupled on-line to both GC system

  9. Selective extraction of CO2 from simulated flue gas using polymeric ionic liquid sorbent coatings in solid-phase microextraction gas chromatography.

    Science.gov (United States)

    Zhao, Qichao; Anderson, Jared L

    2010-07-02

    The CO2 selectivity of two polymeric task-specific ionic liquid sorbent coatings, poly(1-vinyl-3-hexylimidazolium) bis[(trifluoromethyl)sulfonyl]imide [poly(VHIM-NTf2)] and poly(1-vinyl-3-hexylimidazolium) taurate [poly(VHIM-taurate)], was examined using solid-phase microextraction (SPME) for the determination of CO2 in simulated flue gas. For comparison purposes, a commercial SPME fiber, Carboxen-PDMS, was also studied. A study into the effect of humidity revealed that the poly(VHIM-taurate) fiber exhibited enhanced resistance to water, presumably due to the unique mechanism of CO2 capture. The effect of temperature on the performance of the PIL-based and Carboxen fibers was examined by generating calibration curves under various temperatures. The sensitivity, linearity, and linear range of the three fibers were evaluated. The extraction of CH4 and N2 was performed and the selectivities of the PIL-based and Carboxen fibers were compared. The poly(VHIM-NTf2) fiber was found to possess superior CO2/CH4 and CO2/N2 selectivities compared to the Carboxen fiber, despite the smaller film thicknesses of the PIL-based fibers. A scanning electron microscopy study suggests that the amine group of the poly(VHIM-taurate) is capable of selectively reacting with CO2 but not CH4 or N2, resulting in a significant surface morphology change of the sorbent coating.

  10. On-cartridge derivatisation using a calixarene solid-phase extraction sorbent for facile, sensitive and fast determination of formaldehyde in beer.

    Science.gov (United States)

    Deng, Zhifen; Hu, Kai; Zhang, Yongming; Zhao, Wenjie; Wang, Fei; Guo, Ling; Zhang, Wenfen; He, Juan; Huang, Yanjie; Zhang, Shusheng

    2016-11-15

    This work demonstrates the successful application of an on-cartridge derivatisation procedure for facile, fast and sensitive determination of formaldehyde in beer by HPLC-UV. The derivatisation and solid-phase extraction (SPE) were integrated into a novel calixarene SPE sorbent: tetraazacalix[2]arene[2]triazine bonded silica gel. Specifically, 2,4-dinitrophenylhydrazine was adsorbed onto the sorbent in advance, based on the charge-transfer interaction between the macrocyclic molecule and nitrobenzenes. The method was optimised and validated: under the optimal conditions of derivatisation, SPE and HPLC separation, good linearity was obtained in the range of 0.080-3.2μgmL(-1) with a correlation coefficient of 0.9939, the limit of detection was 3.0ngmL(-1) (S/N=3), the limit of quantification was 10ngmL(-1) (S/N=10), and the recovery level using this method was desirable at 75-84%. The developed method was successfully applied to determine formaldehyde content in real beer samples; the results were in the range of 0.11-1.1μgmL(-1).

  11. An On-Line Solid Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry Method for the Determination of Perfluoroalkyl Acids in Drinking and Surface Waters

    Directory of Open Access Journals (Sweden)

    Michela Mazzoni

    2015-01-01

    Full Text Available An UHPLC-MS/MS multiresidue method based on an on-line solid phase extraction (SPE procedure was developed for the simultaneous determination of 9 perfluorinated carboxylates (from 4 to 12 carbon atoms and 3 perfluorinated sulphonates (from 4 to 8 carbon atoms. This work proposes using an on-line solid phase extraction before chromatographic separation and analysis to replace traditional methods of off-line SPE before direct injection to LC-MS/MS. Manual sample preparation was reduced to sample centrifugation and acidification, thus eliminating several procedural errors and significantly reducing time-consuming and costs. Ionization suppression between target perfluorinated analytes and their coeluting SIL-IS were detected for homologues with a number of carbon atoms less than 9, but the quantitation was not affected. Total matrix effect corrected by SIL-IS, inclusive of extraction efficacy, and of ionization efficiency, ranged between −34 and +39%. The percentage of recoveries, between 76 and 134%, calculated in different matrices (tap water and rivers impacted by different pollutions was generally satisfactory. LODs and LOQs of this on-line SPE method, which also incorporate recovery losses, ranged from 0.2 to 5.0 ng/L and from 1 to 20 ng/L, respectively. Validated on-line SPE-LC/MS/MS method has been applied in a wide survey for the determination of perfluoroalkyl acids in Italian surface and ground waters.

  12. Utilizing a novel sorbent in the solid phase extraction for simultaneous determination of 15 pesticide residues in green tea by GC/MS.

    Science.gov (United States)

    Huo, Feifei; Tang, Hua; Wu, Xue; Chen, Dazhou; Zhao, Tan; Liu, Pei; Li, Lei

    2016-06-15

    Pesticide residues exceeding standard in green tea is a widespread problem of the world's attention, containing organochlorine pesticides (OCPs), organophosphorus pesticides (OPPs), and pyrethroids. In this research, three dimensionally honeycomb Mg-Al layered double oxide (TDH-Mg-Al-LDO) combined with graphitized carbon black (GCB), packed as a column, was used as a novel solid phase extraction sorbent, applying in simultaneous determination of 15 pesticide residues in green tea coupled with GC-MS. Compared with different type of SPE column, it showed that TDH-Mg-Al-LDO exhibited great advantages in the extraction of 15 pesticide residues from green tea, which was seldom reported before. Different experiment conditions, such as combination order of Mg-Al-LDO and GCB, dosage of sorbents, type and volume of eluting solvent were thoroughly studied and optimized. The limits of detection (LODs) of 15 pesticides ranged from 0.9 to 24.2ng/g and the limits of quantifications (LOQs) were ranging from 3.0 to 80.0ng/g. The recoveries using this method at three spiked concentration levels (10, 100 and 500ng/g for Fenthion, P,P'-DDE, O,P'-DDT, P,P'-DDD and Bifenthrin, 100, 500 and 2000ng/g for the others) range from 71.1 to 119.0%. The relative standard deviation (RSD) was from 0.1 to 7.6% in all case. The result indicated that the proposed analytical method had been successfully applied for the simultaneous determination of 15 pesticide residues in commercial green tea.

  13. Graphene-derivatized silica as an efficient solid-phase extraction sorbent for pre-concentration of fluoroquinolones from water followed by liquid-chromatography fluorescence detection.

    Science.gov (United States)

    Speltini, Andrea; Sturini, Michela; Maraschi, Federica; Consoli, Luana; Zeffiro, Alberto; Profumo, Antonella

    2015-01-30

    This work presents a novel analytical method based on graphene for the determination of five widely used fluoroquinolones (FQs) in aqueous matrices. The procedure entails solid-phase extraction (SPE) on graphene-derivatized silica (200mg), followed by liquid chromatography with fluorescence detection. Monolayer graphene oxide (GO) flakes were covalently bonded onto aminopropyl silica microparticles, and then treated with aqueous hydrazine to obtain the reduced GO (RGO). The final material (RGO-silica) was characterized by thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and BET analysis, and for the first time evaluated as mixed-mode sorbent for the SPE of FQs from natural waters. Accuracy was studied on tap/raw river water in the concentration range 5-10,000ngL(-1), obtaining mean absolute recoveries from 72 to 118%. The inter-day precision was good, showing relative standard deviations (RSDs) in the range 5-15%. Sample volumes up to 1L provided enrichment factors up to 1000, achieving accurate quantification of concentrations as low as 5ngL(-1). The analytes were simultaneously and quantitatively eluted from the RGO-silica cartridge in a single fraction by using acetonitrile combined with aqueous tetrabutyl ammonium hydroxide. The batch-to-batch reproducibility was verified on three independently prepared RGO-silica samples. RGO-silica was advantageous in terms of adsorption capacity and reusability with respect to commercial sorbents; the cartridge proved to be reusable for at least 10 consecutive extractions, with no significant loss of efficiency (recovery >70%). The analytical procedure was applied to the determination of FQs in actual environmental waters.

  14. Utilizing a nano-sorbent for the selective solid-phase extraction of vanillic acid prior to its determination by photoluminescence spectroscopy.

    Science.gov (United States)

    Abdolmohammad-Zadeh, Hossein; Mahmoudi-Kordi, Fatemeh; Rahmati, Manoochehr

    2014-12-01

    Vanillic acid (VA) is a phenolic acid, and acts as a natural antioxidant in fruits, vegetables and plants. The extraction and determination of trace levels of VA in plants is important, because stimulation of protein synthesis and activation of antioxidant enzymes occur in the presence of phenolic acids at trace levels. In this research, a photoluminescence spectroscopic method was developed for the quantification of VA in plant samples after separation and pre-concentration. Selective extraction of VA from aqueous solution was performed using a solid-phase extraction column packed with nickel-aluminum layered double hydroxide as a nano-sorbent. After elution of extracted analyte from the column using 3 mL of a 3 mol/L NaOH solution, its concentration was determined spectrofluorometrically at λ(em) = 357 nm with excitation at λ(ex) = 280 nm. The spectrofluorometry method gave a linear response for VA within the range 20.0-900.0 µg/L, with a correlation coefficient of 0.9982. The limit of detection and sorption capacity were 7.6 µg/L and 66.2 mg/g, respectively. The method was validated by comparing the obtained results with gas chromatographic data. This method was used to determine VA in Chenopodium album and Prangos asperula plants.

  15. Development of an aflatoxin B1 specific molecularly imprinted solid phase extraction sorbent for the selective pre-concentration of toxic aflatoxin B1 from child weaning food, Tsabana

    Directory of Open Access Journals (Sweden)

    Semong Oratile

    2017-03-01

    Full Text Available This paper presents the synthesis, optimization and application of a molecularly imprinted polymer (MIP sorbent for the selective extraction and pre-concentration of the potent toxin, aflatoxin B1 (AFB1, from the child weaning food, Tsabana (manufactured in Serowe, Botswana. As a food safety regulatory measure, Tsabana must be cleared of hazardous aflatoxins, especially AFB1, before consumption. This is because AFB1 is the most common and potent of the aflatoxins commonly found in cereals. Accurate analysis of AFB1 is challenging because it exists in very low concentrations in complex, ‘dirty’ matrices such as food, making it difficult to detect using analytical instruments, even if these analytical techniques have sensitivities at the femto level. The MIP extraction sorbent synthesized in this paper deals with these challenges by selectively pre-concentrating AFB1 from real Tsabana samples, successfully achieving a pre-concentration factor of 5 and therefore significantly increasing ABF1 signal intensity for easier detection. Further advantages of this system include the short time (25.0 minutes and reasonable optimal MIP dose (20.0 mg needed for maximum AFB1 extraction by the sorbent. Scanning electron microscopy revealed that the prepared AFB1 powder particles have spherical geometries and reasonably small sizes (800 nm, two advantageous physical characteristics that are associated with excellent sorbent materials.

  16. Water-compatible molecularly imprinted polymer as a sorbent for the selective extraction and purification of adefovir from human serum and urine.

    Science.gov (United States)

    Pourfarzib, Mojgan; Dinarvand, Rasoul; Akbari-Adergani, Behrouz; Mehramizi, Ali; Rastegar, Hossein; Shekarchi, Maryam

    2015-05-01

    A molecularly imprinted polymer has been synthesized to specifically extract adefovir, an antiviral drug, from serum and urine by dispersive solid-phase extraction before high-performance liquid chromatography with UV analysis. The imprinted polymers were prepared by bulk polymerization by a noncovalent imprinting method that involved the use of adefovir (template molecule) and functional monomer (methacrylic acid) complex prior to polymerization, ethylene glycol dimethacrylate as cross-linker, and chloroform as porogen. Molecular recognition properties, binding capacity, and selectivity of the molecularly imprinted polymers were evaluated and the results show that the obtained polymers have high specific retention and enrichment for adefovir in aqueous medium. The new imprinted polymer was utilized as a molecular sorbent for the separation of adefovir from human serum and urine. The serum and urine extraction of adefovir by the molecularly imprinted polymer followed by high-performance liquid chromatography showed a linear calibration curve in the range of 20-100 μg/L with excellent precisions (2.5 and 2.8% for 50 μg/L), respectively. The limit of detection and limit of quantization were determined in serum (7.62 and 15.1 μg/L), and urine (5.45 and 16 μg/L). The recoveries for serum and urine samples were found to be 88.2-93.5 and 84.3-90.2%, respectively.

  17. Development of a selective sorbent for the solid-phase extraction of terbuthylazine in olive oil samples: a molecular imprinting strategy.

    Science.gov (United States)

    Garcia, Raquel; Martins, Nuno; Carreiro, Elisabete P; Simões, Marco; Carrott, Maria M L Ribeiro; Carrott, Peter J M; Burke, Anthony J; Cabrita, Maria João

    2015-04-01

    Aiming to implement an analytical methodology that is highly selective for the extraction and quantification of terbuthylazine from olive oil, we successfully achieved: (i) the development of a molecularly imprinted polymer by bulk polymerization using terbuthylazine as template molecule, methacrylic acid as functional monomer, ethylene glycol dimethacrylate as cross-linker, and dichloromethane as porogen; (ii) characterization of the imprinting material using Fourier transform infrared spectroscopy, thermogravimetric analysis, nitrogen adsorption at 77 K, and scanning electron microscopy; (iii) their molecular recognition for the template molecule using high-performance liquid chromatography, and (iv) optimization of a solid-phase extraction procedure using as sorbent the synthesized molecularly imprinted polymer for the selective extraction and clean-up of terbuthylazine from spiked organic olive oil and further quantification of the pesticide levels by high-performance liquid chromatography. The suitability of the implemented analytical methodology was demonstrated, as concentrations of terbuthylazine below the tolerated maximum residue limits in the spiked organic olive oil samples could be satisfactorily analyzed with good precision/accuracy with high recovery rates (96%). Overall, the implemented methodology has proven to be reliable and robust and is highly promising in the field of sample preparation, particularly for the isolation/preconcentration of terbuthylazine in complex food samples.

  18. Development of an automated sequential injection on-line solvent extraction-back extraction procedure as demonstrated for the determination of cadmium with detection by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2002-01-01

    An automated sequential injection (SI) on-line solvent extraction-back extraction separation/preconcentration procedure is described. Demonstrated for the assay of cadmium by electrothermal atomic absorption spectrometry (ETAAS), the analyte is initially complexed with ammonium pyrrolidinedithioc......An automated sequential injection (SI) on-line solvent extraction-back extraction separation/preconcentration procedure is described. Demonstrated for the assay of cadmium by electrothermal atomic absorption spectrometry (ETAAS), the analyte is initially complexed with ammonium....../preconcentration process of the ensuing sample. An enrichment factor of 21.4, a detection limit of 2.7 ng/l, along with a sampling frequency of 13s/h were obtained at a sample flow rate of 6.0mlmin/sup -1/. The precision (R.S.D.) at the 0.4 mug/l level was 1.8% as compared to 3.2% when quantifying the organic extractant...

  19. Development of a simple extraction cell with bi-directional continuous flow coupled on-line to ICP-MS for assessment of elemental associations in solid samples

    DEFF Research Database (Denmark)

    Buanuam, Janya; Tiptanasup, Kasipa; Shiowatana, Juwadee

    2006-01-01

    A continuous-flow system comprising a novel, custom-built extraction module and hyphenated with inductively coupled plasma-mass spectrometric (ICP-MS) detection is proposed for assessing metal mobilities and geochemical associations in soil compartments as based on using the three step BCR (now...... to discretely introduce appropriate extract volumes to the detector at a given time and with a given dilution factor. The proposed hyphenated method demonstrates excellent performance for on-line monitoring of major and trace elements (Ca, Mn, Fe, Ni, Pb, Zn and Cd) released when applying the various extracting...... the extraction time. Thus, the intimate elemental association between Cd and Zn in contaminated soils could be assessed....

  20. Dendrimer-functionalized mesoporous silica as a reversed-phase/anion-exchange mixed-mode sorbent for solid phase extraction of acid drugs in human urine.

    Science.gov (United States)

    Li, Yun; Yang, Jiajia; Huang, Chaonan; Wang, Longxing; Wang, Jincheng; Chen, Jiping

    2015-05-01

    A new dendrimer-functionalized mesoporous silica material based on large-pore 3D cubic Korea Advanced Institute of Science and Technology-6 (KIT-6) was synthesized by the growing of dendritic branches inside the mesopores of aminopropyl functionalized KIT-6. Detailed physical characterizations using transmission electron microscopy, nitrogen adsorption-desorption measurements, Fourier transform infrared (FTIR) spectroscopy, and elemental analysis reveal that the multifunctional dendrimers have been grown successfully within the confined spaces of mesopores. Although the 3D ordered mesoporous architecture of KIT-6 was well preserved, there was a significant and continuous decrease in pore size, specific surface area (SBET) and pore volume when increasing dendrimer generation up to six. In order to get a compromise between the SBET, pore size and density of functionalities, the dendrimer-functionalized KIT-6 (DF-KIT-6) for generation 2 (SBET, 314.2 m(2) g(-1); pore size, 7.9 nm; carbon and nitrogen contents, 19.80% and 1.92%) was selected for solid phase extraction (SPE) applications. The DF-KIT-6 was then evaluated as a reversed-phase/anion-exchange mixed-mode sorbent for extraction of the selected acidic drugs (ketoprofen, KEP; naproxen, NAP; and ibuprofen, IBU), since the dendrimers contained both hydrocarbonaceous and amine functionalities. The effective parameters on extraction efficiency such as sample pH and volume, type and volume of eluent and wash solvents were optimized. Under the optimized experimental conditions, the DF-KIT-6 based SPE coupled with HPLC-UV method demonstrated good sensitivity (0.4-4.6 ng mL(-1) detection of limits) and linearity (R(2)>0.990 for 10-2000 ng mL(-1) of KEP and IBU, and 1-200 ng mL(-1) of NAP). The potential use of DF-KIT-6 sorbent for preconcentration and cleanup of acid drugs in human urine samples was also demonstrated. Satisfactory recoveries at two spiking levels (30 and 300 ng mL(-1) for KEP and IBU, 3 and 30 ng mL(-1

  1. On-line monitoring the extract process of Fu-fang Shuanghua oral solution using near infrared spectroscopy and different PLS algorithms

    Science.gov (United States)

    Kang, Qian; Ru, Qingguo; Liu, Yan; Xu, Lingyan; Liu, Jia; Wang, Yifei; Zhang, Yewen; Li, Hui; Zhang, Qing; Wu, Qing

    2016-01-01

    An on-line near infrared (NIR) spectroscopy monitoring method with an appropriate multivariate calibration method was developed for the extraction process of Fu-fang Shuanghua oral solution (FSOS). On-line NIR spectra were collected through two fiber optic probes, which were designed to transmit NIR radiation by a 2 mm flange. Partial least squares (PLS), interval PLS (iPLS) and synergy interval PLS (siPLS) algorithms were used comparatively for building the calibration regression models. During the extraction process, the feasibility of NIR spectroscopy was employed to determine the concentrations of chlorogenic acid (CA) content, total phenolic acids contents (TPC), total flavonoids contents (TFC) and soluble solid contents (SSC). High performance liquid chromatography (HPLC), ultraviolet spectrophotometric method (UV) and loss on drying methods were employed as reference methods. Experiment results showed that the performance of siPLS model is the best compared with PLS and iPLS. The calibration models for AC, TPC, TFC and SSC had high values of determination coefficients of (R2) (0.9948, 0.9992, 0.9950 and 0.9832) and low root mean square error of cross validation (RMSECV) (0.0113, 0.0341, 0.1787 and 1.2158), which indicate a good correlation between reference values and NIR predicted values. The overall results show that the on line detection method could be feasible in real application and would be of great value for monitoring the mixed decoction process of FSOS and other Chinese patent medicines.

  2. Generic on-line solid phase extraction sample preparation strategies for the analysis of drugs in biological matrices by LC-MS/MS.

    Science.gov (United States)

    Bourgogne, Emmanuel; Grivet, Chantal; Varesio, Emmanuel; Hopfgartner, Gérard

    2015-01-01

    In the present work we investigate the integration of a single hardware platform (Prospekt-2) allowing on-line SPE with pre-/post-trapping dilution and direct injection of plasma extracts, and also compare the benefits and challenges of the different approaches for pharmaceutical drugs with heterogeneous physicochemical properties. In the first part, the generic use of on-line SPE with direct plasma injection or after protein precipitation was investigated for the quantitative analysis of talinolol. In the second part, pre-trapping and post-trapping dilution for on-line SPE is discussed for generic method development on an oxadiazole and its major metabolite. Finally, the difference of performance between direct plasma injection vs. off-line liquid-liquid extraction is also described for the quantification of buprenorphine and naltrexone down to 50 and 100 pg/ml using a 0.25 ml plasma aliquot. All assays were in human plasma and detection was performed by mass spectrometry detection either on simple or triple stage quadrupoles. Regardless of the tested strategy, assays were found linear, with precision and accuracy with <15% for all quality controls samples and <20% for lower limit of quantitation.

  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. Novel Poly(imide dioxime) Sorbents: Development and testing for enhanced extraction of uranium from natural seawater

    Energy Technology Data Exchange (ETDEWEB)

    Das, Sadananda; Brown, Suree S.; Mayes, Richard T.; Janke, Christopher J.; Tsouris, Costas; Kuo, Li-Jung; Gill, Gary A.; Dai, Sheng

    2016-04-09

    A new series of amidoxime-based polymer adsorbents were synthesized at the Oak Ridge National Laboratory (ORNL) by electron beam induced grafting of acrylonitrile and itaconic acid onto polyethylene fiber. Hydroxylamine derivatives of poly(acrylonitrile) (PAN) moiety are demonstrated to possess two kinds of functional groups: open-chain amidoxime and cyclic imide dioxime. The open-chain amidoxime is shown to convert to imide dioxime on heat treatment in the presence of an aprotic solvent, like dimethylsulfoxide (DMSO). The formation of amidoxime and imide dioxime was confirmed by 13-C CPMAS spectra. The adsorbents were evaluated for uranium adsorption efficiency at ORNL with simulated seawater spiked with 8 ppm uranium and 5 gallon seawater in a batch reactor, and in flow-through columns with natural seawater at the Marine Science Laboratory (MSL) of Pacific Northwest National Laboratory (PNNL) at Sequim Bay, WA. The DMSO-heat-treated sorbents adsorbed uranium as high as 4.48 g-U/kg-ads. from seawater. Experimental evidence is presented that the poly(imide dioxime) is primarily responsible for enhanced uranium adsorption capacity from natural seawater. The conjugated system in the imide dioxime ligand possesses increased electron donation ability, which is believed to significantly enhance the uranyl coordination in seawater

  5. Development and characterization of a nanodendritic silver-based solid-phase extraction sorbent for selective enrichment of endocrine-disrupting chemicals in water and milk samples.

    Science.gov (United States)

    Gao, Yuanji; Xia, Bing; Liu, Jie; Ji, Baocheng; Ma, Fengwei; Ding, Lisheng; Li, Bangjing; Zhou, Yan

    2015-11-01

    In this study, 4-[4-phenylazo-phenoxy] butyl-1-thiol (AzSH) functionalized nanodendritic silver (AzS@AgNDs) materials were prepared as a solid-phase extraction (SPE) sorbent for the selective extraction of estrogens. AzS@AgNDs possess an extremely large surface-to-volume ratio and a small average particle size. The performance of the material was evaluated by selective enrichment of hexestrol, diethylstilbestrol, dienestrol and bisphenol A in water and milk samples followed by rapid ultra-performance liquid chromatography-electrospray ionization mass spectrometry (UPLC-ESI-MS) analyses. The results exhibited that AzS@AgNDs had excellent adsorption capability for the targeted estrogens. The limits of detection of the four estrogens ranged from 0.1 to 5.0 pg/mL. The recoveries of the estrogens spiked into tap water were over the range of 83.6-105.3% with relative standard deviations of 2.8-6.0%. The results indicated the capability of this method for the rapid determination of estrogens in milk and other environmental water samples. In addition, this method would be useful for the determination of human exposure and health risk assessments trace level of endocrine-disrupting compounds (EDCs) in drinking water.

  6. N-methylimidazolium ionic liquid-functionalized silica as a sorbent for selective solid-phase extraction of 12 sulfonylurea herbicides in environmental water and soil samples.

    Science.gov (United States)

    Fang, Guozhen; Chen, Jing; Wang, Junping; He, Jinxing; Wang, Shuo

    2010-03-05

    A novel material for solid-phase extraction (SPE) was synthesized by chemical immobilization of a functionalized N-methylimidazolium ionic liquid on silica gel. Cartridges packed with the synthetic material were successfully applied to the pre-concentration of trace-level thifensulfuron-methyl, metsulfuron-methyl, chlorsulfuron, sulfometuron-methyl, rimsulfuron, ethametsulfuron, tribenuron-methyl, bensulfuron-methyl, prosulfuron, pyrazosulfuron, chlorimuron-ethyl and primisulfuron from environmental water and soil samples. The 12 sulfonylurea herbicides (SUs) obtained a good resolution in less than 50 min using HPLC with a UV detector. The recovery studies using the ionic liquid-functionalized silica as a sorbent were performed by three consecutive extractions of water and soil samples at two spiked levels. The average recovery for each analyte was in the range of 53.8-118.2% for the water samples and 60.9-121.3% for the soil sample, with RSDs lower than 11.3% in all cases. The ionic liquid-functionalized silica cartridges showed higher selectivity for the SUs than commercially available C(18) cartridges did.

  7. Use of microextraction by packed sorbents following selective pressurised liquid extraction for the determination of brominated diphenyl ethers in sewage sludge by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Martínez-Moral, María Pilar; Tena, María Teresa

    2014-10-17

    In this work, a method based on selective pressurised liquid extraction followed by microextraction by packed sorbents (MEPS) for the determination of brominated diphenyl ethers (BDEs) in sewage sludge is presented. The factors affecting the MEPS procedure were optimised. Acetone:water (25:75) sPLE extracts were drawn-ejected 10 times through C18 cartridges at 5 μL s(-1). The cartridge was dried five times with 250 μL of air and the BDEs were eluted at 25 μL s(-1) with 100 μL of n-hexane that were directly injected at 13 μL s(-1) in the GC-MSMS system. Under these conditions, there were no carry-over effects. The method was characterised in terms of limits of detection, repeatability, intermediate precision and accuracy. The use of MEPS for the determination of BDEs in sewage sludge means an improvement of the limits of detection due to the preconcentration and clean-up performed before the injection of the whole elute in the PTV injector. The GC-MSMS LODs (25 pg mL(-1)) were improved with MEPS to less than 3 pg mL(-1). RSD less than 7% and recovery values from 92% to 102% were shown. Finally, the method was applied to the sPLE extract analyses of sewage sludge from several wastewater treatment plants in La Rioja. To our knowledge, this is the first time that the MEPS technique has been applied to the analysis of BDEs, and the first time that it has been used for the analysis of extracts from a solid sample.

  8. Moving-bed sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Ayala, R.E.; Gupta, R.P.; Chuck, T.

    1995-12-01

    The objective of this program is to develop mixed-metal oxide sorbent formulations that are suitable for moving-bed, high-temperature, desulfurization of coal gas. Work continues on zinc titanates formulations and Z-sorb III sorbent.

  9. Isolation and Bioactivity Analysis of Ethyl Acetate Extract from Acer tegmentosum Using In Vitro Assay and On-Line Screening HPLC-ABTS+ System

    Directory of Open Access Journals (Sweden)

    Kwang Jin Lee

    2014-01-01

    Full Text Available The Acer tegmentosum (3 kg was extracted using hot water, and the freeze-dried extract powder was partitioned successively using dichloromethane (DCM, ethyl acetate (EA, butyl alcohol (n-BuOH, and water. From the EA extract fraction (1.24 g, five phenolic compounds were isolated by the silica gel, octadecyl silica gel, and Sephadex LH-20 column chromatography. Based on spectroscopic methods such as 1H-NMR, 13C-NMR, and LC/MS the chemical structures of the compounds were confirmed as feniculin (1, avicularin (2, (+-catechin (3, (−-epicatechin (4, and 6′-O-galloyl salidroside (5. Moreover, a rapid on-line screening HPLC-ABTS+ system for individual bioactivity of the EA-soluble fraction (five phenolic compounds was developed. The results indicated that compounds 1 and 2 were first isolated from the A. tegmentosum. The anti-inflammatory activities and on-line screening HPLC-ABTS+ assay method of these compounds in LPS-stimulated murine macrophages were rapid and efficient for the investigation of bioactivity of A. tegmentosum.

  10. Automated on-line liquid–liquid extraction system for temporal mass spectrometric analysis of dynamic samples

    Energy Technology Data Exchange (ETDEWEB)

    Hsieh, Kai-Ta; Liu, Pei-Han [Department of Applied Chemistry, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China); Urban, Pawel L. [Department of Applied Chemistry, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China); Institute of Molecular Science, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China)

    2015-09-24

    Most real samples cannot directly be infused to mass spectrometers because they could contaminate delicate parts of ion source and guides, or cause ion suppression. Conventional sample preparation procedures limit temporal resolution of analysis. We have developed an automated liquid–liquid extraction system that enables unsupervised repetitive treatment of dynamic samples and instantaneous analysis by mass spectrometry (MS). It incorporates inexpensive open-source microcontroller boards (Arduino and Netduino) to guide the extraction and analysis process. Duration of every extraction cycle is 17 min. The system enables monitoring of dynamic processes over many hours. The extracts are automatically transferred to the ion source incorporating a Venturi pump. Operation of the device has been characterized (repeatability, RSD = 15%, n = 20; concentration range for ibuprofen, 0.053–2.000 mM; LOD for ibuprofen, ∼0.005 mM; including extraction and detection). To exemplify its usefulness in real-world applications, we implemented this device in chemical profiling of pharmaceutical formulation dissolution process. Temporal dissolution profiles of commercial ibuprofen and acetaminophen tablets were recorded during 10 h. The extraction-MS datasets were fitted with exponential functions to characterize the rates of release of the main and auxiliary ingredients (e.g. ibuprofen, k = 0.43 ± 0.01 h{sup −1}). The electronic control unit of this system interacts with the operator via touch screen, internet, voice, and short text messages sent to the mobile phone, which is helpful when launching long-term (e.g. overnight) measurements. Due to these interactive features, the platform brings the concept of the Internet-of-Things (IoT) to the chemistry laboratory environment. - Highlights: • Mass spectrometric analysis normally requires sample preparation. • Liquid–liquid extraction can isolate analytes from complex matrices. • The proposed system automates

  11. Steam induced structural changes of a poly(ethylenimine) impregnated γ-alumina sorbent for CO2 extraction from ambient air.

    Science.gov (United States)

    Sakwa-Novak, Miles A; Jones, Christopher W

    2014-06-25

    Poly(ethylenimine) (PEI) impregnated mesoporous γ-alumina sorbents are utilized for CO2 adsorption from dry and humid simulated ambient air, and the sorbents are regenerated under an environment of flowing steam for times ranging from 5 min to 24 h of continuous exposure. The sorbents are compared on the basis of equilibrium CO2 capacities from simulated air at 400 ppm of CO2, 50% relative humidity, and 30 °C as well as their physiochemical characterization by means of X-ray diffraction (XRD), (27)Al NMR spectroscopy, IR spectroscopy, Raman spectroscopy, N2 physisorption, and elemental analysis. The sorbents retain better than 90% of the initial equilibrium capacity of ∼1.7 mmol/g at steam exposure times up to 12 h; however, PEI leaching reduced the capacity of the sorbent to 0.66 mmol/g after 24 h of continuous treatment. It is demonstrated that the γ-alumina support partially hydrates to form a boehmite crystal phase at steam times of 90 min and longer but that this phase transition occurs predominately between 90 min and 12 h of steam treatment, slowing at longer times of 12 and 24 h of treatment. Evidence is presented to suggest that the presence of boehmite on the sorbent surface does not significantly alter the amine efficiency of impregnated PEI. The collected results suggest that γ-alumina/PEI composite materials are promising sorbents for CO2 capture from ambient air with regeneration in flowing steam.

  12. Characterization of particle morphology of biochanin A molecularly imprinted polymers and their properties as a potential sorbent for solid-phase extraction

    Energy Technology Data Exchange (ETDEWEB)

    Chrzanowska, Anna M.; Poliwoda, Anna, E-mail: Anna.Poliwoda@uni.opole.pl; Wieczorek, Piotr P.

    2015-04-01

    Molecularly imprinted polymers (MIPs) with biochanin A as a template were obtained using a bulk polymerization with non-covalent imprinting approach. The polymers were prepared in acetonitrile as porogen, using ethylene glycol dimethacrylate (EDMA) as cross-linking agent. The synthesis, with an application of 1′,1′-azobis(cyclohexanecarbonitrile) (ACHN) as an initiator, has been performed thermally. During the synthesis process the effect of different functional monomers such as methacrylic acid (MAA), acrylamide (AA) and 4-vinylpyridine (4-VP) was investigated. The application of nitrogen sorption porosimetry, scanning electron microscopy (SEM), and Fourier transform infrared spectroscopy (FTIR) permitted the characterization and evaluation of synthesized polymers. The adsorption capacity of obtained MIPs was checked by using the binding testing. All synthesized polymers were evaluated as solid-phase extraction (SPE) sorbents for isolation and preconcentration of biochanin A and its analogues, daidzein and genistein. The MIPs exhibited higher affinity for biochanin A over competitive compounds. - Highlights: • The molecularly imprinted polymers with biochanin A as a template were synthesized. • The surface of synthesized monoliths was formed mainly from mesopores (73–77%). • Biochanin A was effectively concentrated in each of the synthesized polymers (recovery > 89.8%). • The results show potential ability of synthesized MIPs in analysis of phytoestrogens in real samples.

  13. Multiwalled carbon nanotubes as a sorbent material for the solid phase extraction of lead from urine and subsequent determination by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Peña Crecente, Rosa M.; Lovera, Carlha Gutiérrez; García, Julia Barciela; Méndez, Jennifer Álvarez; Martín, Sagrario García; Latorre, Carlos Herrero

    2014-11-01

    The determination of lead in urine is a way of monitoring the chemical exposure to this metal. In the present paper, a new method for the Pb determination by electrothermal atomic absorption spectrometry (ETAAS) in urine at low levels has been developed. Lead was separated from the undesirable urine matrix by means of a solid phase extraction (SPE) procedure. Oxidized multiwalled carbon nanotubes have been used as a sorbent material. Lead from urine was retained at pH 4.0 and was quantitatively eluted using a 0.7 M nitric acid solution and was subsequently measured by ETAAS. The effects of parameters that influence the adsorption-elution process (such as pH, eluent volume and concentration, sampling and elution flow rates) and the atomic spectrometry conditions have been studied by means of different factorial design strategies. Under the optimized conditions, the detection and quantification limits obtained were 0.08 and 0.26 μg Pb L- 1, respectively. The results demonstrate the absence of a urine matrix effect and this is the consequence of the SPE process carried out. Therefore, the developed method is useful for the analysis of Pb at low levels in real samples without the influence of other urine components. The proposed method was applied to the determination of lead in urine samples of unexposed healthy people and satisfactory results were obtained (in the range 3.64-22.9 μg Pb L- 1).

  14. Determination of carbofuran in surface water and biological tissue by sol-gel immunoaffinity extraction and on-line preconcentration/HPLC/UV analysis.

    Science.gov (United States)

    Vera-Avila, Luz E; Márquez-Lira, Bani P; Villanueva, Marcos; Covarrubias, Rosario; Zelada, Gustavo; Thibert, Valérie

    2012-01-15

    A selective and simple analytical method for the trace level determination of carbofuran in complex environmental and biological samples was developed based on immunoaffinity extraction (IAE) followed by on-line preconcentration and HPLC/UV analysis of the purified extract. The immunosorbent for IAE was prepared by sol-gel encapsulation of monoclonal anti-carbofuran antibodies, and was fully characterized for capacity, repeatability, binding strength, binding kinetics and cross-reactivity. Method performance was evaluated with two different types of difficult samples: dam water and methanolic extracts of epithelial cervical-uterine tissue. Linear behavior and quantitative recoveries were obtained from the analysis of samples spiked with carbofuran at 0.2-4 ng/mL (dam water, 50 mL samples) and 10-40 ng/mL (biological tissue extract, 2 mL samples). RSD (n=7) and detection limits were, respectively, 10.1% (spike 0.40 ng/mL) and 0.13 ng/mL for dam water; 8.5% (spike 20 ng/mL) and 5 ng/mL for the biological tissue extract. The excellent sample purification achieved with the IAE column allows precise and accurate determination of carbofuran in complex matrices, even when using non-selective UV detection in the chromatographic analysis.

  15. On-line micro-volume introduction system developed for lower density than water extraction solvent and dispersive liquid-liquid microextraction coupled with flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-07-06

    Highlights: Black-Right-Pointing-Pointer A dispersive liquid-liquid micro extraction method for lead and copper determination. Black-Right-Pointing-Pointer A micro-volume transportation system for extractant solvent lighter than water. Black-Right-Pointing-Pointer Analysis of natural water samples. - Abstract: A simple and fast preconcentration/separation dispersive liquid-liquid micro extraction (DLLME) method for metal determination based on the use of extraction solvent with lower density than water has been developed. For this purpose a novel micro-volume introduction system was developed enabling the on-line injection of the organic solvent into flame atomic absorption spectrometry (FAAS). The effectiveness and efficiency of the proposed system were demonstrated for lead and copper preconcentration in environmental water samples using di-isobutyl ketone (DBIK) as extraction solvent. Under the optimum conditions the enhancement factor for lead and copper was 187 and 310 respectively. For a sample volume of 10 mL, the detection limit (3 s) and the relative standard deviation were 1.2 {mu}g L{sup -1} and 3.3% for lead and 0.12 {mu}g L{sup -1} and 2.9% for copper respectively. The developed method was evaluated by analyzing certified reference material and it was applied successfully to the analysis of environmental water samples.

  16. On-line extraction and determination of two herbicides: comparison between two modes of three-phase hollow fiber microextraction.

    Science.gov (United States)

    Tajik, Mohammad; Yamini, Yadollah; Esrafili, Ali; Ebrahimpour, Behnam

    2015-02-01

    Two different modes of three-phase hollow fiber liquid-phase microextraction were studied for the extraction of two herbicides, bensulfuron-methyl and linuron. In these two modes, the acceptor phases in the lumen of the hollow fiber were aqueous and organic solvents. The extraction and determination were performed using an automated hollow fiber microextraction instrument followed by high-performance liquid chromatography. For both three-phase hollow fiber liquid-phase microextraction modes, the effect of the main parameters on the extraction efficiency were investigated and optimized by central composite design. Under optimal conditions, both modes showed good linearity and repeatability, but the three-phase hollow fiber liquid-phase microextraction based on two immiscible organic solvents has a better extraction efficiency and figures of merit. The calibration curves for three-phase hollow fiber liquid-phase microextraction with an organic acceptor phase were linear in the range of 0.3-200 and 0.1-150 μg/L and the limits of detection were 0.1 and 0.06 μg/L for bensulfuron-methyl and linuron, respectively. For the conventional three-phase hollow fiber liquid-phase microextraction, the calibration curves were linear in the range of 3.0-250 and 15-400 μg/L and LODs were 1.0 and 5.0 μg/L for bensulfuron-methyl and linuron, respectively. The real sample analysis was carried out by three-phase hollow fiber liquid phase microextraction based on two immiscible organic solvents because of its more favorable characteristics.

  17. Hyphenating size-exclusion chromatography with electrospray mass spectrometry; using on-line liquid-liquid extraction to study the lipid composition of lipoprotein particles.

    Science.gov (United States)

    Osei, Michael; Griffin, Julian L; Koulman, Albert

    2015-11-15

    Lipoproteins belong to the most commonly measured clinical biochemical parameters. Lipidomics is an orthogonal approach and aims to profile the individual lipid molecules that jointly form the lipoprotein particles. However, in the first step of the extraction of lipid molecules from serum, an organic solvent is used leading to dissociation of the lipoproteins. Thus far it has been impossible to combine lipidomics and lipoprotein analysis in one analytical system. Human plasma was diluted in phosphate-buffered saline (PBS) and injected onto a Superose 6 PC 3.2 column with PBS as a mobile phase to separate lipoproteins. The eluent was led to a Syrris FLLEX module, which also received CHCl3 /MeOH (3:1). The two phases were mixed and subsequently separated using a Teflon membrane in an especially designed pressurized flow chamber. The organic phase was led to a standard electrospray source of an Orbitrap mass spectrometer. Size-exclusion chromatography (SEC) has been commonly applied to separate lipoproteins and is considered a practical alternative to ultracentrifugation. Through the on-line liquid-liquid extraction method it becomes possible to obtained detailed mass spectra of lipids across different lipoprotein fractions. The extracted ion chromatograms of specific lipid signals showed their distribution against the size of lipoprotein particles. The application of on-line liquid-liquid extraction allows for the continuous electrospray-based mass spectral analysis of SEC eluent, providing the detailed lipid composition of lipoprotein particles separated by size. This approach provides new possibilities for the study of the biochemistry of lipoproteins. © 2015 The Authors. Rapid Communications in Mass Spectrometry Published by John Wiley & Sons Ltd.

  18. On-line monitoring of extraction process of Flos Lonicerae Japonicae using near infrared spectroscopy combined with synergy interval PLS and genetic algorithm

    Science.gov (United States)

    Yang, Yue; Wang, Lei; Wu, Yongjiang; Liu, Xuesong; Bi, Yuan; Xiao, Wei; Chen, Yong

    2017-07-01

    There is a growing need for the effective on-line process monitoring during the manufacture of traditional Chinese medicine to ensure quality consistency. In this study, the potential of near infrared (NIR) spectroscopy technique to monitor the extraction process of Flos Lonicerae Japonicae was investigated. A new algorithm of synergy interval PLS with genetic algorithm (Si-GA-PLS) was proposed for modeling. Four different PLS models, namely Full-PLS, Si-PLS, GA-PLS, and Si-GA-PLS, were established, and their performances in predicting two quality parameters (viz. total acid and soluble solid contents) were compared. In conclusion, Si-GA-PLS model got the best results due to the combination of superiority of Si-PLS and GA. For Si-GA-PLS, the determination coefficient (Rp2) and root-mean-square error for the prediction set (RMSEP) were 0.9561 and 147.6544 μg/ml for total acid, 0.9062 and 0.1078% for soluble solid contents, correspondingly. The overall results demonstrated that the NIR spectroscopy technique combined with Si-GA-PLS calibration is a reliable and non-destructive alternative method for on-line monitoring of the extraction process of TCM on the production scale.

  19. Flow injection analysis with on-line nylon powder extraction for room-temperature phosphorescence determination of thiabendazole.

    Science.gov (United States)

    Piccirilli, G N; Escandar, G M

    2009-07-30

    A fast and very selective flow-through phosphorescence optosensor was designed and characterized for the determination of the fungicide thiabendazole in water samples. For the first time, thiabendazole was determined using a flow-through optosensor based on the phosphorescence signals obtained when it is retained in a solid support. While thiabendazole does not phosphoresce in packing materials commonly used to fill the flow-cell, significant emission signals are observed when it is retained on nylon powder in the presence of iodide and sulfite. The experimental set-up was based on a flow-injection manifold coupled to an on-line phosphorescence detector containing nylon powder packed in a conventional flow-cell. Potassium iodide and sodium sulfite were added to sample aliquots to improve the thiabendazole phosphorescence and injected in the flow manifold using water as carrier. After the phosphorescence emission was registered, the analyte was eluted from the packed nylon with a 65% (v/v) methanol-water mixture. Optimal instrumentation, experimental and flow conditions were evaluated. Using a sample volume of 2000 microL, the analytical signal showed a very good linearity in the range 12.9-110 ng mL(-1), with a detection limit of 4.5 ng mL(-1), and a sample throughput of about 14 samples per hour. The effects of the presence of concomitant species in the thiabendazole phosphorescence signal were studied, and a comparison with the fluorescence nylon-powder optosensor was carried out and discussed. Finally, the applicability of the proposed optosensor was tested in water samples, and satisfactory recoveries ranging between 97% and 105% were obtained.

  20. Organically modified silica with pyrazole-3-carbaldehyde as a new sorbent for solid-liquid extraction of heavy metals

    National Research Council Canada - National Science Library

    Radi, Smaail; Tighadouini, Said; Bacquet, Maryse; Degoutin, Stéphanie; Cazier, Francine; Zaghrioui, Mustapha; Mabkhot, Yahia N

    ...). The new prepared material was used as an adsorbent for the solid-phase extraction (SPE) of Pb(II), Cd(II), Cu(II) and Zn(II) from aqueous solutions using a batch method, prior to their determination by flame atomic adsorption spectrometry...

  1. Multiwalled carbon nanotubes as a sorbent material for the solid phase extraction of lead from urine and subsequent determination by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Peña Crecente, Rosa M.; Lovera, Carlha Gutiérrez; García, Julia Barciela; Méndez, Jennifer Álvarez; Martín, Sagrario García; Latorre, Carlos Herrero, E-mail: carlos.herrero@usc.es

    2014-11-01

    The determination of lead in urine is a way of monitoring the chemical exposure to this metal. In the present paper, a new method for the Pb determination by electrothermal atomic absorption spectrometry (ETAAS) in urine at low levels has been developed. Lead was separated from the undesirable urine matrix by means of a solid phase extraction (SPE) procedure. Oxidized multiwalled carbon nanotubes have been used as a sorbent material. Lead from urine was retained at pH 4.0 and was quantitatively eluted using a 0.7 M nitric acid solution and was subsequently measured by ETAAS. The effects of parameters that influence the adsorption–elution process (such as pH, eluent volume and concentration, sampling and elution flow rates) and the atomic spectrometry conditions have been studied by means of different factorial design strategies. Under the optimized conditions, the detection and quantification limits obtained were 0.08 and 0.26 μg Pb L{sup −1}, respectively. The results demonstrate the absence of a urine matrix effect and this is the consequence of the SPE process carried out. Therefore, the developed method is useful for the analysis of Pb at low levels in real samples without the influence of other urine components. The proposed method was applied to the determination of lead in urine samples of unexposed healthy people and satisfactory results were obtained (in the range 3.64–22.9 μg Pb L{sup −1}). - Highlights: • Lead determination in urine using a solid phase extraction procedure followed by ETAAS • Carbon nanotubes as SPE adsorbent for Pb in urine • Matrix elimination for the Pb determination in urine by using SPE based on carbon nanotubes • The detection limit was 0.08 μg Pb L{sup −1}.

  2. QuEChERS-based extraction with dispersive solid phase extraction clean-up using PSA and ZrO2-based sorbents for determination of pesticides in bovine milk samples by HPLC-DAD.

    Science.gov (United States)

    Rejczak, Tomasz; Tuzimski, Tomasz

    2017-02-15

    In this study, a quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction technique was adapted to develop a simple sample treatment for multi-residue pesticide analysis in milk samples. The proposed method is based on liquid-liquid partitioning with acetonitrile followed by dispersive solid phase extraction clean-up using primary secondary amine along with zirconia-coated silica particles for extract purification. Identification and quantification of 30 pesticides was conducted via high performance liquid chromatography with diode-array detection (HPLC-DAD). Recoveries were from 70 to 100% for the vast majority of the analytes, with relative standard deviations less than 20% being observed. HPLC-DAD provided suitable linearity, precision and accuracy. For 28 of 30 analytes in the study method limit of quantification values (mLOQs) comply with the most recent European Union guidelines for the maximum residue levels (MRLs) in milk. Negligible matrix effect was observed due to efficient extract clean-up with ZrO2-based sorbents.

  3. [Determination of estrogen residues in drinking water by on-line solid phase extraction based on sol-gel technique coupled with high performance liquid chromatography].

    Science.gov (United States)

    Li, Longfei; Su, Min; Shi, Xiaolei; Wang, Yana; Wang, Minmin; He, Jinxing

    2014-02-01

    A method for the determination of diethylstilbestrol (DES), hexestrol (HEX) and dienestrol (DS) residues in drinking water was established by on-line solid phase extraction (SPE) coupled with high performance liquid chromatography (HPLC). The material synthesized on the base of sol-gel technology was employed as adsorbent. This material was prepared using 3-aminopropyltriethoxysilane (APTES) as the functional monomer, tetraethoxysilane (TEOS) as the crosslinking agent, and acetic acid as the initiator. The synthesized adsorbent showed outstanding property for the estrogen extraction. The estrogen can be caught effectively from water samples and the extraction can be achieved rapidly. Some important parameters, such as pH of sample solution, eluent solvents, loading flow rate, which might influence extraction efficiency, were optimized. The results indicated that the limit of detection (S/N = 3) of the developed method could reach 0.07-0.13 microg/L under the conditions of pH 7.0 of sample solution, methanol and 1% (v/v) acetic acid aqueous solution as the eluent solvent and the loading flow rate of 2 mL/min. The recoveries of the three estrogens from the water samples at three spiked levels ranged from 82.31% to 99.43% with RSD of 1.61%-7.15%. The method was simple, rapid, and suitable to detect the trace residues of estrogens in drinking water.

  4. A needle extraction utilizing a molecularly imprinted-sol-gel xerogel for on-line microextraction of the lung cancer biomarker bilirubin from plasma and urine samples.

    Science.gov (United States)

    Moein, Mohammad Mahdi; Jabbar, Dunia; Colmsjö, Anders; Abdel-Rehim, Mohamed

    2014-10-31

    In the present work, a needle trap utilizing a molecularly imprinted sol-gel xerogel was prepared for the on-line microextraction of bilirubin from plasma and urine samples. Each prepared needle could be used for approximately one hundred extractions before it was discarded. Imprinted and non-imprinted sol-gel xerogel were applied for the extraction of bilirubin from plasma and urine samples. The produced molecularly imprinted sol-gel xerogel polymer showed high binding capacity and fast adsorption/desorption kinetics for bilirubin in plasma and urine samples. The adsorption capacity of molecularly imprinted sol-gel xerogel polymer was approximately 60% higher than that of non-imprinted polymer. The effect of the conditioning, washing and elution solvents, pH, extraction time, adsorption capacity and imprinting factor were investigated. The limit of detection and the lower limit of quantification were set to 1.6 and 5nmolL(-1), respectively using plasma or urine samples. The standard calibration curves were obtained within the concentration range of 5-1000nmolL(-1) in both plasma and urine samples. The coefficients of determination values (R(2)) were ≥0.998 for all runs. The extraction recovery was approximately 80% for BR in the human plasma and urine samples.

  5. [Determination of 28 organochlorine and pyrethroid pesticides in pine nuts using solid-phase extraction and on-line gel permeation chromatography-gas chromatography/mass spectrometry].

    Science.gov (United States)

    Kang, Qinghe; Wu, Yan; Gao, Kaiyang; Li, Zhibin

    2009-03-01

    An analytical method has been developed for the determination of 28 organochlorine pesticides and pyrethroid pesticides in pine nuts. The sample was extracted With acetonitrile-water (4:1, v/v) as the extraction solution by means of high-speed homogenization. The crude extract was purified by an Aluminium-N solid phase extraction column to remove most of the fat and sterols in the sample, then on-line gel permeation chromatography-gas chromatography/ mass spectrometry (GPC-GC/MS) analysis was performed. The recoveries for the most of pesticides in the sample spiked with the standards of 0.05 mg/kg were 70%-120%, and the relative standard deviations were less than 15%. The limits of detection of 28 organochlorine pesti- and pyrethroid pesticides were 0.002-0.05 mg/kg. The linear relationship and the recovery results were satisfactory. The method is rapid, accurate, highly senstive, and can be used for the simultaneous determination of pesticide residues in pine nuts.

  6. Selective solid-phase extraction using molecular imprinted polymer sorbent for the analysis of florfenicol in food samples.

    Science.gov (United States)

    Sadeghi, Susan; Jahani, Moslem

    2013-11-15

    A molecularly imprinted polymer (MIP) for the selective solid phase extraction (SPE) of florfenicol (FF) was prepared using FF as template and 4-vinyl pyridine (4-VP) as functional monomer. For comparison, non-imprinted polymer (NIP) was synthesized in the absence of FF. The synthesized polymers were characterised by infrared spectroscopy (IR), scanning electron microscopy (SEM), thermogravimetry analysis (TGA) and differential thermal analysis (DTA). A molecularly imprinted solid phase extraction (MISPE) procedure was performed in column method by spectrophotometry detection technique. The prepared FF-MIP showed higher adsorption capacity than the non-imprinted polymer (NIP) and the maximum static adsorption capacities of FF on the MIP and the NIP were 4.32 and 2.88mgg(-1), respectively. Kinetics of the adsorption was fast and the adsorption equilibrium was achieved in 30min. The accuracy of the developed method was satisfactory for determination of FF in fish, chicken meat and honey samples.

  7. Zeolite imidazolate frameworks 8 as sorbent and its application to sonication-assisted emulsification microextraction combined with vortex-assisted porous membrane-protected micro-solid-phase extraction for fast analysis of acidic drugs in environmental water samples.

    Science.gov (United States)

    Ge, Dandan; Lee, Hian Kee

    2012-09-28

    A novel and fast procedure, sonication-assisted emulsification microextraction combined with vortex-assisted porous membrane protected micro-solid-phase extraction (SAEME-VA-μ-SPE), was developed for the gas chromatography-mass spectrometric determination of acidic drugs from environmental water samples. One advantage of the new procedure is that any solvent immiscible with water can be used as extractant solvent of SAEME and any solid sorbent can be used for μ-SPE in the SAEME-VA-μ-SPE process. In the present work, zeolite imidazolate framework 8 (ZIF-8) was employed as extraction sorbent for μ-SPE and 1-octanol as extractant solvent for SAEME. ZIF-8 has very good thermal, chemical and water stability, which make it a suitable material for the extraction of trace analytes from aqueous samples. Under the optimized extraction conditions, the developed method exhibited low limits of detection (0.01-0.04 ng/ml), good linearity (with r² between 0.9965 and 0.9993) from 0.5 to 50 ng/ml and satisfactory repeatability (between 4.1% and 7.6%). In essence SAEME-VA-μ-SPE is a combination of two different and efficient miniaturized techniques. It was demonstrated to be a fast, accurate, and convenient pretreatment procedure for trace analysis of environmental water samples.

  8. Mesoporous silica based MCM-41 as solid-phase extraction sorbent combined with micro-liquid chromatography-quadrupole-mass spectrometry for the analysis of pharmaceuticals in waters.

    Science.gov (United States)

    Dahane, S; Martínez Galera, M; Marchionni, M E; Socías Viciana, M M; Derdour, A; Gil García, M D

    2016-05-15

    This paper reports the first application of the silica based mesoporous material MCM-41 as a sorbent in solid phase extraction, to pre-concentrate pharmaceuticals of very different polarity (atenolol, nadolol, pindolol, timolol, bisoprolol, metoprolol, betaxolol, ketoprofen, naproxen, ibuprofen, diclofenac, tolfenamic acid, flufenamic acid and meclofenamic acid) in surface waters. The analytes were extracted from 100mL water samples at pH 2.0 (containing 10(-3) mol/L of sodium chloride) by passing the solution through a cartridge filled with 100 mg of MCM-41. Following elution, the pharmaceuticals were determined by micro-liquid chromatography and triple quadrupole-mass spectrometry. Two selected reaction monitoring transitions were monitored per compound, the most intense one being used for quantification and the second one for confirmation. Matrix effect was found in real waters for most analytes and was overcome using the standard addition method, which compared favorably with the matrix matched calibration method. The detection limits in solvent (acetonitrile:water 10:90, v/v) ranged from 0.01 to 1.48 μg/L and in real water extracts from 0.10 to 3.85 μg/L (0.001-0.0385 μg/L in the water samples). The quantitation limits in solvent were in the range 0.02-4.93 μg/L, whereas in real water extracts were between 0.45 and 10.00 μg/L (0.0045 and 0.1000 μg/L in the water samples). When ultrapure water samples were spiked at two concentration levels of each pharmaceutical (0.1 and 0.2 μg/L) and quantified using solvent based calibration graphs, recoveries were near 100%. However, recoveries for most pharmaceuticals were comparable or better than de described above, when river water samples (spiked at the same concentration levels) were quantified by the standard addition method and slightly worse using the matrix matched calibration method. Five real samples (two rivers, one dam and two fountain water samples) were analyzed by the developed method, atenolol

  9. Extraction and analysis of pollutant organics from contaminated solids using off-line supercritical fluid extraction (SFE) and on-line SFE-infrared spectroscopy. Task 2. Semiannual report, November 1995--March 1996

    Energy Technology Data Exchange (ETDEWEB)

    Hawthorne, S.B.

    1996-04-01

    This document describes activities in the following tasks associated with a project on environmental management technology decontamination and commercialization: A commercialized version of a field-portable instrument for performing supercritical fluid extraction (SFE) with on-line Fourier transform infrared (FT-IR) detection;pyrolysis of plastic wastes associated with mixtures of radioactive wastes;management and reporting activities; centrifugal membrane filtration with application to tank waste remediation; technology development integration activities associated with remedial action and waste management.

  10. Extraction and analysis of pollutant organics from contaminated solids using off-line supercritical fluid extraction (SFE) and on-line SFE-infrared spectroscopy. Task 2. Semiannual report, November 1995--March 1996

    Energy Technology Data Exchange (ETDEWEB)

    Hawthorne, S.B.

    1996-04-01

    This document describes activities in the following tasks associated with a project on environmental management technology decontamination and commercialization: A commercialized version of a field-portable instrument for performing supercritical fluid extraction (SFE) with on-line Fourier transform infrared (FT-IR) detection;pyrolysis of plastic wastes associated with mixtures of radioactive wastes;management and reporting activities; centrifugal membrane filtration with application to tank waste remediation; technology development integration activities associated with remedial action and waste management.

  11. Automatized flow-batch method for fluorescent determination of free glycerol in biodiesel samples using on-line extraction.

    Science.gov (United States)

    Lima, Marcelo B; Insausti, Matías; Domini, Claudia E; Pistonesi, Marcelo F; de Araújo, Mário C Ugulino; Band, Beatriz S Fernández

    2012-01-30

    An automatic method, based on flow-batch (FB), for determining glycerol in biodiesel was developed. The FB systems draw upon the useful features of flow, batch and multi-commutation approaches. The standards and samples preparation, as well as, derivatization and analysis were fully automated. For that purpose, a homemade chamber was built. The proposed method is based on liquid-liquid extraction of glycerol and simultaneous oxidation with periodate, generating formaldehyde that reacts with acetylacetone. A fluorescent product of 3,5-diacetyl-1,4-dihydrolutidine was obtained. The fluorescence signal was recorded at λ(ex) =417 nm and λ(em) = 514 nm. A linear response was observed from 0.10 to 5.00 mg L(-1) glycerol, variation coefficient 1.5%, sampling rate 14 h(-1) and detection limit 0.036 mg L(-1) glycerol. The procedure was successfully applied to the analysis of biodiesel samples, and the results agreed with the reference method (ASTM D6584-07) at 95% confidence level. Copyright © 2011 Elsevier B.V. All rights reserved.

  12. Determination of arachidonic acid by on-line solid-phase extraction HPLC with UV detection for screening of cytosolic phospholipase A2α inhibitors.

    Science.gov (United States)

    Hanekamp, Walburga; Lehr, Matthias

    2012-07-01

    An on-line solid-phase extraction (SPE)-liquid chromatographic method with ultraviolet detection at 200nm for screening of inhibitors of cytosolic phospholipase A(2)α (cPLA(2)α) was developed and validated. cPLA(2)α was isolated from porcine platelets. Enzyme activity was determined by measuring the release of arachidonic acid from a phospholipid substrate using automated on-line sample clean up on a trap column followed by isocratic back-flush elution on a RP18 analytical column. While the use of a conventional RP18 column for trapping the analyte led to peak broadening only after a few runs due to pollution of the column by binding of components present in the enzyme preparation, the application of a turbulent flow column (TurboFlow Cyclone™) resulted in sharp peaks even after a plurality of injections. Interestingly, for sample introduction a turbulent flow of the mobile phase produced by high flow rates was not necessary to maintain good peak shapes. The same result could also be achieved applying low flow rates (0.5 mL/min). Several known cPLA(2)α inhibitors were used to validate the test system.

  13. Organically modified silica with pyrazole-3-carbaldehyde as a new sorbent for solid-liquid extraction of heavy metals.

    Science.gov (United States)

    Radi, Smaail; Tighadouini, Said; Bacquet, Maryse; Degoutin, Stéphanie; Cazier, Francine; Zaghrioui, Mustapha; Mabkhot, Yahia N

    2013-12-24

    A new chelating matrix, SiNP, has been prepared by immobilizing 1.5-dimethyl-1H-pyrazole-3-carbaldehyde on silica gel modified with 3-aminopropyl-trimethoxysilane. This new chelating material was well characterized by elemental analysis, FT-IR spectroscopy, cross polarization magic angle spinning solid state 13C-NMR, nitrogen adsorption-desorption isotherm, BET surface area, BJH pore size, and scanning electron microscopy (SEM). The new product exhibits good chemical and thermal stability as determined by thermogravimetry curves (TGA). The new prepared material was used as an adsorbent for the solid-phase extraction (SPE) of Pb(II), Cd(II), Cu(II) and Zn(II) from aqueous solutions using a batch method, prior to their determination by flame atomic adsorption spectrometry. The adsorption capacity was investigated using kinetics and pH effects. Common coexisting ions did not interfere with separation and determination.

  14. Graphene-Based Materials as Solid Phase Extraction Sorbent for Trace Metal Ions, Organic Compounds, and Biological Sample Preparation.

    Science.gov (United States)

    Ibrahim, Wan Aini Wan; Nodeh, Hamid Rashidi; Sanagi, Mohd Marsin

    2016-07-03

    Graphene is a new carbon-based material that is of interest in separation science. Graphene has extraordinary properties including nano size, high surface area, thermal and chemical stability, and excellent adsorption affinity to pollutants. Its adsorption mechanisms are through non-covalent interactions (π-π stacking, electrostatic interactions, and H-bonding) for organic compounds and covalent interactions for metal ions. These properties have led to graphene-based material becoming a desirable adsorbent in a popular sample preparation technique known as solid phase extraction (SPE). Numerous studies have been published on graphene applications in recent years, but few review papers have focused on its applications in analytical chemistry. This article focuses on recent preconcentration of trace elements, organic compounds, and biological species using SPE-based graphene, graphene oxide, and their modified forms. Solid phase microextraction and micro SPE (µSPE) methods based on graphene are discussed.

  15. Regenerable solid imine sorbents

    Science.gov (United States)

    Gray, McMahan; Champagne, Kenneth J.; Fauth, Daniel; Beckman, Eric

    2013-09-10

    Two new classes of amine-based sorbents are disclosed. The first class comprises new polymer-immobilized tertiary amine sorbents; the second class new polymer-bound amine sorbents. Both classes are tailored to facilitate removal of acid anhydrides, especially carbon dioxide (CO.sub.2), from effluent gases. The amines adsorb acid anhydrides in a 1:1 molar ratio. Both classes of amine sorbents adsorb in the temperature range from about 20.degree. C. upwards to 90.degree. C. and can be regenerated by heating upwards to 100.degree. C.

  16. Evaluation of alternative sorbents for dispersive solid-phase extraction clean-up in the QuEChERS method for the determination of pesticide residues in rice by liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Cabrera, Liziara da C; Caldas, Sergiane S; Prestes, Osmar D; Primel, Ednei G; Zanella, Renato

    2016-05-01

    Many compounds are used for pest control during the production and storage of rice, making it necessary to employ multiclass methods for pesticide residues determination. For this purpose, QuEChERS-based methods are very efficient, fast and accurate, and improvements in the clean-up step are important, especially for complex matrices, like cereals. In this work, different sorbents such as chitosan, florisil(®) , alumina, diatomaceous earth, graphitized carbon black, besides the commonly used primary secondary amine and octadecylsilane, were evaluated for dispersive solid-phase extraction clean-up in acetate-buffered QuEChERS method for the determination of residues of 20 representative pesticides and one metabolite in rice by liquid chromatography coupled to tandem mass spectrometry. The sorbent C18 presented the best results, however, chitosan showed similar results, and the best performance among the unconventional sorbents evaluated. The method limit of quantification, attending accuracy (70-120% recovery) and precision (RSD ≤20%) criteria, ranged from 5 to 20 μg/kg. Results showed that chitosan is an effective alternative to reduce analysis costs, maintaining the method reliability and accuracy.

  17. Monodisperse silica nanoparticles coated with gold nanoparticles as a sorbent for the extraction of phenol and dihydroxybenzenes from water samples based on dispersive micro-solid-phase extraction: Response surface methodology.

    Science.gov (United States)

    Khezeli, Tahere; Daneshfar, Ali

    2015-08-01

    A selective and sensitive method was developed based on dispersive micro-solid-phase extraction for the extraction of hydroquinone, resorcinol, pyrocatechol and phenol from water samples prior to high-performance liquid chromatography with UV detection. SiO2 , SiO2 @MPTES, and SiO2 @MPTES@Au nanoparticles (MPTES = 3-mercaptopropyltriethoxysilane) were synthesized and characterized by scanning electronic microscopy, thermogravimetric analysis, differential thermogravimetric analysis, and infrared spectroscopy. Variables such as the amount of sorbent (mg), pH and ionic strength of sample the solution, the volume of eluent solvent (μL), vortex and ultrasonic times (min) were investigated by Plackett-Burman design. The significant variables optimized by a Box-Behnken design were combined by a desirability function. Under optimized conditions, the calibration graphs of phenol and dihydroxybenzenes were linear in a concentration range of 1-500 μg/L, and with correlation coefficients more than 0.995. The limits of detection for hydroquinone, resorcinol, pyrocatechol, and phenol were 0.54, 0.58, 0.46, and 1.24 μg/L, and the limits of quantification were 1.81, 1.93, 1.54, and 4.23 μg/L, respectively. This procedure was successfully employed to determine target analytes in spiked water samples; the relative mean recoveries ranged from 93.5 to 98.9%.

  18. On-line solid phase extraction using ion-pair microparticles combined with ICP-OES for the simultaneous preconcentration and determination of uranium and thorium

    Energy Technology Data Exchange (ETDEWEB)

    Yousefi, Seyed Reza; Zolfonoun, Ehsan [Nuclear Science and Technology Research Institute, Tehran (Iran, Islamic Republic of). NFCRS

    2016-07-01

    In this work, after on-line and in-situ solid phase extraction technique was used for the extraction and preconcentration of uranium and thorium from aqueous samples prior to inductively coupled plasma optical emission spectrometry (ICP-OES) determination. In this method, sodium hexafluorophosphate (as an ion-pairing agent) was added to the sample solution containing the cationic surfactant (dodecyltrimethylammonium bromide) and the complexing agent (dibenzoylmethane). A cloudy solution was formed as a result of formation of an ion pair between surfactant and hexafluorophosphate. The solid microparticles were passed through a microcolumn filter and the adsorbed microparticles were subsequently eluted with acid, which was directly introduced into the ICP-OES nebulizer. The main variables affecting the pre-concentration and determination steps of uranium and thorium were studied and optimized. Under the optimum conditions, the enhancement factors of 97 and 95 and the detection limits of 0.52 and 0.21 μg L{sup -1} were obtained for uranium and thorium, respectively.

  19. Stability of arsenic peptides in plant extracts: off-line versus on-line parallel elemental and molecular mass spectrometric detection for liquid chromatographic separation.

    Science.gov (United States)

    Bluemlein, Katharina; Raab, Andrea; Feldmann, Jörg

    2009-01-01

    The instability of metal and metalloid complexes during analytical processes has always been an issue of an uncertainty regarding their speciation in plant extracts. Two different speciation protocols were compared regarding the analysis of arsenic phytochelatin (As(III)PC) complexes in fresh plant material. As the final step for separation/detection both methods used RP-HPLC simultaneously coupled to ICP-MS and ES-MS. However, one method was the often used off-line approach using two-dimensional separation, i.e. a pre-cleaning step using size-exclusion chromatography with subsequent fraction collection and freeze-drying prior to the analysis using RP-HPLC-ICP-MS and/or ES-MS. This approach revealed that less than 2% of the total arsenic was bound to peptides such as phytochelatins in the root extract of an arsenate exposed Thunbergia alata, whereas the direct on-line method showed that 83% of arsenic was bound to peptides, mainly as As(III)PC(3) and (GS)As(III)PC(2). Key analytical factors were identified which destabilise the As(III)PCs. The low pH of the mobile phase (0.1% formic acid) using RP-HPLC-ICP-MS/ES-MS stabilises the arsenic peptide complexes in the plant extract as well as the free peptide concentration, as shown by the kinetic disintegration study of the model compound As(III)(GS)(3) at pH 2.2 and 3.8. But only short half-lives of only a few hours were determined for the arsenic glutathione complex. Although As(III)PC(3) showed a ten times higher half-life (23 h) in a plant extract, the pre-cleaning step with subsequent fractionation in a mobile phase of pH 5.6 contributes to the destabilisation of the arsenic peptides in the off-line method. Furthermore, it was found that during a freeze-drying process more than 90% of an As(III)PC(3) complex and smaller free peptides such as PC(2) and PC(3) can be lost. Although the two-dimensional off-line method has been used successfully for other metal complexes, it is concluded here that the fractionation and

  20. Sorbent Scoping Studies

    Energy Technology Data Exchange (ETDEWEB)

    Chancellor, Christopher John [Los Alamos National Lab. (LANL), Carlsbad, NM (United States). Difficult Waste Team

    2016-11-14

    The Los Alamos National Laboratory – Carlsbad Operations (LANL-CO) office was tasked by the DOE CBFO, Office of the Manager to: • Perform a review of the acceptable knowledge (AK) to identify the oxidizers and sorbents in transuranic (TRU) waste streams. • Conduct scoping studies on the oxidizers and sorbents identified in AK review to inform the Quality Level 1 (QL1) testing. • Conduct a series of QL1 tests to provide the scientific data to support a basis of knowledge document for determining the criteria for: 1) accepting waste at the Waste Isolation Pilot Plant (WIPP) without treatment, 2) determining waste that will require treatment, and 3) if treatment is required, how the treatment must be performed. The purpose of this report is to present the results of the AK review of sorbents present in active waste streams, provide a technical analysis of the sorbent list, report the results of the scoping studies for the fastest burning organic sorbent, and provide the list of organic and inorganic sorbents to be used in the development of a Test Plan for Preparation and Testing of Sorbents Mixed with Oxidizer found in Transuranic Waste (DWT-TP-001). The companion report, DWT-RPT-001, Oxidizer Scoping Studies, has similar information for oxidizers identified during the AK review of TRU waste streams. The results of the oxidizer and sorbent scoping studies will be used to inform the QL1 test plan. The QL1 test results will support the development of a basis of knowledge document that will evaluate oxidizing chemicals and sorbents in TRU waste and provide guidance for treatment.

  1. Modified clay sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Fogler, H.S.; Srinivasan, K.R.

    1990-04-10

    This patent describes a clay-based sorbent. It comprises a clay having an external surface and lamellar layers; and cationic surfactant ions having a hydrocarbon portion and a cationic head portion, the cationic surfactant ions being irreversibly bound to the external surface by the hydrocarbon portion. This patent also describes cetylpyridinium-aluminum hydroxy-montmorillonite; the clay-based sorbent wherein the clay is a non-expandable clay; and the clay-based sorbent wherein the cationic surfactant ions are selected from the group consisting of ionized cetylpyridinium chloride and cetylakonium chloride.

  2. Ultraviolet vapor generation atomic fluorescence spectrometric determination of mercury in natural water with enrichment by on-line solid phase extraction

    Science.gov (United States)

    Qin, Deyuan; Gao, Feng; Zhang, Zhaohui; Zhao, Liqian; Liu, Jixin; Ye, Jianping; Li, Junwei; Zheng, Fengxi

    2013-10-01

    A novel method, which coupled an on-line solid phase extraction (SPE) enrichment with ultraviolet vapor generation (UVG) atomic fluorescence spectrometry (AFS), was developed to improve the sensitivity of mercury determination and to remove the interference of some anion and organics to UVG of mercury. A high mercury retention efficiency and maximum exclusion of inorganic and organic matrix in water samples were achieved by using C18 SPE mini cartridge modified with sodium diethyldithiocarbamate (DDTC). Fast and efficient elution from the cartridge was found by using L-cysteine mixing solution. Furthermore, through the investigation of different UV reactor designs, the most important factor was the structure of the reactor (which corresponded roughly to the photon flux) wherein the tubing was sintered into the UV lamp to give the highest UV generation efficiency. The second factor was the materials of the tubing (which roughly corresponded to the working wavelength). Synthetic quartz, characterized by the highest transparency at 185 nm, attained the highest UVG efficiency, suggesting that the most favorable wavelength for UVG was 185 nm. Under optimum conditions, the achievable detection limit (3σ) with sample loadings of 10.0 mL was 0.03 ng L- 1 and 0.08 ng L- 1 with different manifolds, respectively. The method was successfully applied to the determination of Hg in tap water, river water and lake water samples.

  3. Automated determination of total captopril in urine by liquid chromatography with post-column derivatization coupled to on-line solid phase extraction in a sequential injection manifold.

    Science.gov (United States)

    Karakosta, Theano D; Tzanavaras, Paraskevas D; Themelis, Demetrius G

    2012-01-15

    The present study reports a new liquid chromatographic (HPLC) method for the determination of the anti-hypertension drug captopril (CAP) in human urine. After its separation from the sample matrix in a reversed phase HPLC column, CAP reacts with the thiol-selective reagent ethyl-propiolate (EP) in a post-column configuration and the formed thioacrylate derivative is detected at 285 nm. Automated 4-fold preconcentration of the analyte prior to analysis was achieved by an on-line solid phase extraction (SPE) step using a sequential injection (SI) manifold. The Oasis HLB SPE cartridges offered quantitative recoveries and effective sample cleaning by applying a simple SPE protocol. The limits of detection and quantitation were 10 μg L(-1) and 35 μg L(-1) respectively. The percent recoveries for the analysis of human urine samples ranged between 90 and 96% and 95 and 104% using aqueous and matrix matched calibration curves respectively. Copyright © 2011 Elsevier B.V. All rights reserved.

  4. On-line monitoring of the photocatalytic degradation of 2,4-D and dicamba using a solid-phase extraction-multisyringe flow injection system.

    Science.gov (United States)

    Chávez-Moreno, Carmín; Ferrer, Laura; Hinojosa-Reyes, Laura; Hernández-Ramírez, Aracely; Cerdà, Víctor; Guzmán-Mar, Jorge

    2013-11-15

    A fully automated on-line system for monitoring the photocatalytic degradation of herbicides was developed using multisyringe flow injection analysis (MSFIA) coupled to a solid phase extraction (SPE) unit with UV detection. The calibration curves were linear in the concentration range of 100-1000 μg L(-1) for 3,6-dichloro-2-methoxybenzoic acid (dicamba) and 500-3000 μg L(-1) for 2,4-dichlorophenoxyacetic acid (2,4-D), while the detection limits were 30 and 135 μg L(-1) for dicamba and 2,4-D, respectively. The monitoring of the photocatalytic degradation (TiO2 anatase/UV 254 nm) of these two herbicides was performed by MSFIA-SPE system using a small sample volume (2 mL) in a fully automated approach. The degradation was assessed in ultrapure and drinking water with initial concentrations of 1000 and 2000 μg L(-1) for dicamba and 2,4-D, respectively. Degradation percentages of approximately 85% were obtained for both herbicides in ultrapure water after 45 min of photocatalytic treatment. A similar degradation efficiency in drinking water was observed for 2,4-D, whereas dicamba exhibited a lower degradation percentage (75%), which could be attributed to the presence of inorganic species in this kind of water. Copyright © 2013 Elsevier Ltd. All rights reserved.

  5. Interfacing on-line solid phase extraction with monolithic column multisyringe chromatography and chemiluminescence detection: An effective tool for fast, sensitive and selective determination of thiazide diuretics.

    Science.gov (United States)

    Maya, Fernando; Estela, José Manuel; Cerdà, Víctor

    2010-01-15

    A new, multisyringe flow injection set-up has been developed for the completely automated determination of trace thiazide compounds with diuretic action in different types of samples. The proposed instrumental set-up exploits for the first time, a low pressure on-line solid phase extraction-liquid chromatography-chemiluminescence detection method. This novel combination of sample treatments in flow systems expands the current applicability of low pressure liquid chromatography due to the isolation/preconcentration of the target compounds, besides high selectivity and sensitivity. For the determination of three thiazide compounds named hydroflumethiazide, furosemide and bendroflumethiazide, the proposed set-up provided with the preconcentration of only 1mL of sample, limits of detection of 3, 60 and 40microgL(-1), respectively. Furthermore wide linear dynamic ranges of 6-4000, 140-20,000 and 90-40,000microgL(-1), respectively, were obtained. Besides of this, a high injection throughput of 12h(-1) was also achieved. As in sports, thiazide diuretics are prohibited substances, the proposed method has been applied to their determination in urine samples. Furthermore the potential of the proposed method as a fast-screening approach for emerging contaminants in waters has been also tested by applying it to well water and leachates from a solid waste landfill.

  6. Determination of biocides and pesticides by on-line solid phase extraction coupled with mass spectrometry and their behaviour in wastewater and surface water

    Energy Technology Data Exchange (ETDEWEB)

    Singer, Heinz; Jaus, Sylvia; Hanke, Irene; Lueck, Alfred; Hollender, Juliane [Eawag, Swiss Federal Institute of Aquatic Science and Technology, Ueberlandstrasse 133, CH-8600 Duebendorf (Switzerland); Alder, Alfredo C., E-mail: alfredo.alder@eawag.c [Eawag, Swiss Federal Institute of Aquatic Science and Technology, Ueberlandstrasse 133, CH-8600 Duebendorf (Switzerland)

    2010-10-15

    This study focused on the input of hydrophilic biocides into the aquatic environment and on the efficiency of their removal in conventional wastewater treatment by a mass flux analysis. A fully automated method consisting of on-line solid phase extraction coupled to LC-ESI-MS/MS was developed and validated for the simultaneous trace determination of different biocidal compounds (1,2-benzisothiazoline-3-one (BIT), 3-Iodo-2-propynylbutyl-carbamate (IPBC), irgarol 1051 and 2-N-octyl-4-isothiazolinone (octhilinone, OIT), carbendazim, diazinon, diuron, isoproturon, mecoprop, terbutryn and terbutylazine) and pharmaceuticals (diclofenac and sulfamethoxazole) in wastewater and surface water. In the tertiary effluent, the highest average concentrations were determined for mecoprop (1010 ng/L) which was at comparable levels as the pharmaceuticals diclofenac (690 ng/L) and sulfamethoxazole (140 ng/L) but 1-2 orders of magnitude higher than the other biocidal compounds. Average eliminations for all compounds were usually below 50%. During rain events, increased residual amounts of biocidal contaminants are discharged to receiving surface waters. - Incomplete removal of biocides and pesticides during wastewater treatment.

  7. Parallel extraction columns and parallel analytical columns coupled with liquid chromatography/tandem mass spectrometry for on-line simultaneous quantification of a drug candidate and its six metabolites in dog plasma.

    Science.gov (United States)

    Xia, Y Q; Hop, C E; Liu, D Q; Vincent, S H; Chiu, S H

    2001-01-01

    A method with parallel extraction columns and parallel analytical columns (PEC-PAC) for on-line high-flow liquid chromatography/tandem mass spectrometry (LC/MS/MS) was developed and validated for simultaneous quantification of a drug candidate and its six metabolites in dog plasma. Two on-line extraction columns were used in parallel for sample extraction and two analytical columns were used in parallel for separation and analysis. The plasma samples, after addition of an internal standard solution, were directly injected onto the PEC-PAC system for purification and analysis. This method allowed the use of one of the extraction columns for analyte purification while the other was being equilibrated. Similarly, one of the analytical columns was employed to separate the analytes while the other was undergoing equilibration. Therefore, the time needed for re-conditioning both extraction and analytical columns was not added to the total analysis time, which resulted in a shorter run time and higher throughput. Moreover, the on-line column extraction LC/MS/MS method made it possible to extract and analyze all seven analytes simultaneously with good precision and accuracy despite their chemical class diversity that included primary, secondary and tertiary amines, an alcohol, an aldehyde and a carboxylic acid. The method was validated with the standard curve ranging from 5.00 to 5000 ng/mL. The intra- and inter-day precision was no more than 8% CV and the assay accuracy was between 95 and 107%.

  8. Mercury removal sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Alptekin, Gokhan

    2016-03-29

    Sorbents and methods of using them for removing mercury from flue gases over a wide range of temperatures are disclosed. Sorbent materials of this invention comprise oxy- or hydroxyl-halogen (chlorides and bromides) of manganese, copper and calcium as the active phase for Hg.sup.0 oxidation, and are dispersed on a high surface porous supports. In addition to the powder activated carbons (PACs), this support material can be comprised of commercial ceramic supports such as silica (SiO.sub.2), alumina (Al.sub.2O.sub.3), zeolites and clays. The support material may also comprise of oxides of various metals such as iron, manganese, and calcium. The non-carbon sorbents of the invention can be easily injected into the flue gas and recovered in the Particulate Control Device (PCD) along with the fly ash without altering the properties of the by-product fly ash enabling its use as a cement additive. Sorbent materials of this invention effectively remove both elemental and oxidized forms of mercury from flue gases and can be used at elevated temperatures. The sorbent combines an oxidation catalyst and a sorbent in the same particle to both oxidize the mercury and then immobilize it.

  9. An automated method for the analysis of phenolic acids in plasma based on ion-pairing micro-extraction coupled on-line to gas chromatography/mass spectrometry with in-liner derivatisation

    NARCIS (Netherlands)

    Peters, S.; Kaal, E.; Horsting, I.; Janssen, H.-G.

    2012-01-01

    A new method is presented for the analysis of phenolic acids in plasma based on ion-pairing ‘Micro-extraction in packed sorbent’ (MEPS) coupled on-line to in-liner derivatisation-gas chromatography-mass spectrometry (GC-MS). The ion-pairing reagent served a dual purpose. It was used both to improve

  10. On-line preconcentration and determination of tetracycline residues in milk using solid-phase extraction in conjunction with flow injection spectrophotometry

    Directory of Open Access Journals (Sweden)

    Prinya Masawat

    2008-07-01

    Full Text Available A simple, cheap and highly sensitive system with on-line preconcentration using solid-phase extraction in conjunction with flow injection spectrophotometry for the determination of tetracycline residues in milk samples is described. C18 was used as packing material in a designed minicolumn used for preconcentration of tetracyclines. Tetracycline standard or sample solutions were dissolved in a mixed buffer solution of pH 4.0 containing boric acid, citric acid and sodium phosphate, then loaded to the minicolumn for 6 min followed by elution with a solution containing methanol : mixed buffer solution (40:60 by volume of pH 6.5 The absorbance of the eluate was measured at 370 nm. The calibration graph was linear in the range of 0.20-1.00, 0.20-4.00, and 0.20-1.00 mg L-1 for tetracycline (TC, oxytetracycline (OTC, and chlortetracycline (CTC respectively. The limits of detection were 0.08, 0.10, and 0.09mg L-1 for TC, OTC, and CTC respectively. Relative standard deviations for 20 replicated determinations of 0.20, 0.40, and 0.60 mg L-1 of TC were 7.03, 7.23, and 6.55 % respectively. Per cent recoveries for four commercial types of milk: U.H.T., pasteurised, raw, and sterilised milk were in the range of 86–109 (TC, 90–109 (OTC, and 89–108 (CTC. The sample throughput was 6 h-1.

  11. Occurrence of the herbicide glyphosate and its metabolite AMPA in surface waters in Switzerland determined with on-line solid phase extraction LC-MS/MS.

    Science.gov (United States)

    Poiger, Thomas; Buerge, Ignaz J; Bächli, Astrid; Müller, Markus D; Balmer, Marianne E

    2017-01-01

    Glyphosate is currently one of the most important herbicides worldwide. Its unique properties provide for a wide range of uses in agriculture but also in non-agricultural areas. At the same time, its zwitterionic nature prevents the inclusion in multi-residue analytical methods for environmental monitoring. Consequently, despite its extensive use, data on occurrence of glyphosate in the aquatic environment is still scarce. Based on existing methods, we developed a simplified procedure for the determination of glyphosate and its main metabolite aminomethylphosphonic acid (AMPA) in water samples using derivatization with fluorenylmethyl chloroformate FMOC-Cl, combined with on-line solid phase extraction and liquid chromatography-tandem mass spectrometry (LC-MS/MS) detection. This method was extensively tested on over 1000 samples of surface water, groundwater, and treated wastewater and proved to be simple, sensitive, and reliable. Limits of quantification of 0.005 μg/L were routinely achieved. Glyphosate and AMPA were detected in the vast majority of stream water samples in the area of Zurich, Switzerland, with median concentrations of 0.11 and 0.20 μg/L and 95th percentile concentrations of 2.1 and 2.6 μg/L, respectively. Stream water data and data from treated wastewater indicated that non-agricultural uses may significantly contribute to the overall loads of glyphosate and AMPA in surface waters. In the investigated groundwater samples, selected specifically because they had shown presence of other herbicides in previous monitoring programs, glyphosate and AMPA were generally not detected, except for two monitoring sites in Karst aquifers, indicating that these compounds show much less tendency for leaching.

  12. On-line cloud point extraction combined with electrothermal vaporization inductively coupled plasma atomic emission spectrometry for the speciation of inorganic antimony in environmental and biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Li Yingjie [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin [Department of Chemistry, Wuhan University, Wuhan 430072 (China)]. E-mail: binhu@whu.edu.cn; Jiang Zucheng [Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2006-08-25

    A new method for the determination of inorganic Sb species by on-line cloud point extraction combined with electrothermal vaporization inductively coupled plasma atomic emission spectrometry (ETV-ICP-AES) is presented and evaluated. The method is based on the complexation of Sb(III) with pyrrolidine dithiocarbamate (PDC) which form an hydrophobic complex at pH 5.5 and subsequently enter surfactant-rich phase at pH 5.5, whereas Sb(V) remained in aqueous solutions. The preconcentration step is mediated by micelles of the non-ionic surfactant Triton X-114 with ammonium pyrrolidine dithiocarbamate (APDC). The micellar system containing the complex was loaded into the FIA manifold at a flow rate of 2.5 mL min{sup -1}, and the surfactant-rich phase was retained in a microcolumn packed with absorbent cotton, at pH 5.5. After the surfactant-rich phase was eluted with 100 {mu}L acetonitrile, it was determined by ETV-ICP-AES. Sb(V) is reduced to Sb(III) by L-cysteine prior to determined total Sb, and its assay is based on subtracting Sb(III) from total antimony. The main factors affecting separation/preconcentration and the vaporization behavior of analyte in graphite tube were investigated in detail. Under the optimized conditions, the precision relative standard deviation (R.S.D.) for eight replicate measurements of 0.2 {mu}g mL{sup -1} Sb(III) was 4.3%. The apparent concentration factor, which is defined as the concentration ratio of the analyte in the final diluted surfactant-rich extract ready for ETV-ICP-AES detection and in the initial solution, was 872 for Sb(III). The limit of detection (LOD) for Sb(III) was 0.09 {mu}g L{sup -1}. The proposed method was successfully applied for the speciation of inorganic antimony in different water samples and urine sample with satisfactory results.

  13. Cloud point extraction with/without chelating agent on-line coupled with inductively coupled plasma optical emission spectrometry for the determination of trace rare earth elements in biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Li Yingjie [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin, E-mail: binhu@whu.edu.cn [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2010-02-15

    The on-line incorporation of cloud point extraction (CPE) with/without 8-hydroxyquinoline (8-Ox) as chelating agent into flow injection analysis associated with inductively coupled plasma optical emission spectrometry (ICP-OES) for determining trace rare earth elements (REEs) is presented and evaluated. The significant parameters affecting on-line cloud point extraction of REEs such as sample pH, flow rate, 8-Ox concentration, Triton X-114 concentration were systematically studied. Under the optimized conditions, with the consumption of 3.0 mL sample solution, the limits of detection (3{sigma}) were ranged from 41.4 pg mL{sup -1} (Yb) to 448 pg mL{sup -1} (Gd) with relative standard deviations (RSDs) of 1.0% (Eu)-5.9% (Sm) for on-line CPE-ICP-OES with 8-Ox as chelating agent, and 69.0 pg mL{sup -1} (Sc) to 509.5 pg mL{sup -1} (Sm) with RSDs of 2.9% (Yb)-7.5% (Ho) for on-line CPE-ICP-OES without 8-Ox as chelating agent, respectively. The sample throughput of 17 samples h{sup -1} was obtained for both systems. The developed methods of on-line CPE-ICP-OES were validated by the analysis of certified reference material (GBW07605, tea leaves) and real biological samples of pig liver, Auricularia auricula and mushroom.

  14. Chitosan film loaded with silver nanoparticles-sorbent for solid phase extraction of Al(III), Cd(II), Cu(II), Co(II), Fe(III), Ni(II), Pb(II) and Zn(II).

    Science.gov (United States)

    Djerahov, Lubomir; Vasileva, Penka; Karadjova, Irina; Kurakalva, Rama Mohan; Aradhi, Keshav Krishna

    2016-08-20

    The present study describes the ecofriendly method for the preparation of chitosan film loaded with silver nanoparticles (CS-AgNPs) and application of this film as efficient sorbent for separation and enrichment of Al(III), Cd(II), Cu(II), Co(II), Fe(III), Ni(II), Pb(II) and Zn(II). The stable CS-AgNPs colloid was prepared by dispersing the AgNPs sol in chitosan solution at appropriate ratio and further used to obtain a cast film with very good stability under storage and good mechanical strength for easy handling in aqueous medium. The incorporation of AgNPs in the structure of CS film and interaction between the polymer matrix and nanoparticles were confirmed by UV-vis and FTIR spectroscopy. The homogeneously embedded AgNPs (average diameter 29nm, TEM analysis) were clearly observed throughout the film by SEM. The CS-AgNPs nanocomposite film shows high sorption activity toward trace metals under optimized chemical conditions. The results suggest that the CS-AgNPs nanocomposite film can be feasibly used as a novel sorbent material for solid-phase extraction of metal pollutants from surface waters.

  15. Ultrasound assisted extraction of Maxilon Red GRL dye from water samples using cobalt ferrite nanoparticles loaded on activated carbon as sorbent: Optimization and modeling.

    Science.gov (United States)

    Mehrabi, Fatemeh; Vafaei, Azam; Ghaedi, Mehrorang; Ghaedi, Abdol Mohammad; Alipanahpour Dil, Ebrahim; Asfaram, Arash

    2017-09-01

    In this research, a selective, simple and rapid ultrasound assisted dispersive solid-phase micro-microextraction (UA-DSPME) was developed using cobalt ferrite nanoparticles loaded on activated carbon (CoFe2O4-NPs-AC) as an efficient sorbent for the preconcentration and determination of Maxilon Red GRL (MR-GRL) dye. The properties of sorbent are characterized by X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), Vibrating sample magnetometers (VSM), Fourier transform infrared spectroscopy (FTIR), Particle size distribution (PSD) and Scanning Electron Microscope (SEM) techniques. The factors affecting on the determination of MR-GRL dye were investigated and optimized by central composite design (CCD) and artificial neural networks based on genetic algorithm (ANN-GA). CCD and ANN-GA were used for optimization. Using ANN-GA, optimum conditions were set at 6.70, 1.2mg, 5.5min and 174μL for pH, sorbent amount, sonication time and volume of eluent, respectively. Under the optimized conditions obtained from ANN-GA, the method exhibited a linear dynamic range of 30-3000ngmL(-1) with a detection limit of 5.70ngmL(-1). The preconcentration factor and enrichment factor were 57.47 and 93.54, respectively with relative standard deviations (RSDs) less than 4.0% (N=6). The interference effect of some ions and dyes was also investigated and the results show a good selectivity for this method. Finally, the method was successfully applied to the preconcentration and determination of Maxilon Red GRL in water and wastewater samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Zeolite/iron oxide composite as sorbent for magnetic solid-phase extraction of benzene, toluene, ethylbenzene and xylenes from water samples prior to gas chromatography⬜mass spectrometry.

    Science.gov (United States)

    Fernández, Elena; Vidal, Lorena; Canals, Antonio

    2016-08-05

    This study reports a new composite based on ZSM-5 zeolite decorated with iron oxide magnetic nanoparticles as a valuable sorbent for magnetic solid-phase extraction (MSPE). A proposal is made to determine benzene, toluene, ethylbenzene and xylenes (BTEX) as model analytes in water samples using gas chromatography-mass spectrometry. A two-step multivariate optimization strategy, using Plackett⬜Burman and circumscribed central composite designs, was employed to optimize experimental parameters affecting MSPE. The method was evaluated under optimized extraction conditions (i.e., amount of sorbent, 138mg; extraction time, 11min; sample pH, pH of water (i.e., 5.5⬜6.5); eluent solvent volume, 0.5mL; and elution time, 5min), obtaining a linear response from 1 to 100μgL(↙1) for benzene; from 10 to 100μgL(↙1) for toluene, ethylbenzene and o-xylene; and from 10 to 75μgL(↙1) for m,p-xylene. The repeatability of the proposed method was evaluated at a 40μgL(↙1) spiking level and coefficients of variation ranged between 8 and 11% (n=5). Limits of detection were found to be 0.3μgL(↙1) for benzene and 3μgL(↙1) for the other analytes. These values satisfy the current normative of the Environmental Protection Agency and European Union for BTEX content in waters for human consumption. Finally, drinking water, wastewater and river water were selected as real water samples to assess the applicability of the method. Relative recoveries varied between 85% and 114% showing negligible matrix effects.

  17. ADVANCED SORBENT DEVELOPMENT

    Energy Technology Data Exchange (ETDEWEB)

    Javad Abbasian

    2000-01-01

    The overall objective of this program was to develop regenerable sorbents for use in the temperature range of 343 to 538 C (650 to 1000 F) to remove hydrogen sulfide (H{sub 2}S) from coal-derived fuel gases in a fluidized-bed reactor. The goal was to develop sorbents that are capable of reducing the H{sub 2}S level in the fuel gas to less than 20 ppmv in the specified temperature range and pressures in the range of 1 to 20 atmospheres, with chemical characteristics that permit cyclic regeneration over many cycles without a drastic loss of activity, as well as physical, characteristics that are compatible with the fluidized bed application. This topical report focuses on the investigation directed toward preparation of zinc-based sorbents using the sol-gel approach that has been shown to require only a moderate temperature for calcination, while resulting in significantly more attrition-resistant sorbents. The sorbents prepared in this part of the investigation and the results from their evaluation in packed-bed and fluidized-bed reactors are described in this report.

  18. Development of an on-line coupling of liquid-liquid extraction, normal-phase liquid chromatography and high-resolution gas chromatography producing an analytical marker for the prediction of mutagenicity and carcinogenicity of bitumen and bitumen fumes.

    Science.gov (United States)

    Blomberg, J; de Groot, P C; Brandt, H C; van der Does, J J; Schoenmakers, P J

    1999-07-23

    A fast and fully automated system for the determination of polycyclic aromatic compounds (PACs) is described. The system has been developed to produce an analytical 'marker', correlating chemical characteristics (including PAC analysis) with mutagenicity and carcinogenicity. The products of interest are bitumen fumes, bitumen and other (heavy or even residual) oil products, regardless of their boiling range. Dimethyl sulphoxide (DMSO) extractables obtained from a flow-injection analysis (FIA) system are introduced on-line in a normal-phase liquid chromatographic (NPLC) system. Here, the PACs are separated from the DMSO and possible co-extracted heavy residual species. The final step incorporates on-line gas chromatographic analysis of the three-to-six-ring PAC fraction, followed by flame-ionisation detection for quantification. It was demonstrated that data obtained from samples in the distillate lubrication-oil range correlate well with data obtained from the manual DMSO-extraction method standardised by the Institute of Petroleum as IP346.

  19. Determination of As(III) and total inorganic As in water samples using an on-line solid phase extraction and flow injection hydride generation atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sigrist, Mirna, E-mail: msigrist@fiq.unl.edu.ar [Laboratorio Central, Facultad de Ingenieria Quimica, Universidad Nacional del Litoral, Santiago del Estero 2654-Piso 6, (3000) Santa Fe (Argentina); Albertengo, Antonela; Beldomenico, Horacio [Laboratorio Central, Facultad de Ingenieria Quimica, Universidad Nacional del Litoral, Santiago del Estero 2654-Piso 6, (3000) Santa Fe (Argentina); Tudino, Mabel [Laboratorio de Analisis de Trazas, Departamento de Quimica Inorganica, Analitica y Quimica Fisica/INQUIMAE, Facultad de Ciencias Exactas y Naturales, Pabellon II, Ciudad Universitaria (1428), Buenos Aires (Argentina)

    2011-04-15

    A simple and robust on-line sequential injection system based on solid phase extraction (SPE) coupled to a flow injection hydride generation atomic absorption spectrometer (FI-HGAAS) with a heated quartz tube atomizer (QTA) was developed and optimized for the determination of As(III) in groundwater without any kind of sample pretreatment. The method was based on the selective retention of inorganic As(V) that was carried out by passing the filtered original sample through a cartridge containing a chloride-form strong anion exchanger. Thus the most toxic form, inorganic As(III), was determined fast and directly by AsH{sub 3} generation using 3.5 mol L{sup -1} HCl as carrier solution and 0.35% (m/v) NaBH{sub 4} in 0.025% NaOH as the reductant. Since the uptake of As(V) should be interfered by several anions of natural occurrence in waters, the effect of Cl{sup -}, SO{sub 4}{sup 2-}, NO{sub 3}{sup -}, HPO{sub 4}{sup 2-}, HCO{sub 3}{sup -} on retention was evaluated and discussed. The total soluble inorganic arsenic concentration was determined on aliquots of filtered samples acidified with concentrated HCl and pre-reduced with 5% KI-5% C{sub 6}H{sub 8}O{sub 6} solution. The concentration of As(V) was calculated by difference between the total soluble inorganic arsenic and As(III) concentrations. Detection limits (LODs) of 0.5 {mu}g L{sup -1} and 0.6 {mu}g L{sup -1} for As(III) and inorganic total As, respectively, were obtained for a 500 {mu}L sample volume. The obtained limits of detection allowed testing the water quality according to the national and international regulations. The analytical recovery for water samples spiked with As(III) ranged between 98% and 106%. The sampling throughput for As(III) determination was 60 samples h{sup -1}. The device for groundwater sampling was especially designed for the authors. Metallic components were avoided and the contact between the sample and the atmospheric oxygen was carried to a minimum. On-field arsenic species

  20. Space-filling polyhedral sorbents

    Science.gov (United States)

    Haaland, Peter

    2016-06-21

    Solid sorbents, systems, and methods for pumping, storage, and purification of gases are disclosed. They derive from the dynamics of porous and free convection for specific gas/sorbent combinations and use space filling polyhedral microliths with facial aplanarities to produce sorbent arrays with interpenetrating interstitial manifolds of voids.

  1. Development and validation of a solid-phase extraction method using anion exchange sorbent for the analysis of cannabinoids in plasma and serum by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Gasse, Angela; Pfeiffer, Heidi; Köhler, Helga; Schürenkamp, Jennifer

    2016-07-01

    The aim of this work was to develop and validate a solid-phase extraction (SPE) method for the analysis of cannabinoids with emphasis on a very extensive and effective matrix reduction in order to ensure constant good results in selectivity and sensitivity regardless of the applied measuring technology. This was obtained by the use of an anion exchange sorbent (AXS) and the purposive ionic interaction between matrix components and this sorbent material. In a first step, the neutral cannabinoids ∆9-tetrahydrocannabinol (THC) and 11-hydroxy-∆9-tetrahydrocannabinol (11-OH-THC) were eluted, leaving 11-nor-9-carboxy-∆9-tetrahydrocannabinol (THC-COOH) and the main interfering matrix components bound to the AXS. In a second step, exploiting differences in pH and polarity, it was possible to separate matrix components and THC-COOH, thereby yielding a clean elution of THC-COOH into the same collecting tube as THC and 11-OH-THC. Even when using a simple measuring technology like gas chromatography with single quadrupole mass spectrometry, this two-step elution allows for an obvious decrease in number and intensity of matrix interference in the chromatogram. Hence, in both plasma and serum, the AXS extracts resulted in very good selectivity. Limits of detection and limits of quantification were below 0.25 and 0.35 ng/mL for the neutral cannabinoids in both matrices, 2.0 and 3.0 ng/mL in plasma and 1.6 and 3.3 ng/mL in serum for THC-COOH. The recoveries were ≥79.8 % for all analytes. Interday and intraday imprecisions ranged from 0.8 to 6.1 % relative standard deviation, and accuracy bias ranged from -12.6 to 3.6 %.

  2. THE RESEARCH OF SORBENT PROPERTIES OF MODIFIED PEAT OF TOMSK REGION

    OpenAIRE

    CHUHAREVA N.V.; MARTYNIUK A.T.

    2012-01-01

    Extraction of different components (bitumen) from thermoprocessed up to 200-300°С peat puts the task of searching new alternative decisions of using the obtained remains. They can be used as cheap sorbent materials. The aim of this research is to estimate sorbent properties of peat remains after the extraction bitumen from them.

  3. THE RESEARCH OF SORBENT PROPERTIES OF MODIFIED PEAT OF TOMSK REGION

    Directory of Open Access Journals (Sweden)

    CHUHAREVA N.V.

    2012-01-01

    Full Text Available Extraction of different components (bitumen from thermoprocessed up to 200-300°С peat puts the task of searching new alternative decisions of using the obtained remains. They can be used as cheap sorbent materials. The aim of this research is to estimate sorbent properties of peat remains after the extraction bitumen from them.

  4. Elimination of diastereomer interference to determine Telcagepant (MK-0974) in human plasma using on-line turbulent-flow technology and off-line solid-phase extraction coupled with liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Xu, Yang; Willson, Kenneth J; Anderson, Melanie D G; Musson, Donald G; Miller-Stein, Cynthia M; Woolf, Eric J

    2009-06-01

    To eliminate the diastereomer interference on Telcagepant (MK-0974) determination during clinical study support, on-line high turbulent-flow liquid chromatography (HTLC) methods, HTLC-A and HTLC-B that covered dynamic range of 0.5-500 nM and 5-5000 nM, respectively, were developed. To meet the requirement of rapid assay transfer among multiple laboratories and analysts, a solid-phase extraction (SPE) assay was derived from the existing HTLC-B assay under the same dynamic range. The on-line HTLC assays were achieved through direct injection of plasma samples, extraction of analyte with a Cohesive C18 column (50 mm x 0.5 mm, 50 microm), followed by HPLC separation on a FluoPhase RP column (100 mm x 2.1 mm, 5 microm) and MS/MS detection. The off-line SPE assay used Waters Oasis HLB microElution plate to extract the analytes from plasma matrix before injecting on a FluoPhase RP column (150 mm x 2.1 mm, 5 microm) for LC-MS/MS analysis. Under both on-line and off-line assay conditions, the diastereomer 1c was chromatographically separated from MK-0974. Cross-validation with the pooled samples demonstrated that both on-line and off-line assays provided comparable data with a difference of pros and cons of on-line and off-line assays with regard to man power involved in sample preparation, total analysis time, carryover, cost efficiency, and the requirement for assay transfer are discussed.

  5. On-line MSPD-SPE-HPLC/FLD analysis of polycyclic aromatic hydrocarbons in bovine tissues.

    Science.gov (United States)

    Gutiérrez-Valencia, Tania M; García de Llasera, Martha P

    2017-05-15

    A fast method was optimized and validated for simultaneous trace determination of four polycyclic aromatic hydrocarbons: benzo[a]anthracene, benzo[b]fluoranthene, benzo[k]fluoranthene and benzo[a]pyrene in bovine tissues. The determination was performed by matrix solid-phase dispersion (MSPD) coupled on-line to solid phase extraction (SPE) and high performance liquid chromatography (HPLC) with fluorescence detection (FLD). The sample was dispersed on C18 silica sorbent and then the on-line MSPD-SPE-HPLC/FLD method was applied. Several parameters were optimized: cleaning and elution sequences applied to the MSPD cartridge, the flow rate and dilution of extract used for SPE loading. The on-line method was validated over a concentration range of 0.1-0.6ngg(-1) obtaining good linearity (r⩾0.998) and precision (RSD)⩽10%. Recovery ranged from 96 to 99% and the limits of detection were 0.012ngg(-1). This methodology was applied to liver samples from unhealthy animals. The results demonstrate that MSDP-SPE-HPLC/FLD method provides reliable, sensitive, accurate and fast data to the food control.

  6. Novel on-line column extraction apparatus coupled with binary peak focusing for high-performance liquid chromatography determination of rifampicin in human plasma: a strategy for therapeutic drug monitoring.

    Science.gov (United States)

    Li, Wei; Peng, Min; Long, Minghui; Qiu, Ximin; Yang, Liping

    2014-12-01

    In order to develop a method that is completely suitable for the routine therapeutic drug monitoring, a sensitive and fully automated on-line column extraction apparatus in combination with high-performance liquid chromatography allowing binary peak focusing was developed and validated for the determination of rifampicin in human plasma. Rifapentine was used as an internal standard. The analytical cycle started with the injection of 100 μL of the sample pretreated by protein precipitation in a Venusil SCX extraction column. After the elution, the analytes were transferred and concentrated in an Xtimate C18 trap column. Finally, the trapped analytes were separated by an Xtimate C18 analytical column and were analyzed by an ultraviolet detector at 336 nm. With this new strategy, continuous on-line analysis of the compounds was successfully performed. The method showed excellent performance for the analysis of rifampicin in plasma samples, including calibration curve linearity (All r were larger than 0.9996), sensitivity (lowest limit of quantification was 0.12 μg/mL), method accuracy (within 6.6% in terms of relative error), and precision (relative standard deviations of intra- and interday precision were less than 7.8%). These results demonstrated that the simple, reliable, and automatic method based on on-line column extraction and binary peak focusing is a promising approach for therapeutic drug monitoring in complex biomatrix samples.

  7. LC-HR-MS/MS standard urine screening approach: Pros and cons of automated on-line extraction by turbulent flow chromatography versus dilute-and-shoot and comparison with established urine precipitation.

    Science.gov (United States)

    Helfer, Andreas G; Michely, Julian A; Weber, Armin A; Meyer, Markus R; Maurer, Hans H

    2017-02-01

    Comprehensive urine screening for drugs and metabolites by LC-HR-MS/MS using Orbitrap technology has been described with precipitation as simple workup. In order to fasten, automate, and/or simplify the workup, on-line extraction by turbulent flow chromatography and a dilute-and-shoot approach were developed and compared. After chromatographic separation within 10min, the Q-Exactive mass spectrometer was run in full scan mode with positive/negative switching and subsequent data dependent acquisition mode. The workup approaches were validated concerning selectivity, recovery, matrix effects, process efficiency, and limits of identification and detection for typical drug representatives and metabolites. The total workup time for on-line extraction was 6min, for the dilution approach 3min. For comparison, the established urine precipitation and evaporation lasted 10min. The validation results were acceptable. The limits for on-line extraction were comparable with those described for precipitation, but lower than for dilution. Thanks to the high sensitivity of the LC-HR-MS/MS system, all three workup approaches were sufficient for comprehensive urine screening and allowed fast, reliable, and reproducible detection of cardiovascular drugs, drugs of abuse, and other CNS acting drugs after common doses.

  8. Application of Deep Eutectic Solvent Modified Cotton as a Sorbent for Online Solid-Phase Extraction and Determination of Trace Amounts of Copper and Nickel in Water and Biological Samples.

    Science.gov (United States)

    Karimi, Mehdi; Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji

    2017-03-01

    Deep eutectic solvent (DES) was used as the extractant to improve the extraction properties of cotton. DES of choline chloride-urea (ChCl-urea) was prepared and immobilized on the surface of cotton fibers. The resulting sorbent was packed on a microcolumn, and a flow injection flame atomic absorption spectrometry was designed for the online separation and determination of trace amounts of copper and nickel. Various parameters affecting the extraction recovery of analytes such as pH, sample volume, sample loading rate, nature, volume, concentration, and flow rate of eluent were investigated and optimized. Under the optimum conditions, the method showed good linearity in the concentration range of 0.25-50.0 and 4.0-125.0 μg L(-1) with the coefficient of determination (r (2)) of 0.9991 and 0.9990 for copper and nickel, respectively. The method was very sensitive with the detection limits (defined as 3Sb/m) of 0.05 and 0.60 μg L(-1) for Cu and Ni, respectively. It was successfully applied for the determination of Cu and Ni in water and biological samples. The accuracy of the method was evaluated through the recovery experiments and independent analysis by electrothermal atomic absorption spectrometry.

  9. Core-shell polydopamine magnetic nanoparticles as sorbent in micro-dispersive solid-phase extraction for the determination of estrogenic compounds in water samples prior to high-performance liquid chromatography-mass spectrometry analysis.

    Science.gov (United States)

    Socas-Rodríguez, Bárbara; Hernández-Borges, Javier; Salazar, Pedro; Martín, Miriam; Rodríguez-Delgado, Miguel Ángel

    2015-06-05

    In this work, core-shell Fe3O4@poly(dopamine) magnetic nanoparticles (m-NPs) were prepared and characterized in our laboratory and applied as sorbents for the magnetic-micro solid phase extraction (m-μSPE) of twelve estrogenic compounds of interest (i.e. 17α-estradiol, 17β-estradiol, estrone, hexestrol, 17α-ethynylestradiol, diethylstibestrol, dienestrol, zearalenone, α-zearalanol, β-zearalanol, α-zearalenol and β-zearalenol) from different water samples. Separation, determination and quantification were achieved by high-performance liquid chromatography coupled to ion trap mass spectrometry with electrospray ionization. NPs@poly(dopamine) were synthesized by a chemical coprecipitation procedure and characterized by different surface characterization techniques (X-ray diffraction, X-ray photoelectron spectroscopy, thermogravimetric analysis, transmission and scanning electron microscopy, infrared and Raman spectroscopy, vibrating sample magnetometry, microelectrophoresis and adsorption/desorption isotherms). Parameters affecting the extraction efficiency of m-μSPE (i.e. polymerization time, pH of the sample, extraction and elution conditions) were studied and optimized. The methodology was validated for Milli-Q, mineral, tap and wastewater using 2-methoxyestradiol as internal standard, obtaining recoveries ranging from 70 to 119% with relative standard deviation values lower than 20% and limits of quantification in the range 0.02-1.1 μg/L. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. On-line solid phase extraction using the Prospekt-2 coupled with a liquid chromatography/tandem mass spectrometer for the determination of dextromethorphan, dextrorphan and guaifenesin in human plasma.

    Science.gov (United States)

    Kuhlenbeck, Debbie L; Eichold, Thomas H; Hoke, Steven H; Baker, Timothy R; Mensen, Robert; Wehmeyer, Kenneth R

    2005-01-01

    An on-line liquid chromatography/tandem mass spectrometry (LC-MS/MS) procedure, using the Prospekt- 2 system, was developed and used for the determination of the levels of the active ingredients of cough/cold medications in human plasma matrix. The experimental configuration allows direct plasma injection by performing on- line solid phase extraction (SPE) on small cartridge columns prior to elution of the analyte(s) onto the analytical column and subsequent MS/MS detection. The quantitative analysis of three analytes with differing polarities, dextromethorphan (DEX), dextrorphan (DET) and guaifenesin (GG) in human plasma presented a significant challenge. Using stable-isotope-labeled internal standards for each analyte, the Prospekt-2 on-line methodology was evaluated for sensitivity, suppression, accuracy, precision, linearity, analyst time, analysis time, cost, carryover and ease of use. The lower limit of quantitation for the on-line SPE procedure for DEX, DET and GG was 0.05, 0.05 and 5.0 ng mL(-1), respectively, using a 0.1 mL sample volume. The linear range for DEX and DET was 0.05-50 ng mL(-1) and was 5-5,000 ng mL(-1) for GG. Accuracy and precision data for five different levels of QC samples were collected over three separate days. Accuracy ranged from 90% to 112% for all three analytes, while the precision, as measured by the %RSD, ranged from 1.5% to 16.0%

  11. ADVANCED SORBENT DEVELOPMENT PROGRAM

    Energy Technology Data Exchange (ETDEWEB)

    Unknown

    1998-06-16

    The overall objective of this program was to develop regenerable sorbents for use in the temperature range of 343 to 538 C (650 to 1000 F) to remove hydrogen sulfide (H{sub 2}S) from coal-derived fuel gases in a fluidized-bed reactor. The goal was to develop sorbents that are capable of reducing the H{sub 2}S level in the fuel gas to less than 20 ppmv in the specified temperature range and pressures in the range of 1 to 20 atmospheres, with chemical characteristics that permit cyclic regeneration over many cycles without a drastic loss of activity, as well as physical characteristics that are compatible with the fluidized bed application.

  12. Solid phase extraction-capillary electrophoresis determination of sulphonamide residues in milk samples by use of C18-carbon nanotubes as hybrid sorbent materials.

    Science.gov (United States)

    Polo-Luque, M L; Simonet, B M; Valcárcel, M

    2013-07-07

    The exceptional sorption capabilities of carbon nanotubes were used to preconcentrate trace sulphonamides from milk samples. To this end, single walled carbon nanotubes (SWNTs) and multi-walled carbon nanotubes (MWNTs) dispersed in the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate were retained on a C18 stationary phase to obtain a hybrid material in a simple manner. In this approach ionic liquids are an excellent alternative to improve the dispersion of CNTs, without chemical modification or the use of solid substances or organic solvents. MWNTs provided better results than SWNTs. Carbon nanotubes retained in the C18 sorbent matrix were found to confer aromatic character, increasing its preconcentration capacity as a result. The conventional C18 stationary phase played a two-fold role: as a support to retain carbon nanotubes in the cartridge and as a medium to prevent their aggregation. The modified MWNT/C18 and SWNT/C18 materials were used to preconcentrate residual sulphonamides (SAs) in milk samples for their determination at concentrations as low as 0.03-0.069 mg L(-1) by capillary electrophoresis. Analyte recoveries from spiked samples ranged from 103.2 to 98.8% and precision, as RSD, from 8.2 to 5.4%.

  13. Application of a hybrid ordered mesoporous silica as sorbent for solid-phase multi-residue extraction of veterinary drugs in meat by ultra-high-performance liquid chromatography coupled to ion-trap tandem mass spectrometry.

    Science.gov (United States)

    Casado, Natalia; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel

    2016-08-12

    A quick, sensitive and selective analytical reversed-phase multi-residue method using ultra-high performance liquid chromatography coupled to an ion-trap mass spectrometry detector (UHPLC-IT-MS/MS) operating in both positive and negative ion mode was developed for the simultaneous determination of 23 veterinary drug residues (β-blockers, β-agonists and Non-Steroidal Anti-inflammatory Drugs (NSAIDs)) in meat samples. The sample treatment involved a liquid-solid extraction followed by a solid-phase extraction (SPE) procedure. SBA-15 type mesoporous silica was synthetized and modified with octadecylsilane, and the resulting hybrid material (denoted as SBA-15-C18) was applied and evaluated as SPE sorbent in the purification of samples. The materials were comprehensively characterized, and they showed a high surface area, high pore volume and a homogeneous distribution of the pores. Chromatographic conditions and extraction procedure were optimized, and the method was validated according to the Commission Decision 2002/657/EC. The method detection limits (MDLs) and the method quantification limits (MQLs) were determined for all the analytes in meat samples and found to range between 0.01-18.75μg/kg and 0.02-62.50μg/kg, respectively. Recoveries for 15 of the target analytes ranged from 71 to 98%. In addition, for comparative purpose SBA-15-C18 was evaluated towards commercial C18 amorphous silica. Results revealed that SBA-15-C18 was clearly more successful in the multi-residue extraction of the 23 mentioned analytes with higher recovery values. The method was successfully tested to analyze prepacked preparations of mince bovine meat. Traces of propranolol, ketoprofen and diclofenac were detected in some samples.

  14. Recovery evaluation of organophosphorus pesticides from bee pollen by matrix solid-phase dispersion extraction using sorbents based on silica and titania

    Science.gov (United States)

    Torres-Perea, C.; Muñoz-Rodríguez, D.; Medina-Peralta, S.; Carrera-Figueiras, C.; Moguel-Ordóñez, Y. B.

    2013-06-01

    This work focused on the evaluation of the recovery of organophosphorus pesticides from bee pollen after matrix solid phase-dispersion extraction (MSPD). Materials based on silica, titania and titania modified with polivylnylimidazole or polyestirene were used as adsorbents for the extraction of pesticides. Small amounts of fortified pollen (0.1 g, at 1 micro-g/g of pesticides), adsorbent (0.4 g) and solvent elution (1 mL de acetonitrile - ACN) were used in the extractions. For recovery evaluation, pollen extracts were analyzed by gas chromatography coupled with mass spectrometry.

  15. Simultaneous speciation of inorganic arsenic and antimony in water samples by hydride generation-double channel atomic fluorescence spectrometry with on-line solid-phase extraction using single-walled carbon nanotubes micro-column

    Energy Technology Data Exchange (ETDEWEB)

    Wu Hong, E-mail: wuhong1968@hotmail.com; Wang Xuecui; Liu Bing; Liu Yueling; Li Shanshan; Lu Jusheng; Tian Jiuying; Zhao Wenfeng; Yang Zonghui

    2011-01-15

    A new method was developed for the simultaneous speciation of inorganic arsenic and antimony in water by on-line solid-phase extraction coupled with hydride generation-double channel atomic fluorescence spectrometry (HG-DC-AFS). The speciation scheme involved the on-line formation and retention of the ammonium pyrrolidine dithiocarbamate complexes of As(III) and Sb(III) on a single-walled carbon nanotubes packed micro-column, followed by on-line elution and simultaneous detection of As(III) and Sb(III) by HG-DC-AFS; the total As and total Sb were determined by the same protocol after As(V) and Sb(V) were reduced by thiourea, with As(V) and Sb(V) concentrations obtained by subtraction. Various experimental parameters affecting the on-line solid-phase extraction and determination of the analytes species have been investigated in detail. With 180 s preconcentration time, the enrichment factors were found to be 25.4 for As(III) and 24.6 for Sb(III), with the limits of detection (LODs) of 3.8 ng L{sup -1} for As(III) and 2.1 ng L{sup -1} for Sb(III). The precisions (RSD) for five replicate measurements of 0.5 {mu}g L{sup -1} of As(III) and 0.2 {mu}g L{sup -1} of Sb(III) were 4.2 and 4.8%, respectively. The developed method was validated by the analysis of standard reference materials (NIST SRM 1640a), and was applied to the speciation of inorganic As and Sb in natural water samples.

  16. Evaluation of a new carbon/zirconia-based sorbent for cleanup of food extracts in multiclass analysis of pesticides and environmental contaminants

    Science.gov (United States)

    A novel carbon/zirconia based material, SupelTM QuE Verde (Verde), was evaluated in a filter-vial dispersive solid phase extraction (d-SPE) cleanup of QuEChERS extracts of pork, salmon, kale, and avocado for residual analysis of pesticides and environmental contaminants. Low pressure (LP) GC-MS/MS w...

  17. Graphene-encapsulated silica as matrix solid-phase dispersion extraction sorbents for the analysis of poly-methoxylated flavonoids in the leaves of Murraya panaculata (L.) Jack.

    Science.gov (United States)

    Sun, Ting; Li, Xuwen; Yang, Jie; Li, Lanjie; Jin, Yongri; Shi, Xiaolei

    2015-06-01

    In this study, graphene-encapsulated silica was synthesized by a hydrothermal reduction strategy. The presence of silica in graphene was identified by Fourier-transform infrared spectrometry, X-ray diffraction and scanning electron microscopy. The graphene-encapsulated silica subsequently was used as adsorbent for matrix solid-phase dispersion extraction of poly-methoxylated flavonoids from the dried leaves of Murraya panaculata (L.) Jack. Compared with the other adsorbents (graphene, silica gel, C18 silica, neutral alumina, diatomaceous earth) and without any adsorbents, better results were obtained. Then a method for analysis of poly-methoxylated flavonoids was established by coupling matrix solid-phase dispersion extraction with ultra high performance liquid chromatography and UV detection. Compared with reflux extraction and ultrasonic extraction, the proposed method is quicker, more efficient and more environmental protection. Less than 10 min is needed from extraction to detection.

  18. Sorbents for mercury removal from flue gas

    Energy Technology Data Exchange (ETDEWEB)

    Granite, Evan J.; Hargis, Richard A.; Pennline, Henry W.

    1998-01-01

    A review of the various promoters and sorbents examined for the removal of mercury from flue gas is presented. Commercial sorbent processes are described along with the chemistry of the various sorbent-mercury interactions. Novel sorbents for removing mercury from flue gas are suggested. Since activated carbons are expensive, alternate sorbents and/or improved activated carbons are needed. Because of their lower cost, sorbent development work can focus on base metal oxides and halides. Additionally, the long-term sequestration of the mercury on the sorbent needs to be addressed. Contacting methods between the flue gas and the sorbent also merit investigation.

  19. Preparation of Fe3O4@PPy magnetic nanoparticles as solid-phase extraction sorbents for preconcentration and separation of phthalic acid esters in water by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Zhao, Hongyan; Huang, Manyan; Wu, Jianrong; Wang, Li; He, Hua

    2016-02-01

    The purpose of this paper is to introduce a solid-phase extraction method of separating and determining of phthalic acid esters (PAEs) by PPy-coated Fe3O4 magnetic nanoparticles (Fe3O4@PPy MNPs). In the process, nanoparticles were served as sorbents and the optimal conditions of the extraction have been explored. The composite was synthesized through the chemical oxidation method, combining pyrrole monomer with Fe3O4 magnetic ball in the form of aggregation state and the coated nanoparticles possessed core-shell construction. The PPy-coated Fe3O4 magnetic microspheres have been extensively characterized by transmission electron microscopy, Fourier transform infrared spectroscopy and vibrating sample magnetometry. The optimum conditions were investigated by orthogonal experimental design, which was used to testing the influence of main factors and the interactions among them. The orthoplan is famous for the merit that it can study the whole experiments comprehensively through minimal tests. Under the optimal extraction conditions: 20mg of modified magnetite nanoparticles, eluting with acetic ester of 2mL, 40min of MSPE, eluting in 1h and 20mL of sample volume, good linearity (r(2)>0.9912) of all calibration curves was obtained in validation experiments. And the limits of detection (LODs) were from 0.006 to 0.021ng/mL. The recoveries in different sample matrices were in the range from 80.4% to 108.2% with relative standard deviations less than 12.8%. The present work demonstrates the applicability of the developed method for the determination of PAEs in water sample and the results justified that it can be applied successfully to the selective isolation and enrichment of PAEs in real water samples.

  20. Novos sorventes baseados em poli (metiloctilsiloxano sobre sílica para uso em extração em fase sólida New sorbents based on poly(methyloctylsiloxane immobilized on silica for use in solid-phase extraction

    Directory of Open Access Journals (Sweden)

    Sonia C. N. Queiroz

    2006-07-01

    Full Text Available This paper presents an easy and practical procedure to obtain silica-based C-8 type sorbents for use in solid-phase extraction. The materials are prepared by depositing poly(methyloctylsiloxane, PMOS, on the silica support. Two different treatments for immobilization were used: thermal treatment or gamma irradiation. Suitable recoveries were obtained after pre-concentration of dilute solutions, at the ng/L level, of a mixture of pesticides, indicating the good performance of the materials.

  1. Novos sorventes baseados em poli (metiloctilsiloxano) sobre sílica para uso em extração em fase sólida New sorbents based on poly(methyloctylsiloxane) immobilized on silica for use in solid-phase extraction

    OpenAIRE

    Queiroz, Sonia C. N.; Melo,Lúcio F. C.; Isabel C. S. F. Jardim

    2006-01-01

    This paper presents an easy and practical procedure to obtain silica-based C-8 type sorbents for use in solid-phase extraction. The materials are prepared by depositing poly(methyloctylsiloxane), PMOS, on the silica support. Two different treatments for immobilization were used: thermal treatment or gamma irradiation. Suitable recoveries were obtained after pre-concentration of dilute solutions, at the ng/L level, of a mixture of pesticides, indicating the good performance of the materials.

  2. On-line solid phase extraction-gas chromatography-cryotrapping-infrared spectrometry for the trace-level determination of microcontaminants in aqueous samples

    NARCIS (Netherlands)

    Hankemeier, T; Hooijschuur, E.; Vreuls, R.J.J.; Brinkman, U.A.Th.; Visser, T.

    1998-01-01

    A large-volume on-column GC-cryotrapping-IR system was developed for injections of up to 100 μl of organic extracts. Considerable reduction of the solvent-and-water background and enhanced analyte detectability was achieved by using an open-split interface between the GC column and the IR detector a

  3. On-line coupling of solid-phase extraction with mass spectrometry for the analysis of biological samples III. Determination of prednisolone in serum

    NARCIS (Netherlands)

    van Hout, M.W.J.; Hofland, C.M; Niederlander, H.A G; Bruins, A.P.; de Zeeuw, R.A.; de Jong, G.J.

    2003-01-01

    Solid-phase extraction (SPE) was directly coupled to mass spectrometry (MS) to assess the feasibility of the system for the rapid determination of prednisolone in serum. A C-18 stationary phase allowed washing of the cartridge with 25% methanol. Elution was performed by switching the methanol

  4. On-line solid phase extraction-gas chromatography-cryotrapping-infrared spectrometry for the trace-level determination of microcontaminants in aqueous samples

    NARCIS (Netherlands)

    Hankemeier, T; Hooijschuur, E.; Vreuls, R.J.J.; Brinkman, U.A.Th.; Visser, T.

    1998-01-01

    A large-volume on-column GC-cryotrapping-IR system was developed for injections of up to 100 μl of organic extracts. Considerable reduction of the solvent-and-water background and enhanced analyte detectability was achieved by using an open-split interface between the GC column and the IR detector

  5. On-line coupling of solid-phase extraction with mass spectrometry for the analysis of biological samples III. Determination of prednisolone in serum

    NARCIS (Netherlands)

    van Hout, MWJ; Hofland, CM; Niederlander, HAG; Bruins, AP; de Zeeuw, RA; de Jong, GJ

    2003-01-01

    Solid-phase extraction (SPE) was directly coupled to mass spectrometry (MS) to assess the feasibility of the system for the rapid determination of prednisolone in serum. A C-18 stationary phase allowed washing of the cartridge with 25% methanol. Elution was performed by switching the methanol percen

  6. Synthesis and characterisation of nano structure lead (II) ion-imprinted polymer as a new sorbent for selective extraction and preconcentration of ultra trace amounts of lead ions from vegetables, rice, and fish samples.

    Science.gov (United States)

    Behbahani, Mohammad; Bagheri, Akbar; Taghizadeh, Mohsen; Salarian, Mani; Sadeghi, Omid; Adlnasab, Laleh; Jalali, Kobra

    2013-06-01

    This paper describes the preparation of new Pb(II)-imprinted polymeric particles using 2-vinylpyridine as a functional monomer, ethylene glycol dimethacrylate as the cross-linker, 2,2'- azobisisobutyronitrile as the initiator, diphenylcarbazone as the ligand, acetonitril as the solvent, and Pb(NO(3))(2) as the template ion, through bulk polymerisation technique. The imprinted lead ions were removed from the polymeric matrix using 5 mL of HCl (2 mol.L(-1)) as the eluting solvent. The lead ion concentration was determined by flame atomic absorption spectrometry. Optimum pH for maximum sorption was obtained at 6.0. Sorption and desorption of Pb(II) ions on the IIP particles were quite fast and achieved fully over 5 min. In the proposed method, the maximum sorbent capacity of the ion-imprinted polymer was calculated to be 75.4 mg g(-1). The preconcentration factor, relative standard deviation, and limit of detection of the method were found to be 245, 2.1%, and 0.42 ng mL(-1), respectively. The prepared ion-imprinted polymer particles have an increased selectivity toward Pb(II) ions over a range of competing metal ions with the same charge and similar ionic radius. This ion-imprinted polymer is an efficient solid phase for extraction and preconcentration of lead ions in complex matrixes. For proving that the proposed method is reliable, a wide range of food samples with different and complex matrixes was used.

  7. Multi-walled carbon nanotubes as solid-phase extraction sorbents for simultaneous determination of type A trichothecenes in maize, wheat and rice by ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Dong, Maofeng; Si, Wenshuai; Jiang, Keqiu; Nie, Dongxia; Wu, Yongjiang; Zhao, Zhihui; De Saeger, Sarah; Han, Zheng

    2015-12-01

    A solid-phase extraction (SPE) procedure using multi-walled carbon nanotubes (MWCNTs) as sorbents coupled with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed for simultaneous determination of four type A trichothecenes in maize, wheat and rice for the first time. Several key parameters including the composition of sample loading solutions, washing and elution solvents were thoroughly investigated to achieve optimal SPE recoveries and efficiency. Performance of the MWCNTs materials was significantly affected by pH, and after optimization, n-hexane and 5% methanol aqueous solution as the washing solutions and methanol containing 1% formic acid as the elution solvent presented an excellent purification efficiency for the four targets in the different matrices. The method was validated by determining the linearity (R(2)≥0.992), recovery (73.4-113.7%), precision (1.2-17.1%) and sensitivity (limit of quantification in the range of 0.02-0.10μg/kg), and was further applied for simultaneous determination of type A trichothecenes in 30 samples. Although low contamination levels of type A trichothecenes in wheat, maize and rice were observed revealing mitigated risks to consumers in Shanghai, China, the developed method has proven to be a valuable tool for type A trichothecenes monitoring in complex crop matrices.

  8. On-line dynamic extraction and automated determination of readily bioavailable hexavalent chromium in solid substrates using micro-sequential injection bead-injection lab-on-valve hyphenated with electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald

    2006-01-01

    A novel and miniaturized micro-sequential injection bead injection lab-on-valve (μSI-BI-LOV) fractionation system was developed for in-line microcolumn soil extraction under simulated environmental scenarios and accurate monitoring of the content of easily mobilisable hexavalent chromium in soil...... environments at the sub-low parts-per-million level. The flow system integrates dynamic leaching of hexavalent chromium using deionized water as recommended by the German Standard DIN 38414-S4 method; on-line pH adjustment of the extract by a 0.01 mol L-1 Tris-HNO3 buffer solution; isolation of the chromate......). The effect of simulated acidic rain on the accessibility of chromate forms for plant uptake was also investigated. The proposed approach offers several advantages over conventional speciation/fractionation protocols in the batch mode, including immediate separation with concomitant preconcentration...

  9. On-line restricted access molecularly imprinted solid phase extraction of ivermectin in meat samples followed by HPLC-UV analysis.

    Science.gov (United States)

    de Lima, Marcela Marília; Vieira, André Coutinho; Martins, Isarita; Boralli, Vanessa Bergamin; Borges, Keyller Bastos; Figueiredo, Eduardo Costa

    2016-04-15

    A new restricted access molecularly imprinted polymer coated with bovine serum albumin (RAMIP-BSA) was synthesized, characterized and used for direct analysis of ivermectin from bovine meat samples, in a two-dimensional liquid chromatography system with UV detection. Ivermectin, 4-vynilpiridine and ethylene glycol dimethacrylate were employed as template, functional monomer and cross-linker, respectively. A BSA layer was cross-linked around the polymer, resulting in a biocompatible chemical barrier able to eliminate about 100% of protein from the samples. Ivermectin was extracted from the minced meat samples through a solvent extraction using methanol:water (70:30, v:v), and the extracts were directly injected into the two-dimensional liquid chromatography system, without any other treatment. Samples, fortified with ivermectin from 50 to 500 μg kg(-1), were used to build the analytical calibration curve (r=0.996). The limit of quantification was 50 μg kg(-1). Precision and accuracy presented variation coefficients, as well as relative errors lower than 17.0% and within -18.5% and 22.0%, respectively.

  10. Study on solid phase extraction and graphite furnace atomic absorption spectrometry for the determination of nickel, silver, cobalt, copper, cadmium and lead with MCI GEL CHP 20Y as sorbent.

    Science.gov (United States)

    Yang, Guangyu; Fen, Weibo; Lei, Chun; Xiao, Weilie; Sun, Handong

    2009-02-15

    A solid phase extraction and graphite furnace atomic absorption spectrometry (GFAAS) for the determination of nickel, silver, cobalt, copper, cadmium and lead with MCI GEL CHP 20Y as sorbent was studied. Trace amounts of chromium, nickel, silver, cobalt, copper, cadmium and lead were reacted with 2-(2-quinolinil-azo)-4-methyl-1,3-dihydroxidobenzene (QAMDHB) followed by adsorption onto MCI GEL CHP 20Y solid phase extraction column, and 1.0molL(-1) HNO(3) was used as eluent. The metal ions in 300mL solution can be concentrated to 1.0mL, representing an enrichment factor of 300 was achieved. The recoveries of analytes at pH 8.0 with 1.0g of resin were greater than 95% without interference from alkaline, earth alkaline and some metal ions. When detected with graphite furnace atomic absorption spectrometry, the detection limits in the original samples were 1.4ngL(-1) for Cr(III), 1.0ngL(-1) for Ni(II), 0.85ngL(-1) for Ag(I), 1.2ngL(-1) for Co(II), 1.0ngL(-1) for Cu(II), 1.2ngL(-1) for Cd(II) and 1.3ngL(-1) for Pb(II). The validation of the procedure was performed by the analysis of the certified standard reference materials, and the presented procedure was applied to the determination of analytes in biological, water and soil samples with good results (recoveries range from 89 to 104%, and R.S.D.% lower than 3.2%. The results agreed with the standard value or reference method).

  11. Synthesis of new hybrid sorbent by grafting 2,6-diacetyl pyridine onto microporous β-zeolite and its application in solid phase extraction of heavy metals from environmental samples

    Indian Academy of Sciences (India)

    HARINATH YAPATI; SREENU BHOGINENI; SURESH CHIRUMAMILLA; K SESHAIAH

    2016-05-01

    The aim of this study was synthesis of a new hybrid material and its application in solid phaseextraction of metal ions from environmental samples. The hybrid material was synthesized by grafting3-aminopropyl trimethoxy silane onto Β-zeolite and functionalizing with 2,6-diacetyl pyridine in a stepwise covalentprocess. This hybrid material was characterized by FT-IR and XRD studies. The hybrid material was usedas sorbent in solid phase extraction of Pb(II), Ni(II), Cu(II) and Cd(II). The method is based on the collectionof metal ions onto 2,6-DAP-PA-Β-zeolite and the sorbed metal ions were eluted with 10mL of 1M $HNO_{3}.The influences of analytical parameters such as pH of the sample solution, volume of sample, type and volumeof eluent, flow rate of the sample and eluent that govern the efficiency and throughput of the method wereevaluated. The influence effects of matrix ions (common ions other than the analyte that are present in the sample)on the retentions of the metal ions were also examined. The maximum adsorption capacity values for themetal ions onto 2,6-DAP-PA-Β-zeolite, as calculated from the Langmuir model, were 112.7, 94.2, 105, and102.8mg $g^{-1}$ respectively. The relative standard deviation under optimum conditions was lower than 3.10%.The limits of detection were 0.035 for Pb(II), 0.076 for Ni(II), 0.083 for Cu(II) and 0.059 mg $L^{-1}$ for Cd(II),respectively. The accuracy of the method was estimated by analyzing reference standard materials. The resultsindicate that the method is efficient for the solid phase extraction of trace levels of Pb(II), Ni(II), Cu(II) andCd(II) from environmental samples.

  12. Iron oxide functionalized graphene oxide as an efficient sorbent for dispersive micro-solid phase extraction of sulfadiazine followed by spectrophotometric and mode-mismatched thermal lens spectrometric determination.

    Science.gov (United States)

    Kazemi, Elahe; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad; Abbasi, Amir; Rashidian Vaziri, Mohammad Reza; Behjat, Abbas

    2016-01-15

    A simple and rapid dispersive micro-solid phase extraction (DMSPE) combined with mode-mismatched thermal lens spectrometry as well as fiber optic linear array spectrophotometry was developed for the separation, extraction and determination of sulfadiazine. Graphene oxide was synthesized using the modified Hummers method and functionalized with iron oxide nanoparticles by means of a simple one step chemical coprecipitation method. The synthesized iron oxide functionalized graphene oxide was utilized as an efficient sorbent in DMSPE of sulfadiazine. The retained analyte was eluted by using 180µL of a 6:4 mixture of methanol/acetic acid solution and was spectrophotometrically determined based on the formation of an azo dye through coupling with thenoyltrifluoroacetone. Under the optimized conditions, with the application of spectrophotometry technique and with a sample volume of 100mL, the method exhibited a linear dynamic range of 3-80µg L(-1) with a detection limit of 0.82µg L(-1), an enrichment factor of 200 as well as the relative standard deviations of 2.6% and 4.3% (n=6) at 150µg L(-1) level of sulfadiazine for intra- and inter-day analyses, respectively. Whereas, through the application of the thermal lens spectrometry and a sample volume of 10mL, the method exhibited a linear dynamic range of 1-800µg L(-1) with a detection limit of 0.34µg L(-1) and the relative standard deviations of 3.1% and 5.4% (n=6) at 150µg L(-1) level of sulfadiazine for intra- and inter-day analyses, respectively. The method was successfully applied to the determination of sulfadiazine in milk, honey and water samples.

  13. Trace and ultratrace determination of heavy metal ions by energy-dispersive X-ray fluorescence spectrometry using graphene as solid sorbent in dispersive micro solid-phase extraction

    Energy Technology Data Exchange (ETDEWEB)

    Kocot, Karina; Sitko, Rafal, E-mail: rafal.sitko@us.edu.pl

    2014-04-01

    In this paper, the adsorptive properties of graphene nanosheets were used for simultaneous preconcentration of cobalt, nickel, copper and lead ions from water samples. The developed methodology is based on dispersive micro-solid phase extraction (DMSPE) which is miniaturized and a simplified version of classical solid phase extraction technique. In proposed procedure only 200 μL of suspension containing graphene (0.2 mg), ammonium pyrrolidine dithiocarbamate (APDC) (0.8 mg) and Triton-X-100 (0.1 mg) is rapidly injected to 50 mL of water sample. Then, graphene nanosheets with adsorbed metal-APDC chelates are collected on membrane filter and measured using energy-dispersive X-ray fluorescence (EDXRF) spectrometry. The various parameters including pH, amount of APDC, sample volume, amount of Triton-X-100 and sorption time were optimized in order to obtain the best recoveries. The experiment shows that Co, Ni, Cu and Pb can be simultaneously preconcentrated at pH of 5 with high recoveries (97%, 96%, 99% and 96% for Co, Ni, Cu and Pb, respectively) and very good precision (RSDs within 2.6–3.4%). Due to the excellent enrichment factors ranging from 400 to 2500 the proposed DMSPE–EDXRF procedure offers low detection limits. For optimized measurement conditions (voltage and current of X-ray tube, primary beam filter) the detection limits are even 0.08, 0.07, 0.08 and 0.20 ng mL{sup −1} for Co, Ni, Cu and Pb, respectively. - Highlights: • Excellent detection limits using EDXRF • A new preconcentration procedure combining DMSPE and EDXRF measurement • Graphene as a promising and efficient solid sorbent in DMSPE • Simple, fast, inexpensive and environmental friendly method.

  14. An assessment of the liquid-gas partitioning behavior of major wastewater odorants using two comparative experimental approaches: liquid sample-based vaporization vs. impinger-based dynamic headspace extraction into sorbent tubes.

    Science.gov (United States)

    Iqbal, Mohammad Asif; Kim, Ki-Hyun; Szulejko, Jan E; Cho, Jinwoo

    2014-01-01

    The gas-liquid partitioning behavior of major odorants (acetic acid, propionic acid, isobutyric acid, n-butyric acid, i-valeric acid, n-valeric acid, hexanoic acid, phenol, p-cresol, indole, skatole, and toluene (as a reference)) commonly found in microbially digested wastewaters was investigated by two experimental approaches. Firstly, a simple vaporization method was applied to measure the target odorants dissolved in liquid samples with the aid of sorbent tube/thermal desorption/gas chromatography/mass spectrometry. As an alternative method, an impinger-based dynamic headspace sampling method was also explored to measure the partitioning of target odorants between the gas and liquid phases with the same detection system. The relative extraction efficiency (in percent) of the odorants by dynamic headspace sampling was estimated against the calibration results derived by the vaporization method. Finally, the concentrations of the major odorants in real digested wastewater samples were also analyzed using both analytical approaches. Through a parallel application of the two experimental methods, we intended to develop an experimental approach to be able to assess the liquid-to-gas phase partitioning behavior of major odorants in a complex wastewater system. The relative sensitivity of the two methods expressed in terms of response factor ratios (RFvap/RFimp) of liquid standard calibration between vaporization and impinger-based calibrations varied widely from 981 (skatole) to 6,022 (acetic acid). Comparison of this relative sensitivity thus highlights the rather low extraction efficiency of the highly soluble and more acidic odorants from wastewater samples in dynamic headspace sampling.

  15. Molecularly imprinted polymer cartridges coupled on-line with high performance liquid chromatography for simple and rapid analysis of human insulin in plasma and pharmaceutical formulations.

    Science.gov (United States)

    Moein, Mohammad Mahdi; Javanbakht, Mehran; Akbari-adergani, Behrouz

    2014-04-01

    In this paper, a novel method is described for automated determination of human insulin in biological fluids using principle of sequential injection on a molecularly imprinted solid-phase extraction (MISPE) cartridge as a sample clean-up technique combined with high performance liquid chromatography (HPLC). The water-compatible molecularly imprinted polymers (MIPs) were prepared using methacrylic acid as a functional monomer, ethylene glycol dimethacrylate as a cross-linker, chloroform as a porogen and insulin as a template molecule. The imprinted polymers were then employed as the solid-phase extraction sorbent for on-line extraction of insulin from human plasma samples. To achieve the best condition, influential parameters on the extraction efficiency were thoroughly investigated. Rapid and simple analysis of the hormone was successfully accomplished through the good selectivity of the prepared sorbent coupled with HPLC. Limits of detection (LOD) and quantification (LOQ) of 0.2 ng mL(-1), 0.7 ng mL(-1), and 0.03 ng mL(-1), 0.1 ng mL(-1) were obtained in plasma and urine respectively. The obtained data exhibited the great recoveries for extraction of insulin from human plasma and pharmaceutical samples, higher than 87%.

  16. Study of the factors affecting the performance of microextraction by packed sorbent (MEPS) using liquid scintillation counter and liquid chromatography-tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Altun, Zeki [Karlstad University, Faculty of Technology and Science, SE-651 88 Karlstad (Sweden); Abdel-Rehim, Mohamed [Karlstad University, Faculty of Technology and Science, SE-651 88 Karlstad (Sweden); Clinical Pharmacology and DMPK, AstraZeneca R and D Soedertaelje, SE-151 85 Soedertaelje (Sweden)], E-mail: Mohamed.Abdel-Rehim@Astrazeneca.com

    2008-12-23

    Microextraction by packed sorbent (MEPS) is a new technique for sample preparation that can be connected on-line with LC or GC. In MEPS, approximately 1-2 mg of the solid packing material is inserted into a syringe (100-250 {mu}L) as a plug. Sample preparation takes place on the packed bed. The bed can be packed or coated to provide selective and suitable sampling conditions. The new method is very promising for extraction of drugs and metabolites from biological samples. In this paper, some factors affecting the performance of MEPS such as recovery, carry-over, leakage, washing volume and elution volume were studied using C18 and hydroxylated polystyrene-divinylbenzene copolymer (ENV+) as sorbents. Radioactively labelled bupivacaine in plasma samples was used as test analyte. For the extraction of this drug, using methanol/water 95:5 (v/v) (0.25% ammonium hydroxide) was used as elution solvent. The analyte response increased with increasing the elution volume and it was linear upp up to 100 {mu}L utilizing liquid scintillation counter. Further, for concentrating the sample, we found that MEPS may be used such that the sample can be drawn through the needle, up and down, several times. The analyte leakage increases as the volume washing increases, though higher washing volumes may also result in cleaner extracts. To eliminate analyte carry-over, the sorbents were washed first with 3 x 250 {mu}L elution solution and then with 3 x 250 {mu}L washing solution. In addition, the reproducibility measurements show relatively good relative standard deviation (RSD) % values concerning analyte recovery and analyte leakage. The present study provides an understanding of basic aspects when optimizing methods for MEPS. In this study, MEPS was used off-line with liquid scintillation counter and on-line with LC-MS/MS.

  17. Inflammatory Response to Sorbent Hemodialysis.

    Science.gov (United States)

    Rosales, Laura; Thijssen, Stephan; Kruse, Anja; Sipahioglu, Murat Hairy; Hirachan, Padam; Raimann, Jochen G; Kuntsevich, Viktoriya; Carter, Mary; Levin, Nathan W; Kotanko, Peter

    2015-01-01

    Inflammation is common and associated with morbidity and mortality in hemodialysis (HD) patients. Exposure to endotoxin contained in the dialysate may trigger inflammation. Dialysate volume is substantially reduced in sorbent HD compared with standard single-pass dialysis. In this prospective study (Clinicaltrials.gov, number: NCT00788905), we compared the inflammatory response to single-pass and sorbent HD. Patients receiving single-pass HD were studied during 1 week of sorbent HD (Allient system; Renal Solutions, Warrendale, PA) and 1 week of single-pass HD. Patients were dialyzed using high-flux polysulfone dialyzers. Midweek pre- and post-HD serum levels of high-sensitivity C-reactive protein, interleukin (IL)-1β, IL-6, IL-10, interferon gamma, tumor necrosis factor alpha (TNF-α), and eotaxin were determined and their intradialytic change corrected for hemoconcentration during single-pass HD and sorbent HD compared by paired t-test. We enrolled 18 patients, nine completed the study. Although TNF-α decreased during both single-pass and sorbent HD (p < 0.001), none of the other biomarkers changed significantly during HD. We observed no difference between single-pass and sorbent HD. For the markers investigated in this study, there was no difference in the acute intradialytic inflammatory response to single-pass or sorbent HD.

  18. Study on Edge Extraction Methods for Image-based Icing On-line Monitoring on Overhead Transmission Lines%输电线路覆冰图像边缘提取方法研究

    Institute of Scientific and Technical Information of China (English)

    王小朋; 胡建林; 吴彬

    2008-01-01

    A new method of measuring the icing thickness of transmission lines on-line is proposed in this paper. In this method, the pictures of transmission lines which are photoed by the camera on the iron tower are processed immediately to extract the edges of the transmission line conductor and transmission line insulators. The icing thickness can be gained by comparing the edges of the iced transmission line and the uniced one. Two icing image edge extraction methods are described in detail, that is, a method based on the combination of the wavelet transform and the floating threshold method and a method based on the combination of the optimal threshold method and the mathematical morphology transform. The icing images from the artificial climatic chamber and transmission lines are used to test the methods above. The results show that the method based on the wavelet transform and the floating threshold method does well in the extraction of relatively smooth edges, such as glaze icing on conductor and icing on the insulator;meanwhile, the method based on the optimal threshold method and the mathematical morphology transform does well in the edge extraction of icing on the conductor, especially the opaque rime icing on the conductor with complicated edges.

  19. Solid-Sorbent Air Sampler

    Science.gov (United States)

    Galen, T. J.

    1986-01-01

    Portable unit takes eight 24-hour samples. Volatile organic compounds in air collected for analysis by portable, self-contained sampling apparatus. Sampled air drawn through sorbent material, commercial porous polymer of 2, 3-diphenyl-p-phenylene oxide. High-boiling-point organic compounds adsorbed onto polymer, while low-boiling-point organics pass through and returned to atmosphere. Sampler includes eight sample tubes filled with polymeric sorbent. Organic compounds in atmosphere absorbed when air pumped through sorbent. Designed for checking air in spacecraft, sampler adaptable to other applications as leak detection, gas-mixture analysis, and ambient-air monitoring.

  20. Evaluation of the effect of TM208 on the activity of five cytochrome P450 enzymes using on-line solid-phase extraction HPLC-DAD: a cocktail approach.

    Science.gov (United States)

    Lin, Wensi; Zhang, Jianmei; Ling, Xiaomei; Yu, Ning; Li, Jing; Yang, Haisong; Li, Runtao; Cui, Jingrong

    2013-04-01

    A rapid, simple, and sensitive on-line solid-phase extraction HPLC-DAD method for simultaneous evaluation of the activity of five CYP450 isoforms (CYP1A2, CYP2C19, CYP2D6, CYP2E1 and CYP3A4) in vivo has been developed and validated. The five specific probe substrates include caffeine (1A2), metoprolol (2D6), dapsone (3A4), omeprazole (2C19) and chlorzoxazone (2E1). Automated pre-purification of plasma and enrichment of analytes were performed using a C18 on-line solid-phase extraction cartridge. After being eluted from the cartridge, the analytes and the internal standard antipyrine were separated on a C18 RP analytical column and analyzed by DAD. The method was validated to quantify the concentration ranges of 0.05-50.0 μg/ml for dapsone and omeprazole, 0.1-50.0 μg/ml for caffeine and 0.2-50.0 μg/ml for metoprolol and chlorzoxazone. The linearity (R(2)) for all analytes tested was exceeded 0.99. The intra-day precision ranged from 0.29 to 13% and the inter-day precision ranged from 5.0 to 15%, respectively. The intra-day and inter-day accuracy were between 86.7% and 113.6%. The extraction recoveries were in the range 82.8-109.9% for all the analytes and internal standard antipyrine. This method was successfully applied to evaluate the effects of TM208 on rat five CYP450 isoforms.

  1. Simultaneous determination of caffeine, theophylline and theobromine in human plasma by on-line solid-phase extraction coupled to reversed-phase chromatography.

    Science.gov (United States)

    Emara, Samy

    2004-10-01

    A reversed-phase liquid chromatographic column switching system was described for the determination of caffeine (CF), theophylline (TH) and theobromine (TB) in human plasma with a direct injection procedure. A short protein-coated mu Bondapak CN silica pre-column (20 x 3 mm, i.d.) was used for enrichment of the drugs and clean up from weakly retained plasma components using phosphate buffer saline pH 7.4. After washing step, the retained drugs were flushed into a reversed-phase column (5 microm TSK gel ODS-80 TM, 150 x 4.6 mm i.d.) with a mobile phase of methanol-0.01 M phosphate buffer, pH 3.5 (30:70, v/v) for the final separation. The eluent was monitored with a UV detector at 275 nm. The resulting chromatograms showed no interference from endogenous plasma components. A linear relationship between the concentration of drug and peak height was confirmed in the range of 0.5-20 microg/mL for all drugs. High extraction recoveries from plasma ranging from 96.12 to 100.32% were achieved. Validation of the method was examined performing intra- and inter-day accuracy and precision and was found to be satisfactory. The coefficients of variation of the three drugs were less than 3% for intra-day and less than 4% for inter-day run assays.

  2. Determination of bezafibrate, methotrexate, cyclophosphamide, orlistat and enalapril in waste and surface waters using on-line solid-phase extraction liquid chromatography coupled to polarity-switching electrospray tandem mass spectrometry.

    Science.gov (United States)

    Garcia-Ac, Araceli; Segura, Pedro A; Gagnon, Christian; Sauvé, Sébastien

    2009-04-01

    We developed a rapid method for the monitoring of five selected pharmaceuticals in the influent and effluent of municipal wastewater treatment plants (WWTP) as well as in the effluent-receiving waters. To that end, we optimized and validated an analytical method based on on-line solid-phase extraction (on-line SPE) coupled with reversed-phase liquid chromatography-switching polarity electrospray ionization-tandem mass spectrometry (LC-ESI(+/-)-MS/MS). The target analytes have a variable hydrophobic character and belong to various therapeutic classes including the lipid regulator bezafibrate, the chemotherapy drugs methotrexate and cyclophosphamide, the lipase inhibitor orlistat and the angiotensin converting enzyme (ACE) inhibitor used in the treatment of hypertension, enalapril. The method combines positive and negative voltage switching modes, therefore all analytes can be determined using a single injection and without any reduction in sensitivity. In order to detect traces of these compounds, a preconcentration step before detection is performed by loading 1.00 mL of sample in an on-line SPE cartridge and eluting from the cartridge using a reversed-phase liquid chromatography gradient. Analysis of wastewater and surface water samples was greatly affected by co-eluting matrix compounds, to compensate for matrix effects quantitation was therefore performed using standard additions. Method intra-day precision was less than 6.5% and limits of detection in fortified matrix effluent samples ranged from 9 to 20 ng L(-1). Four of the target pharmaceuticals were detected in the WWTP effluents, enalapril and bezafibrate being the most abundant compounds with concentrations of 35 and 239 ng L(-1), respectively. Concentrations of these same compounds in surface water samples from sites downstream in the St. Lawrence River were 8 and 63 ng L(-1), respectively, which was mainly due to dilution.

  3. CFB sorbent selection enhances performance

    Energy Technology Data Exchange (ETDEWEB)

    Buecker, B.; Wofford, J.; DuBose, R.; Ray, D.

    1997-07-01

    The quality and particle size of the sorbent has a direct influence on the efficiency of sulfur dioxide (SO{sub 2}) removal in a circulating fluidized bed (CFB) boiler. This report outlines tests and subsequent operation of a CFB unit at the University of North Carolina at Chapel Hill Cogeneration Facility (UNC-CH) that proved how dramatically a change in sorbent can change the efficiency of performance.

  4. High capacity immobilized amine sorbents

    Science.gov (United States)

    Gray, McMahan L.; Champagne, Kenneth J.; Soong, Yee; Filburn, Thomas

    2007-10-30

    A method is provided for making low-cost CO.sub.2 sorbents that can be used in large-scale gas-solid processes. The improved method entails treating an amine to increase the number of secondary amine groups and impregnating the amine in a porous solid support. The method increases the CO.sub.2 capture capacity and decreases the cost of utilizing an amine-enriched solid sorbent in CO.sub.2 capture systems.

  5. Direct modification of hydrogen/deuterium-terminated diamond particles with polymers to form reversed and strong cation exchange solid phase extraction sorbents.

    Science.gov (United States)

    Yang, Li; Jensen, David S; Vail, Michael A; Dadson, Andrew; Linford, Matthew R

    2010-12-03

    We describe direct polymer attachment to hydrogen and deuterium-terminated diamond (HTD and DTD) surfaces using a radical initiator (di-tert-amyl peroxide, DTAP), a reactive monomer (styrene) and a crosslinking agent (divinylbenzene, DVB) to create polystyrene encapsulated diamond. Chemisorbed polystyrene is sulfonated with sulfuric acid in acetic acid. Surface changes were followed by X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and diffuse reflectance Fourier transform infrared spectroscopy (DRIFT). Finally, both polystyrene-modified DTD and sulfonated styrene-modified DTD were used in solid phase extraction (SPE). Percent recovery and column capacity were investigated for both phenyl (polystyrene) and sulfonic acid treated polystyrene SPE columns. These diamond-based SPE supports are stable under basic conditions, which is not the case for silica-based SPE supports.

  6. Highly selective dummy molecularly imprinted polymer as a solid-phase extraction sorbent for five bisphenols in tap and river water.

    Science.gov (United States)

    Sun, Xiaoli; Wang, Jincheng; Li, Yun; Jin, Jing; Zhang, Baoqin; Shah, Syed Mazhar; Wang, Xueli; Chen, Jiping

    2014-05-23

    A simple and fast method for both dummy template selection and polymer composition optimization is proposed here. A series of dummy templates for bisphenols imprinting were screened by running them on a non-imprinted polymer (NIP) column with porogen solvent as mobile phase. The tested dummy templates mainly involved bisphenol S (BPS), bromobisphenol A (TBBPA), bisphenol F (BPF), bisphenol E (BPE), bisphenol B (BPB), bisphenol AF (BPAF), 2,2',6,6'-tetramethyl-4,4'-sulfonyldiphenol (BS-TM) and 4,4'-diaminodiphenylmethane (DADPM). Different monomers and porogens were also investigated for BPS and DADPM using the same method. BPS dummy template was finally selected with acetonitrile and 4-VP as porogen and monomer. The resulting dummy molecularly imprinted polymer (DMIP) achieved superior affinities for BPF, BPE, BPA, BPB and BPAF with imprinting factors 14.5, 13.8, 8.7, 5.7 and 4.2, respectively. An efficient method based on BPS-DMIP-SPE coupled with HPLC-UV was developed for selective extraction of BPF, BPE, BPA, BPB and BPAF in water samples. The method showed excellent recoveries (89.4-102.0%) and precision (RSD 0.3-4.8%, n=5) for tap and river water samples spiked at three concentration levels each (40, 200 and 1000ngL(-1)). The detection limits ranged between 2.2 and 3.8ngL(-1) with a sample volume of 500mL. The result demonstrated the superiority of the optimized method for selective extraction of BPs in water samples at the ngL(-1) level.

  7. Deep Bed Iodine Sorbent Testing FY 2011 Report

    Energy Technology Data Exchange (ETDEWEB)

    Nick Soelberg; Tony Watson

    2011-08-01

    Nuclear fission results in the production of fission products (FPs) and activation products that increasingly interfere with the fission process as their concentrations increase. Some of these fission and activation products tend to evolve in gaseous species during used nuclear fuel reprocessing. Analyses have shown that I129, due to its radioactivity, high potential mobility in the environment, and high longevity (half life of 15.7 million years), can require control efficiencies of up to 1,000x or higher to meet regulatory emission limits. Deep-bed iodine sorption testing has been done to evaluate the performance of solid sorbents for capturing iodine in off-gas streams from nuclear fuel reprocessing plants. The objectives of the FY 2011 deep bed iodine sorbent testing are: (1) Evaluate sorbents for iodine capture under various conditions of gas compositions and operating temperature (determine sorption efficiencies, capacities, and mass transfer zone depths); and (2) Generate data for dynamic iodine sorption modeling. Three tests performed this fiscal year on silver zeolite light phase (AgZ-LP) sorbent are reported here. Additional tests are still in progress and can be reported in a revision of this report or a future report. Testing was somewhat delayed and limited this year due to initial activities to address some questions of prior testing, and due to a period of maintenance for the on-line GC. Each test consisted of (a) flowing a synthetic blend of gases designed to be similar to an aqueous dissolver off-gas stream over the sorbent contained in three separate bed segments in series, (b) measuring each bed inlet and outlet gas concentrations of iodine and methyl iodide (the two surrogates of iodine gas species considered most representative of iodine species expected in dissolver off-gas), (c) operating for a long enough time to achieve breakthrough of the iodine species from at least one (preferably the first two) bed segments, and (d) post-test purging

  8. Nanostructured Metal Oxide Sorbents for the Collection and Recovery of Uranium from Seawater

    Energy Technology Data Exchange (ETDEWEB)

    Chouyyok, Wilaiwan; Warner, Cynthia L.; Mackie, Katherine E.; Warner, Marvin G.; Gill, Gary A.; Addleman, Raymond S.

    2016-02-07

    The ability to collect uranium from seawater offers the potential for a long-term green fuel supply for nuclear energy. However, extraction of uranium, and other trace minerals, is challenging due to the high ionic strength and low mineral concentrations in seawater. Herein we evaluate the use of nanostructured metal oxide sorbents for the collection and recovery of uranium from seawater. Chemical affinity, chemical adsorption capacity and kinetics of preferred sorbent materials were evaluated. High surface area manganese and iron oxide nanomaterials showed excellent performance for uranium collection from seawater. Inexpensive nontoxic carbonate solutions were demonstrated to be an effective and environmental benign method of stripping the uranium from the metal oxide sorbents. Various formats for the utilization of the nanostructured metals oxide sorbent materials are discussed including traditional and nontraditional methods such as magnetic separation. Keywords: Uranium, nano, manganese, iron, sorbent, seawater, magnetic, separations, nuclear energy

  9. Development and characterization of cation exchange sorbent of St - DVB copolymer support for solid-phase extraction%St-DVB基质阳离子交换固相萃取填料的研制及应用

    Institute of Scientific and Technical Information of China (English)

    申书昌; 李媛媛; 柏叶春

    2011-01-01

    以玉米淀粉为分散剂,偶氮二异丁腈 (AIBN)为引发剂,二乙烯基苯(DVB)为交联剂,在在氮气保护下,用悬浮聚合法制备了交联苯乙烯-二乙烯苯(St-DVB )高分子微球,用浓硫酸进行磺化,制成了以St-DVB为基质的阳离子交换固相萃取填料.考察了搅拌速度对交联聚苯乙烯微球粒径大小及分布的影响.分别用TEM,SEM/EDS和傅里叶红外光谱法对填料进行了形貌及结构分析,测定了磺化物的磺化度.自制阳离子交换固相萃取小柱,对水中的莠去津进行了应用试验,考察了性能.%In this paper, used eom-starch as dispersing agent, 2,2-azobisisobutyronitrile as initiator of polymerization, divinyl benzene as cross-linking agent,polystyrene-divinyl benzene microspheres were prepared by suspension polymerization under nitrogen.The polystyrene-divinyl benzene microspheres were sulfonated by concentrated sulfuric acid, the polystyrene-divinyl benzene sulphonic acid material as a cation exchange sorbent for solid phase extraction packing. stirring speed were investigated to cress-linked polystyrene partiele size and distribution. The form , structure and composition of the polystyrene-divinyl benzene and the polystyrene -divinyl benzene sulphonie acid mierospheres were characterized by means of transmission electron mieraseope , scanning electron microscope/energy dispersive X-ray spectrometer and fourier transform infrared spectroscopy measurement respectively the sulfonate sulfonation degree was Determinated by acid-soda titration method. The cation exchange solid phase extraction column made using the self-made and a plastic syringe. The atrazine in water was detected by solid phase extraetion-HPLC

  10. Novel sorbents for environmental remediation

    Science.gov (United States)

    Manariotis, Ioannis D.; Karapanagioti, Hrissi K.; Werner, David

    2014-05-01

    Nowadays, one of the major environmental problems is the pollution of aquatic systems and soil by persistent pollutants. Persistent pollutants have been found widespread in sediments, surface waters, and drinking water supplies. The removal of pollutants can be accomplished prior to their discharge to receiving bodies or by immobilizing them onto soil. Sorption is the most commonly applied process, and activated carbons have been widely used. Rapid progress in nanotechnology and a new focus on biomass-based instead of non-renewable starting materials have produced a wide range of novel engineered sorbents including biosorbents, biochars, carbon-based nanoparticles, bio-nano hybrid materials, and iron-impregnated activated carbons. Sorbent materials have been used in environmental remediation processes and especially in agricultural soil, sediments and contaminated soil, water treatment, and industrial wastewater treatment. Furthermore, sorbents may enhance the synergistic action of other processes, such as volatilization and biodegradation. Novel sorbents have been employed for the removal or immobilization of persistent pollutants such as and include heavy metals (As, Cr, Cu, Pb, Cd, and Hg), halogenated organic compounds, endocrine disrupting chemicals, metalloids and non-metallic elements, and other organic pollutants. The development and evaluation of novel sorbents requires a multidisciplinary approach encompassing environmental, nanotechnology, physical, analytical, and surface chemistry. The necessary evaluations encompass not only the efficiency of these materials to remove pollutants from surface waters and groundwater, industrial wastewater, polluted soils and sediments, etc., but also the potential side-effects of their environmental applications. The aim of this work is to present the results of the use of biochar and impregnated carbon sorbents for the removal of organic pollutants and metals. Furthermore, the new findings from the forthcoming session

  11. On-line solid-phase extraction coupled to ultra-performance liquid chromatography with tandem mass spectrometry detection for the determination of benzotriazole UV stabilizers in coastal marine and wastewater samples

    Energy Technology Data Exchange (ETDEWEB)

    Montesdeoca-Esponda, Sarah; Sosa-Ferrera, Zoraida; Santana-Rodriguez, Jose Juan [Universidad de Las Palmas de Gran Canaria, Departamento de Quimica, Las Palmas de Gran Canaria (Spain)

    2012-05-15

    Benzotriazoles are a group of UV absorbing compounds considered emerging contaminants that are used in different personal care products, and therefore, it is of high interest to develop sensitive and fast methods for investigating their presence in the environment. In this work, we present the development and application of a novel method based on on-line solid-phase extraction coupled to ultra-performance liquid chromatography with tandem mass spectrometry detection (SPE-UPLC-MS/MS) for the determination of seven benzotriazole UV stabilizers (BUVSs) in coastal marine and wastewater samples. This process is compared with a conventional off-line SPE procedure followed by UPLC-MS/MS. The parameters affecting the performance of the sample preparation and determination processes were evaluated. The results indicate that the on-line procedure provides for better sensitivity and reproducibility and is faster and easier than the off-line procedure. The detection limits and quantification limits achieved were in the range of 0.6-4.1 ng circle L{sup -1} and 2.1-14 ng circle L{sup -1} and relative standard deviation between 6.2 and 10 %. The developed method was applied to coastal marine and wastewater samples from Gran Canaria Island (Spain). All of the BUVSs studied were detected in the samples from wastewater treatment plants and two were found in the seawater samples (UV P in the range of 2.8-4.4 ng circle L{sup -1} and UV 360 between 3.6 and 5.2 ng circle L{sup -1}). (orig.)

  12. Sol-gel derived sorbents

    Science.gov (United States)

    Sigman, Michael E.; Dindal, Amy B.

    2003-11-11

    Described is a method for producing copolymerized sol-gel derived sorbent particles for the production of copolymerized sol-gel derived sorbent material. The method for producing copolymerized sol-gel derived sorbent particles comprises adding a basic solution to an aqueous metal alkoxide mixture for a pH.ltoreq.8 to hydrolyze the metal alkoxides. Then, allowing the mixture to react at room temperature for a precalculated period of time for the mixture to undergo an increased in viscosity to obtain a desired pore size and surface area. The copolymerized mixture is then added to an immiscible, nonpolar solvent that has been heated to a sufficient temperature wherein the copolymerized mixture forms a solid upon the addition. The solid is recovered from the mixture, and is ready for use in an active sampling trap or activated for use in a passive sampling trap.

  13. 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.

  14. A single-step pesticide extraction and clean-up multi-residue analytical method by selective pressurized liquid extraction followed by on-line solid phase extraction and ultra-high-performance liquid chromatography-tandem mass spectrometry for complex matrices.

    Science.gov (United States)

    Rodrigues, Elsa Teresa; Pardal, Miguel Ângelo; Salgueiro-González, Noelia; Muniategui-Lorenzo, Soledad; Alpendurada, Maria Fátima

    2016-06-24

    Pesticides, a group of compounds linked to human activity, may, when in toxic levels, have a profound effect on water quality, and hence result in adverse consequences to aquatic life and ultimately to human health. Analytical challenges arise when successfully trying to determine these levels in environmental complex matrices. Therefore, fast, simple, sensitive and selective analytical methodologies for multi-residue determination of pesticides (atrazine, azoxystrobin, bentazon, λ-cyhalothrin, penoxsulam and terbuthylazine) in sediment, macrophytes (algae and aquatic plants) and aquatic animals were developed and validated. The established methods were matrix-dependent and were based on Selective Pressurized Liquid Extraction (SPLE) followed by on-line Solid Phase Extraction and Ultra Performance Liquid Chromatography-tandem Mass Spectrometry (on-line SPE-UPLC-ESI-MS/MS). This cutting-edge research methodology uses a small amount of sample, is time saving and reduces the use of organic solvents in compliance with Green Chemistry principles. The analytical features were adequate for all compounds in all studied matrices. The established methodology was applied on real marine samples and no pesticide concentrations above their respective method quantification limits were measured in sediments or aquatic plants. However, terbuthylazine was found in the macroalgae Ulva spp. (108ngg(-1)dw) and all the prospected pesticides were measured above their respective method quantification limits in the bivalve Scrobicularia plana (atrazine: 48ngg(-1)dw, azoxystrobin: 64ngg(-1)dw, bentazon: 33ngg(-1)dw, λ-cyhalothrin: 2531ngg(-1)dw, penoxsulam: 50ngg(-1)dw, and terbuthylazine: 44ngg(-1)dw).

  15. 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

  16. High Temperature Sorbents for Oxygen

    Science.gov (United States)

    Sharma, Pramod K. (Inventor)

    1996-01-01

    A sorbent capable of removing trace amounts of oxygen (ppt) from a gas stream at a high temperature above 200 C is introduced. The sorbent comprises a porous alumina silicate support such as zeolite containing from 1 to 10 percent by weight of ion exchanged transition metal such as copper or cobalt ions and 0.05 to 1.0 percent by weight of an activator selected from a platinum group metal such as platinum. The activation temperature, oxygen sorption and reducibility are all improved by the presence of the platinum activator.

  17. Metal-organic framework templated synthesis of porous inorganic materials as novel sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Taylor-Pashow, Kathryn M. L.; Lin, Wenbin; Abney, Carter W.

    2017-03-21

    A novel metal-organic framework (MOF) templated process for the synthesis of highly porous inorganic sorbents for removing radionuclides, actinides, and heavy metals is disclosed. The highly porous nature of the MOFs leads to highly porous inorganic sorbents (such as oxides, phosphates, sulfides, etc) with accessible surface binding sites that are suitable for removing radionuclides from high level nuclear wastes, extracting uranium from acid mine drainage and seawater, and sequestering heavy metals from waste streams. In some cases, MOFs can be directly used for removing these metal ions as MOFs are converted to highly porous inorganic sorbents in situ.

  18. Metal-organic framework templated synthesis of porous inorganic materials as novel sorbents

    Science.gov (United States)

    Taylor-Pashow, Kathryn M. L.; Lin, Wenbin; Abney, Carter W.

    2017-03-21

    A novel metal-organic framework (MOF) templated process for the synthesis of highly porous inorganic sorbents for removing radionuclides, actinides, and heavy metals is disclosed. The highly porous nature of the MOFs leads to highly porous inorganic sorbents (such as oxides, phosphates, sulfides, etc) with accessible surface binding sites that are suitable for removing radionuclides from high level nuclear wastes, extracting uranium from acid mine drainage and seawater, and sequestering heavy metals from waste streams. In some cases, MOFs can be directly used for removing these metal ions as MOFs are converted to highly porous inorganic sorbents in situ.

  19. Development of an automated sequential injection on-line solvent extraction-back extraction procedure as demonstrated for the determination of cadmium with detection by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2002-01-01

    ) of the SI-system. Afterwards, it is dispensed and mixed with an aqueous back extractant of dilute nitric acid containing Hg(II) ions as stripping agent, thereby facilitating a rapid metal-exchange reaction with the APDC ligand and transfer of the Cd into the aqueous phase. The aqueous phase is separated...

  20. Membrane Extraction and Flow Injection for On-Line Sample Preparation%膜萃取和流动注射在线样品前处理技术

    Institute of Scientific and Technical Information of China (English)

    刘景富; 江桂斌

    2003-01-01

    The objective of this dissertation is to develop on-line sample preparation procedures based on membrane extraction and flow injection (FI) techniques. A novel sample pretreatment technique, which we termed continuous flow liquid membrane extraction(CFLME), was developed for trace-enrichment of polar organic pollutants. The principle and parameters of CFLME were investigated by using sulfonylurea herbicides and bisphenol A as model compounds. At the optimum conditions and with an enrichment time of 120 min and 40 min, metsulfuron methyl and bisphenol A were enriched with an enrichment factor of 1000 and 200, respectively, and the enrichment efficiencies of bisphenol A and the five studied sulfonylurea herbicides were 3.5 ~ 200 fold of that of supported liquid membrane extraction (SLM). Then,an on-line coupled CFLME-HPLC system, with detection limits of 0.05 ~ 0.1 μg/L after 10min of enrichment, was developed for the determination of sulfonylurea herbicides. Futhermore, an on-line coupled CFLME-C18 precolumn-HPLC system was developed for the trace analysis of sulfonylurea herbicides in surface waters at ng/L level. The detection limit of this proposed CFLME-C18 precolumn-HPLC system is 200 fold lower than that of the original C18SPE preconcentration-HPLC detection method. Experiments show that the proposed CFLME technique has the advantages of high selectivity, high enrichment efficiency, low-cost, longterm stability and convenience for coupling on-line with other analytical instruments.On-line sample pretreatment procedures based on FI technique were also studied and approaches for the application of FI technique in routine analysis were proposed. A FI-micropore membrane liquid-liquid system was developed for the routine analysis of anionic surfactants in detergents, and a FI high temperature reaction system was developed for the determination of total inorganic phosphates in detergents and the total reducing sugars in tobacco. To simplify the manifold

  1. Sulphur dioxide removal using activated sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Warmuzinski, K.; Jaschik, M.; Jaschik, J.; Wasilewski, W.; Mrozowski, J. [Inst. Inzynierii Chemical PAN, Gliwice (Poland)

    2001-07-01

    Results are presented of experimental investigation of the dry flue gas desulphurisation (FGD) process at low temperatures using activated sorbents. Solid wastes (ashes) from the dry (with humidification) FGD plant are used as a sorbent. The influence of basic operating parameters on the efficiency of SO{sub 2} removal is determined. More than twofold sulphur dioxide removal efficiency is obtained using activated sorbents in comparison with the efficiency obtained in the process with dry sorbents. The possibility of reduction of sorbent consumption in the dry method of FGD with humidification is found.

  2. Study of application of hydrophobic fibrous sorbents for water purification from metal ions

    OpenAIRE

    Е. V. Petrova; Astashkina, А. P.; Filonenko, D. А.; Otmakhov, V. I.; Izaak, Т. I.; Volokitin, G. G.

    2007-01-01

    Sorption properties of hydrophobic fibrous sorbents on the basis of polypropylene and polyethylene terephthalate produced from thermoplastic polymer wastes to metal ion series in aqueous media has been studied. Based on the experimental data of extraction degree dependencies on fibre laying density, dispersity, presence of air in sorbent, volume of pass solution the mechanism of metal ion sorption from aqueous media with hydrophobic fibrous materials is suggested.

  3. Preliminary results on the determination of ultratrace amounts of cadmium in tea samples using a flow injection on-line solid phase extraction separation and preconcentration technique to couple with a sequential injection hydride generation atomic fluorescence spectrometry.

    Science.gov (United States)

    Duan, Taicheng; Song, Xuejie; Jin, Dan; Li, Hongfei; Xu, Jingwei; Chen, Hangting

    2005-10-31

    In this work, a method was developed for determination of ultra-trace levels of Cd in tea samples by atomic fluorescence spectrometry (AFS). A flow injection solid phase extraction (FI-SPE) separation and preconcentration technique, to on-line couple with a sequential injection hydride generation (SI-HG) technique is employed in this study. Cd was preconcentrated on the SPE column, which was made from a neutral extractant named Cyanex 923, while other matrix ions or interfering ions were completely or mostly separated off. Conditions for the SPE separation and preconcentration, as well as conditions for the HG technique, were studied. Due to the separation of interfering elements, Cd hydride generation efficiency could be greatly enhanced with the sole presence of Co(2+) with a concentration of 200mugL(-1), which is much lower than those in other works previously reported. Interferences on both the Cd separation and preconcentration, and Cd hydride generation (HG) were investigated; it showed that both the separation and preconcentration system, and the HG system had a strong anti-interference ability. The SPE column could be repeatedly used at least 400 times, a R.S.D. of 0.97% was obtained for 6 measurements of Cd with 0.2mugL(-1) and a correlation coefficiency of 1.0000 was obtained for the measurement of a series of solutions with Cd concentrations from 0.1 to 2mugL(-1). The method has a low detection limit of 10.8ngL(-1) for a 25mL solution and was successfully validated by using two tea standard reference materials (GBW08513 and GBW07605).

  4. Simple and quick determination of analgesics and other contaminants of emerging concern in environmental waters by on-line solid phase extraction coupled to liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Ferrer-Aguirre, Alejandra; Romero-González, Roberto; Vidal, J L Martínez; Frenich, Antonia Garrido

    2016-05-13

    A simple and quick analytical method has been developed for the determination of pharmaceutical compounds in water. An on-line solid-phase extraction (SPE) coupled to liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been optimized to determine 7 contaminants of emerging concern in environmental waters at ngL(-1) levels. This procedure requires minimal sample handling and small sample volume (900μL) with a total running time of 18min. Several SPE parameters were evaluated and optimized in order to achieve a high sample throughput. Therefore sample volume, carryover and reusability of the cartridges were evaluated. Performance characteristics were evaluated and good linearity was obtained (R(2)>0.98). Recoveries were evaluated in spiked samples at three concentrations and the values ranged from 71 to 104%. Intra and inter-day precision was lower than 10 and 13% respectively. Limits of quantification were equal to or lower than 10ngL(-1), except for 1,7-dimethylxanthine (20ngL(-1)) and ibuprofen (50ngL(-1)). The method was applied to 20 environmental water samples, and ibuprofen was the compound most widely detected at concentrations up to 42.06μgL(-1), whereas the other compounds were detected in fewer samples at lower concentrations (up to 15.99μgL(-1)).

  5. Surface Functionalized Nanostructured Ceramic Sorbents for the Effective Collection and Recovery of Uranium from Seawater

    Energy Technology Data Exchange (ETDEWEB)

    Chouyyok, Wilaiwan; Pittman, Jonathan W.; Warner, Marvin G.; Nell, Kara M.; Clubb, Donald C.; Gill, Gary A.; Addleman, Raymond S.

    2016-05-02

    The ability to collect uranium from seawater offers the potential for a nearly limitless fuel supply for nuclear energy. We evaluated the use of functionalized nanostructured sorbents for the collection and recovery of uranium from seawater. Extraction of trace minerals from seawater and brines is challenging due to the high ionic strength of seawater, low mineral concentrations, and fouling of surfaces over time. We demonstrate that rationally assembled sorbent materials that integrate high affinity surface chemistry and high surface area nanostructures into an application relevant micro/macro structure enables collection performance that far exceeds typical sorbent materials. High surface area nanostructured silica with surface chemistries composed of phosphonic acid, phosphonates, 3,4 hydroxypyridinone, and EDTA showed superior performance for uranium collection. A few phosphorous-based commercial resins, specifically Diphonix and Ln Resin, also performed well. We demonstrate an effective and environmentally benign method of stripping the uranium from the high affinity sorbents using inexpensive nontoxic carbonate solutions. The cyclic use of preferred sorbents and acidic reconditioning of materials was shown to improve performance. Composite thin films composed of the nanostructured sorbents and a porous polymer binder are shown to have excellent kinetics and good capacity while providing an effective processing configuration for trace mineral recovery from solutions. Initial work using the composite thin films shows significant improvements in processing capacity over the previously reported sorbent materials.

  6. Preparation of an epitope-imprinted polymer with antibody-like selectivity for beta2-microglobulin and application in serum sample analysis with a facile method of on-line solid-phase extraction coupling with high performance liquid chromatography.

    Science.gov (United States)

    Yang, Fangfang; Deng, Dandan; Dong, Xiangchao; Lin, Shen

    2017-03-09

    Molecularly imprinted polymers (MIPs) for protein recognition have great application potential in the biological analysis. However, preparation of protein imprinted polymer is still facing challenge. Beta2-microglobulin (β2m) is a protein biomarker that can be used in diagnosis of different diseases. In this research, a novel MIP with ability of β2m recognition has been developed by epitope and surface-confined imprinting approaches. A peptide with sequence of MIQRTPKIQ was selected as template. A strategy of combination of hierarchical imprinting and template immobilization was employed in the β2m-MIP synthesis. Imprinted binding sites with open-entrance have been created that have good accessibility for β2m and facilitated fast reversible binding kinetics. The experimental results demonstrated that the MIP has good selectivity. It can differentiate the template from peptide with different sequence and distinguish the β2m from other proteins with similar size and pI values. After binding property study of the β2m-MIP, a method of β2m determination in serum was established in which β2m was on-line extracted by MIP and analyzed by HPLC process. The recoveries for spiked serum was ≥83% with RSD <1.1%, indicating that the method has good accuracy and precisions. The LOD and LOQ were 0.058 and 0.195mgL(-1) respectively, which meet the requirements of the β2m analysis. The successful application of the β2m-MIP demonstrated that β2m has reversible binding on the MIP with a kinetics that can meet the requirements of the HPLC analysis. It also indicated that the β2m-MIP has good mechanical strength and reusability that can be applied reliably in the practical analysis. As a synthetic antibody, β2m-MIP is advantageous compared to the biological molecules.

  7. On-line solid-phase extraction coupled with high-performance liquid chromatography and tandem mass spectrometry (SPE-HPLC-MS-MS) for quantification of bromazepam in human plasma: an automated method for bioequivalence studies.

    Science.gov (United States)

    Gonçalves, José Carlos Saraiva; Monteiro, Tânia Maria; Neves, Claúdia Silvana de Miranda; Gram, Karla Regina da Silva; Volpato, Nádia Maria; Silva, Vivian A; Caminha, Ricardo; Gonçalves, Maria do Rocio Bencke; Santos, Fábio Monteiro Dos; Silveira, Gabriel Estolano da; Noël, François

    2005-10-01

    A validated method for on-line solid-phase extraction coupled with high-performance liquid chromatography tandem mass spectrometry (SPE-HPLC-MS-MS) is described for the quantification of bromazepam in human plasma. The method involves a dilution of 300 muL of plasma with 100 muL of carbamazepine (2.5 ng/mL), used as internal standard, vortex-mixing, centrifugation, and injection of 100 muL of the supernate. The analytes were ionized using positive electrospray mass spectrometry then detected by multiple reaction monitoring (MRM). The m/z transitions 316-->182 (bromazepam) and 237-->194 (carbamazepine) were used for quantification. The calibration curve was linear from 1 ng/mL (limit of quantification) to 200 ng/mL. The retention times of bromazepam and carbamazepine were 2.6 and 3.2 minutes, respectively. The intraday and interday precisions were 3.43%-15.45% and 5.2%-17%, respectively. The intraday and interday accuracy was 94.00%-103.94%. This new automated method has been successfully applied in a bioequivalence study of 2 tablet formulations of 6 mg bromazepam: Lexotan(R) from Produtos Roche Químicos e Farmacêuticos SA, Rio de Janeiro, Brazil (reference) and test formulation from Laboratórios Biosintética Ltda, São Paulo, Brazil. Because the 90% CI of geometric mean ratios between reference and test were completely included in the 80%-125% interval, the 2 formulations were considered bioequivalent. The comparison of different experimental conditions for establishing a dissolution profile in vitro along with our bioavailability data further allowed us to propose rationally based experimental conditions for a dissolution test of bromazepam tablets, actually lacking a pharmacopeial monograph.

  8. High capacity carbon dioxide sorbent

    Energy Technology Data Exchange (ETDEWEB)

    Dietz, Steven Dean; Alptekin, Gokhan; Jayaraman, Ambalavanan

    2015-09-01

    The present invention provides a sorbent for the removal of carbon dioxide from gas streams, comprising: a CO.sub.2 capacity of at least 9 weight percent when measured at 22.degree. C. and 1 atmosphere; an H.sub.2O capacity of at most 15 weight percent when measured at 25.degree. C. and 1 atmosphere; and an isosteric heat of adsorption of from 5 to 8.5 kilocalories per mole of CO.sub.2. The invention also provides a carbon sorbent in a powder, a granular or a pellet form for the removal of carbon dioxide from gas streams, comprising: a carbon content of at least 90 weight percent; a nitrogen content of at least 1 weight percent; an oxygen content of at most 3 weight percent; a BET surface area from 50 to 2600 m.sup.2/g; and a DFT micropore volume from 0.04 to 0.8 cc/g.

  9. Humic sorbent from sapropel for purification of waste waters from petroleum

    Science.gov (United States)

    Adeeva, L. N.; Platonova, D. S.

    2017-08-01

    A sorbent by thermal processing sapropel residue, after the extraction of humic acids, subsequent modification with polyhexamethyleneguanidine and pre-isolated humic acids was synthesized. The transformations of the carbon-mineral humic sorbent at a temperature of 20-1000°C in air have been studied by thermal analysis. The presence of various functional groups on the surface of a carbon-mineral humic sorbent from sapropel is confirmed with an IR-spectroscopy method. Sorption of petroleum from water solutions was studied. The static capacity value of the synthesized humic sorbent for petroleum is 85.5±0.3 mg/g. It is established that the process of sorption is described by the equation of Freundlich isotherm.

  10. On-line sample processing involving microextraction techniques as a front-end to atomic spectrometric detection for trace metal assays: A review

    Energy Technology Data Exchange (ETDEWEB)

    Miró, Manuel, E-mail: manuel.miro@uib.es [FI-TRACE Group, Department of Chemistry, Faculty of Sciences, University of the Balearic Islands, E-07122 Palma de Mallorca, Illes Balears (Spain); Hansen, Elo Harald [Granåsen 93, DK-2800 Kgs. Lyngby (Denmark)

    2013-06-11

    Graphical abstract: -- Highlights: •Role of flow injection in automation of microextraction techniques for metal assays. •On-line coupling of liquid phase microextraction (LPME) to atomic spectrometry. •Critical evaluation of on-line single drop and dispersive LPME. •On-line coupling of micro-solid phase extraction (μSPE) to atomic spectrometry. •Critical appraisal of magnetic/carbon nanoparticles and biomass for on-line μSPE. -- Abstract: Within the last decade, liquid-phase microextraction (LPME) and micro-solid phase extraction (μSPE) approaches have emerged as substitutes for conventional sample processing procedures for trace metal assays within the framework of green chemistry. This review surveys the progress of the state of the art in simplification and automation of microextraction approaches by harnessing to the various generations of flow injection (FI) as a front end to atomic absorption spectrometry (AAS), atomic fluorescence spectrometry (AFS) or inductively coupled plasma atomic emission spectrometry or mass spectrometry (ICP-AES/MS). It highlights the evolution of flow injection analysis and related techniques as vehicles for appropriate sample presentation to the detector and expedient on-line matrix separation and pre-concentration of trace levels of metals in troublesome matrices. Rather than being comprehensive this review is aimed at outlining the pros and cons via representative examples of recent attempts in automating green sample preparation procedures in an FI or sequential injection (SI) mode capitalizing on single-drop microextraction, dispersive liquid-phase microextraction and advanced sorptive materials including carbon and metal oxide nanoparticles, ion imprinted polymers, superparamagnetic nanomaterials and biological/biomass sorbents. Current challenges in the field are identified and the synergetic combination of flow analysis, nanotechnology and metal-tagged biomolecule detection is envisaged.

  11. Advanced low-temperature sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Ayala, R.E.; Venkataramani, V.S.; Abbasian, J.; Hill, A.H.

    1995-12-01

    A number of promising technologies are currently being optimized for coal-based power generation, including the Integrated-Gasification Combined Cycle (IGCC) system. If IGCC is to be used successfully for power generation, an economic and efficient way must be found to remove the contaminants, particularly sulfur species, found in coal gas. Except for the hot gas desulfurization system, all major components of IGCC are commercially available or have been shown to meet system requirements. Over the last two decades, the U.S. Department of Energy/Morgantown Energy Technology Center (DOE/METC) has sponsored development of various configurations of high-temperature desulfurization systems including fixed-bed, moving-bed, transport-bed, and fluidized-bed systems. Because of their mode of operation and requirements for sorbent manufacturing, the fixed-bed systems can generally use the same materials as moving-bed configurations, i.e., pelletized or extruded sorbents, while fluidized-bed (circulating or bubbling configurations) and transport reactor configurations use materials generally described as agglomerated or granulated.The objective of this program is to remove hydrogen sulfides from coal gas using sorbent materials.

  12. Silica supported Fe(3)O(4) magnetic nanoparticles for magnetic solid-phase extraction and magnetic in-tube solid-phase microextraction: application to organophosphorous compounds.

    Science.gov (United States)

    Moliner-Martinez, Y; Vitta, Yosmery; Prima-Garcia, Helena; González-Fuenzalida, R A; Ribera, Antonio; Campíns-Falcó, P; Coronado, Eugenio

    2014-03-01

    This work demonstrates the application of silica supported Fe3O4 nanoparticles as sorbent phase for magnetic solid-phase extraction (MSPE) and magnetic on-line in-tube solid-phase microextraction (Magnetic-IT-SPME) combined with capillary liquid chromatography-diode array detection (CapLC-DAD) to determine organophosphorous compounds (OPs) at trace level. In MSPE, magnetism is used as separation tool while in Magnetic-IT-SPME, the application of an external magnetic field gave rise to a significant improvement of the adsorption of OPs on the sorbent phase. Extraction efficiency, analysis time, reproducibility and sensitivity have been compared. This work showed that Magnetic-IT-SPME can be extended to OPs with successful results in terms of simplicity, speed, extraction efficiency and limit of detection. Finally, wastewater samples were analysed to determine OPs at nanograms per litre.

  13. On-line sample processing methods in flow analysis

    DEFF Research Database (Denmark)

    Miró, Manuel; Hansen, Elo Harald

    2008-01-01

    In this chapter, the state of the art of flow injection and related approaches thereof for automation and miniaturization of sample processing regardless of the aggregate state of the sample medium is overviewed. The potential of the various generation of flow injection for implementation of in......-line dilution, derivatization, separation and preconcentration methods encompassing solid reactors, solvent extraction, sorbent extraction, precipitation/coprecipitation, hydride/vapor generation and digestion/leaching protocols as hyphenated to a plethora of detection devices is discussed in detail...

  14. Formación on line On line learning

    Directory of Open Access Journals (Sweden)

    O. Grau-Perejoan

    2008-09-01

    Full Text Available La formación on line es una modalidad de enseñanza a distancia basada en las nuevas tecnologías. En este artículo se pretende hacer una introducción a base de describir a grandes rasgos sus características principales: asincronía, no presencialidad, comunicación escrita, función del profesor on line, así como los retos, los riesgos, las ventajas y los inconvenientes que plantea. Se exponen las diferencias entre la formación on line y la formación presencial, de manera que los docentes puedan adaptar de la mejor manera posible sus propuestas formativas a la modalidad on line. Se introduce el importantísimo papel de la planificación y de la fase de diseño y, finalmente, se repasan conceptos útiles para comprender mejor el mundo de la formación on line como son los conceptos entorno virtual de aprendizaje (EVA o Blended Learning (B-Learning.On line learning is a type of distance education based on new technologies. This article's aim is to introduce its main characteristics -asynchrony, non-presentiality, written communication, e-teacher role- as well as its challenges, risks, advantages and limitations. Differences between on line learning and face-to-face learning are presented in order to enable educational professionals to adapt their courses to the on line methodology. Planning and designing are introduced as key phases and, finally, useful concepts such as Virtual Learning Environment (VLE or Blended Learning (B-Learning are reviewed in order to achieve a better understanding of the on line learning field.

  15. Advanced Low-Temperature Fluid Bed Sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Abbasian, J.; Slimane, R.B.; Wangerow, J.R. [Institute of Gas Technology, Des Plaines, IL (United States)

    1996-12-31

    This paper discusses the results obtained in an ongoing study geared towards developing advanced mixed-metal oxide sorbents for desulfurization of coal-derived fuel gases in the temperature range of 350 to 550{degrees}C. The paper focuses on the study related to the development of durable sorbents suitable for fluidized-bed application and addresses thermodynamic considerations, sulfidation kinetics, regenerability, and the physical and chemical characteristics of a number of novel sorbents.

  16. 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

  17. The solid phase extraction of some metal ions using palladium nanoparticles attached to silica gel chemically bonded by silica-bonded N-propylmorpholine as new sorbent prior to their determination by flame atomic absorption spectroscopy.

    Science.gov (United States)

    Ghaedi, M; Rezakhani, M; Khodadoust, S; Niknam, K; Soylak, M

    2012-01-01

    In this research at first palladium nanoparticle attached to a new chemically bonded silica gel has been synthesized and has been characterized with different techniques such as X-ray diffraction (XRD), fourier transform infrared (FT-IR), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). Then, this new sorbent (chemically modified silica gel with N-propylmorpholine (PNP-SBNPM)) was efficiently used for preconcentration of some metal ions in various food samples. The influence of effective variables including mass of sorbent, flow rate, pH of sample solutions and condition of eluent such as volume, type and concentration on the recoveries of understudy metal ions were investigated. Following the optimization of variables, the interfering effects of some foreign ions on the preconcentration and determination of the investigated metal ions described. At optimum values of variables, all investigated metal ions were efficiently recovered with efficiency more than 95%, relative standard deviation (RSD) between 2.4 and 2.8, and detection limit in the range of 1.4-2.7 ng mL⁻¹. The present method is simple and rapidly applicable for the determination of the understudied metal ions (ng mL⁻¹) in different natural food samples.

  18. The Solid Phase Extraction of Some Metal Ions Using Palladium Nanoparticles Attached to Silica Gel Chemically Bonded by Silica-Bonded N-Propylmorpholine as New Sorbent prior to Their Determination by Flame Atomic Absorption Spectroscopy

    Directory of Open Access Journals (Sweden)

    M. Ghaedi

    2012-01-01

    Full Text Available In this research at first palladium nanoparticle attached to a new chemically bonded silica gel has been synthesized and has been characterized with different techniques such as X-ray diffraction (XRD, fourier transform infrared (FT-IR, transmission electron microscopy (TEM, and scanning electron microscopy (SEM. Then, this new sorbent (chemically modified silica gel with N-propylmorpholine (PNP-SBNPM was efficiently used for preconcentration of some metal ions in various food samples. The influence of effective variables including mass of sorbent, flow rate, pH of sample solutions and condition of eluent such as volume, type and concentration on the recoveries of understudy metal ions were investigated. Following the optimization of variables, the interfering effects of some foreign ions on the preconcentration and determination of the investigated metal ions described. At optimum values of variables, all investigated metal ions were efficiently recovered with efficiency more than 95%, relative standard deviation (RSD between 2.4 and 2.8, and detection limit in the range of 1.4–2.7 ng mL−1. The present method is simple and rapidly applicable for the determination of the understudied metal ions (ng mL−1 in different natural food samples.

  19. Desulfurization sorbent development activities at METC

    Energy Technology Data Exchange (ETDEWEB)

    Siriwardane, R.V.

    1995-06-01

    Development of a suitable regenerable sorbent is a major barrier issue in the hot gas cleanup program for integrated gasification combined-cycle (IGCC) systems. This has been a challenging problem during the last 20 years, since many of the sorbents developed in the program could not retain their reactivity and physical integrity during repeated cycles of sulfidation and regeneration reactions. A series of promising sorbents (METC 2-10), which were capable of sustaining their reactivity and physical integrity during repeated sulfidation/ regeneration cycles, have been developed at the Morgantown Energy Technology Center (METC). These sorbents were tested both in low-pressure (260 KPa/23 psig) and high-pressure (520 KPa/60.7 psig) fixed-bed reactors at 538{degrees}C (1000{degrees}F) with simulated coal gas. High-pressure testing was continued for 20 cycles with steam regeneration. A major research goal during the last year was to lower the cost of materials utilized during the sorbent preparation. The METC 9 sorbent was prepared by substituting low-cost materials for some of the materials in METC 6 sorbent. The sulfur capacity of the two sorbents were similar during the 20-cycle testing. METC 2 sorbent was exposed to coal gas in the Modular Gas Cleanup Rig and it was later tested in the high-pressure fixed-bed reactor. The reactivity of the METC 2 sorbent was unaffected by the exposure to the coal gas. Development of these sorbents will be continued for both fluid-bed and moving-bed applications.

  20. Novel Sorbent-Based Process for High Temperature Trace Metal Removal

    Energy Technology Data Exchange (ETDEWEB)

    Gokhan Alptekin

    2008-09-30

    intermittent operation of the PSDF gasifier (due to the difficulties in the handling of the low quality lignite), only a small fraction of the sorbent capacity was utilized (we measured a mercury capacity of 3.27 mg/kg, which is only a fraction of the 680 mg/kg Hg capacity measured for the same sorbent used at our bench-scale evaluations at TDA). Post reaction examination of the sorbent by chemical analysis also indicated some removal As and Se (we did not detect any significant amounts of Cd in the synthesis gas or over the sorbent). The tests at UNDEERC was more successful and showed clearly that the TDA sorbent can effectively remove Hg and other trace metals (As and Se) at high temperature. The on-line gas measurements carried out by TDA and UNDEERC separately showed that TDA sorbent can achieve greater than 95% Hg removal efficiency at 260 C ({approx}200g sorbent treated more than 15,000 SCF synthesis gas). Chemical analysis conducted following the tests also showed modest amounts of As and Se accumulation in the sorbent bed (the test durations were still short to show higher capacities to these contaminants). We also evaluated the stability of the sorbent and the fate of mercury (the most volatile and unstable of the trace metal compounds). The Synthetic Ground Water Leaching Procedure Test carried out by an independent environmental laboratory showed that the mercury will remain on the sorbent once the sorbent is disposed. Based on a preliminary engineering and cost analysis, TDA estimated the cost of mercury removal from coal-derived synthesis gas as $2,995/lb (this analysis assumes that this cost also includes the cost of removal of all other trace metal contaminants). The projected cost will result in a small increase (less than 1%) in the cost of energy.

  1. Sorbent Structural Impacts Due to Humidity on Carbon Dioxide Removal Sorbents for Advanced Exploration Systems

    Science.gov (United States)

    Watson, David; Knox, James C.; West, Phillip; Stanley, Christine M.; Bush, Richard

    2015-01-01

    The Life Support Systems Project (LSSP) under the Advanced Exploration Systems (AES) program builds upon the work performed under the AES Atmosphere Resource Recovery and Environmental Monitoring (ARREM) project focusing on the numerous technology development areas. The CO2 removal and associated air drying development efforts are focused on improving the current state-of-the-art system on the International Space Station (ISS) utilizing fixed beds of sorbent pellets by seeking more robust pelletized sorbents, evaluating structured sorbents, and examining alternate bed configurations to improve system efficiency and reliability. A component of the CO2 removal effort encompasses structural stability testing of existing and emerging sorbents. Testing will be performed on dry sorbents and sorbents that have been conditioned to three humidity levels. This paper describes the sorbent structural stability screening efforts in support of the LSS Project within the AES Program.

  2. Silver containing sorbents: Physicochemical and biological properties

    Directory of Open Access Journals (Sweden)

    L.N. Rachkovskaya

    2016-06-01

    Full Text Available New silver containing sorbents, based on mineral carriers, such as alumina and silica systems with a meso- and macro- porous structure, have a higher mechanical resistance and, hydrophilic and hydrophobic chemical composition of the surface. These sorbents are easy to find and relatively inexpensive, compared to their known equivalents. They are furthermore characterised by high specific surface and simple preparation, whilst the addition of silver considerably increases their antiseptic activity. The results of research of the physical, chemical and biological properties of the developed substances, as well as bio-comparability of sorbents with biological tissues, are presented in this paper. The modified material acts simultaneously as the carrier for active substances to the area of therapeutic application and as a sorbent used to remove toxic agents from such areas. This approach led us to modify the sorbent, and prolong the delivery of substances such as silver, as an effective antibacterial and antimycotic agent.

  3. Determination of paraben preservatives in seafood using matrix solid-phase dispersion and on-line acetylation gas chromatography-mass spectrometry.

    Science.gov (United States)

    Djatmika, Rosalina; Hsieh, Chih-Chung; Chen, Jhih-Ming; Ding, Wang-Hsien

    2016-11-15

    An effective method for determining four commonly detected paraben preservatives (methyl, ethyl, propyl and butyl paraben) in marketed seafood is presented. This method employs matrix solid-phase dispersion (MSPD) before identification and quantification of the paraben preservatives via on-line acetylation gas chromatography-mass spectrometry (GC-MS). Parameters affecting the extraction efficiency of MSPD were optimized through a Box-Behnken design method. Under optimal condition, 0.5-g of freeze-dried seafood was mixed with 0.5-g of anhydrous sodium sulfate, and dispersed with 1.0-g of Florisil using vortex. After that, the blend was transferred to a glass column containing 1.5-g of silica gel+C18 (w/w, 9:1), which acted as clean-up co-sorbents. Then, target analytes were eluted with 12mL of acetonitrile. The extract was then derivatized on-line in the GC injection-port through reaction with acetic anhydride, and the identity and quantity of the target analytes were determined by the GC-MS system. The limits of quantitation (LOQs) were 0.2 to 1.0ng/g (dry weight). Preliminary results showed that the total concentrations of four selected parabens ranged from 16.7 to 44.7ng/g (dry weight).

  4. Sorbents for the oxidation and removal of mercury

    Energy Technology Data Exchange (ETDEWEB)

    Olson, Edwin S.; Holmes, Michael J.; Pavlish, John Henry

    2014-09-02

    A promoted activated carbon sorbent is described that is highly effective for the removal of mercury from flue gas streams. The sorbent comprises a new modified carbon form containing reactive forms of halogen and halides. Optional components may be added to increase reactivity and mercury capacity. These may be added directly with the sorbent, or to the flue gas to enhance sorbent performance and/or mercury capture. Mercury removal efficiencies obtained exceed conventional methods. The sorbent can be regenerated and reused. Sorbent treatment and preparation methods are also described. New methods for in-flight preparation, introduction, and control of the active sorbent into the mercury contaminated gas stream are described.

  5. Sorbents for the oxidation and removal of mercury

    Science.gov (United States)

    Olson, Edwin S; Holmes, Michael J; Pavlish, John Henry

    2013-08-20

    A promoted activated carbon sorbent is described that is highly effective for the removal of mercury from flue gas streams. The sorbent comprises a new modified carbon form containing reactive forms of halogen and halides. Optional components may be added to increase reactivity and mercury capacity. These may be added directly with the sorbent, or to the flue gas to enhance sorbent performance and/or mercury capture. Mercury removal efficiencies obtained exceed conventional methods. The sorbent can be regenerated and reused. Sorbent treatment and preparation methods are also described. New methods for in-flight preparation, introduction, and control of the active sorbent into the mercury contaminated gas stream are described.

  6. Sorption of methylxanthines by different sorbents

    Science.gov (United States)

    Dmitrienko, S. G.; Andreeva, E. Yu.; Tolmacheva, V. V.; Terent'eva, E. A.

    2013-05-01

    Sorption of caffeine, theophylline, theobromine, diprophylline, and pentoxyphylline on different sorbents (supercross-linked polystyrene, surface-modified copolymer of styrene and divinylbenzene Strata-X, and carbon nanomaterials Taunit and Diasorb-100-C16T) was studied in a static mode in an effort to find new sorbents suitable for sorption isolation and concentration of methylxanthines. The peculiarities of sorption of methylxanthines were explained in relation to the solution acidity, the nature of the sorbates and their concentration, the nature of the solvent, and the structural characteristics of the sorbents.

  7. CERN Video News on line

    CERN Multimedia

    2003-01-01

    The latest CERN video news is on line. In this issue : an interview with the Director General and reports on the new home for the DELPHI barrel and the CERN firemen's spectacular training programme. There's also a vintage video news clip from 1954. See: www.cern.ch/video or Bulletin web page

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

    Science.gov (United States)

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

    2016-03-18

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

  9. 7 CFR 2902.23 - Sorbents.

    Science.gov (United States)

    2010-01-01

    ... Sorbents. (a) Definition. Materials formulated for use in the cleanup and bioremediation of oil and chemical spills, the disposal of liquid materials, or the prevention of leakage or leaching in...

  10. Adsorption and Ultrasound-Assisted Sorbent Regeneration

    Energy Technology Data Exchange (ETDEWEB)

    Yuhe Wang; Liping Ma; Ralph T. Yang

    2006-09-30

    This work was conducted for the department of Energy. In this work, we developed a class of new sorbents that were highly sulfur selective and had high sulfur capacities. The study consisted of two sections. Development of the new sorbents is described in Section 1, and Section was a fundamental study, conducted for a better understanding for desulfurization of jet fuels. More details of the results are given blow separately for the two sections.

  11. On-line coupling of solid-phase extraction with mass spectrometry for the analysis of biological samples. II. Determination of clenbuterol in urine using multiple-stage mass spectrometry in an ion-trap mass spectrometer

    NARCIS (Netherlands)

    van Hout, MWJ; Hofland, CM; Niederlander, HAG; de Jong, GJ

    2000-01-01

    Solid-phase extraction (SPE) was coupled to ion-trap mass spectrometry to determine clenbuterol in urine. For SPE a cartridge exchanger was used and, after extraction, the eluate was directly introduced into the mass spectrometer, For two types of cartridges, i.e. C-18 and polydivinylbenzene (PDVB),

  12. Clean Air OnLine

    Energy Technology Data Exchange (ETDEWEB)

    Finney, D. [Environment Canada, Gatineau, PQ (Canada). Air Pollution Prevention Directorate

    2004-04-07

    This presentation describes Clean Air OnLine, a multi-tiered website dedicated to providing Canadians with information on air quality. The website is under development to support action to reduce air emissions, demonstrate the links between air emissions and environmental impacts, and enhance the understanding of sustainable community development issues such as health, energy, and urban sprawl. Partners in the Clean Air OnLine (CAOL) initiative include Environment Canada and the Clean Air Partnership which includes the Greater Toronto Area pilot project. The audience for CAOL includes municipal decision makers, local decision makers, community leaders, and the general public. The project provides Canadians with air pollution contextual information on pollution sources, pollutants, and related issues. It also provides information on health, environmental and economic impacts and the interrelationships with climate change issues and energy use. tabs., figs.

  13. On-line moisture analysis

    CERN Document Server

    Cutmore, N G

    2002-01-01

    Measurement of the moisture content of iron ore has become a key issue for controlling moisture additions for dust suppression. In most cases moisture content is still determined by manual or automatic sampling of the ore stream, followed by conventional laboratory analysis by oven drying. Although this procedure enables the moisture content to be routinely monitored, it is too slow for control purposes. This has generated renewed interest in on-line techniques for the accurate and rapid measurement of moisture in iron ore on conveyors. Microwave transmission techniques have emerged over the past 40 years as the dominant technology for on-line measurement of moisture in bulk materials, including iron ores. Alternative technologies have their limitations. Infra-red analysers are used in a variety of process industries, but rely on the measurement of absorption by moisture in a very thin surface layer. Consequently such probes may be compromised by particle size effects and biased presentation of the bulk mater...

  14. Continuous fluidized-bed contactor with recycle of sorbent

    Science.gov (United States)

    Scott, Charles D.; Petersen, James N.; Davison, Brian H.

    1996-01-01

    A continuous fluidized-bed contactor containing sorbent particles is used to remove solutes from liquid solvents. As the sorbent particles, for example gel beads, sorb the solute, for example metal ion species, the sorbent particles tend to decrease in diameter. These smaller loaded sorbent particles rise to the top of the contactor, as larger sorbent particles remain at the bottom of the contactor as a result of normal hydraulic forces. The smaller loaded sorbent particles are then recovered, regenerated, and reintroduced into the contactor. Alternatively, the loaded sorbent particles may also slightly increase in diameter, or exhibit no change in diameter but an increase in density. As a result of normal hydraulic forces the larger loaded sorbent particles fall to the bottom of the contactor. The larger loaded sorbent particles are then recovered, regenerated, and reintroduced into the contactor.

  15. A single sorbent for tetracycline enrichment and subsequent solid-matrix time-resolved luminescence

    Energy Technology Data Exchange (ETDEWEB)

    Liu Linshu [Eastern Regional Research Center, Agriculture Research Service, US Department of Agriculture, 600 East Mermaid Lane, Wyndmoor, PA 19038 (United States)]. E-mail: lsliu@errc.ars.usda.gov; Chen Guoying [Eastern Regional Research Center, Agriculture Research Service, US Department of Agriculture, 600 East Mermaid Lane, Wyndmoor, PA 19038 (United States); Fishman, Marshall L. [Eastern Regional Research Center, Agriculture Research Service, US Department of Agriculture, 600 East Mermaid Lane, Wyndmoor, PA 19038 (United States)

    2005-01-10

    The aim of this study was to search for a sorbent that could act as an extraction phase and as a support for solid-matrix time-resolved luminescence (SMTRL). Four potential sorbents were investigated for this purpose using tetracycline (TC) as a model analyte. Sorbents prepared from C18 silica gel or calcium cross-linked pectin gel were able to extract TC from dilute solutions. Europium(III)-TC complex adsorbed on the surface of C18 generated the most intense TRL signal when measured at {lambda}{sub ex} = 388 nm and {lambda}{sub em} = 615 nm. This method achieved a 1 ng/ml limit of detection (LOD) with a 100 {mu}l sample solution in a repeated spotting mode. Hyphenation of sorbent extraction and SMTRL was demonstrated using C18. This method is suitable for screening of TC in foods or aqueous solutions and can be extended to other luminescent lanthanide-chelating analytes in physiological or environmental samples.

  16. Suspension column for recovery and separation of substances using ultrasound-assisted retention of bead sorbents.

    Science.gov (United States)

    Spivakov, Boris Ya; Shkinev, Valeriy M; Danilova, Tatiana V; Knyazkov, Nikolai N; Kurochkin, Vladimir E; Karandashev, Vasiliy K

    2012-12-15

    A novel approach to sorption recovery and separation of different substances is proposed which is based on the use of suspended bead sorbents instead of conventional packed beds of such sorbents. This makes it possible to employ small-sized beads which are trapped in a low-pressure column due to ultrasound-assisted retention, without any frits to hold the sorption material. A flow system including a separation mini-column, named herein a suspension column, has been developed and tested by the studies of solid phase extraction (SPE) of trace metals from bi-distilled water and sea water using a 150-μL column with a silica-based sorbent containing iminodiacetic groups (DIAPAK IDA) and having a grain size of 6 μm. The adsorption properties of DIAPAK IDA suspension (9.5mg) were evaluated through adsorption/desorption experiments, where the effect of solution pH and eluent on the SPE of trace metals were examined by ICP-MS or ICP-AES measurements. When sample solution was adjusted to pH 8.0 and 1 mol L(-1) nitric acid was used as eluent, very good recoveries of more than 90% were obtained for a number of elements in a single-step extraction. To demonstrate the versatility of the approach proposed and to show another advantage of ultrasonic field (acceleration of sorbate/sorbent interaction), a similar system was used for heterogeneous immunoassays of some antigens in ultrasonic field using agarose sorbents modified by corresponding antibodies. It has been shown that immunoglobulins, chlamidia, and brucellos bacteria can be quantitatively adsorbed on 15-μm sorbent (15 particles in 50 μL) and directly determined in a 50-μL mini-chamber using fluorescence detection.

  17. Development of a New Microextraction Fiber Combined to On-Line Sample Stacking Capillary Electrophoresis UV Detection for Acidic Drugs Determination in Real Water Samples

    Directory of Open Access Journals (Sweden)

    Maria Espina-Benitez

    2017-07-01

    Full Text Available A new analytical method coupling a (off-line solid-phase microextraction with an on-line capillary electrophoresis (CE sample enrichment technique was developed for the analysis of ketoprofen, naproxen and clofibric acid from water samples, which are known as contaminants of emerging concern in aquatic environments. New solid-phase microextraction fibers based on physical coupling of chromatographic supports onto epoxy glue coated needle were studied for the off-line preconcentration of these micropollutants. Identification and quantification of such acidic drugs were done by capillary zone electrophoresis (CZE using ultraviolet diode array detection (DAD. Further enhancement of concentration sensitivity detection was achieved by on-line CE “acetonitrile stacking” preconcentration technique. Among the eight chromatographic supports investigated, Porapak Q sorbent showed higher extraction and preconcentration capacities. The screening of parameters that influence the microextraction process was carried out using a two-level fractional factorial. Optimization of the most relevant parameters was then done through a surface response three-factor Box-Behnken design. The limits of detection and limits of quantification for the three drugs ranged between 0.96 and 1.27 µg∙L−1 and 2.91 and 3.86 µg∙L−1, respectively. Recovery yields of approximately 95 to 104% were measured. The developed method is simple, precise, accurate, and allows quantification of residues of these micropollutants in Genil River water samples using inexpensive fibers.

  18. Sequential injection/bead injection lab-on-valve schemes for on-line solid phase extraction and preconcentration of ultra-trace levels of heavy metals with determination by ETAAS and ICPMS

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald; Miró, Manuel

    2003-01-01

    This communication presents an overview of the state-of-the-art of the exploitation of sequential injection (SI)-bead injection (BI)-lab-on-valve (LOV) schemes for automatic on-line sample pre-treatments interfaced with ETAAS and ICPMS detection as conducted in the authors' group. The discussions......, that is, the hydrophilic SP Sephadex C-25 cation exchange and iminodiacetate based Muromac A-1 chelating resins, and the hydrophobic poly(tetrafluoroethylene) (PTFE) and poly(styrene-divinylbenzene) copolymer alkylated with octadecyl groups (C18-PS/DVB). Using ETAAS as detection device, the easy......-to-handle hydrophilic renewable reactors hold the features of improved R.S.D.s and LODs as compared to those operated in the conventional, permanent mode, in addition to the elimination of flow resistance. The hydrophobic columns fall into two categories, that is, the renewable one packed with C18-PS/DVB beads entails...

  19. Simultaneous determination of Pb and Cd in seafood by ICP OES with on-line pre-concentration by solid phase extraction with amberlite XAD-4 after complex formation with DDTP

    Directory of Open Access Journals (Sweden)

    Éder José dos Santos

    2013-02-01

    Full Text Available An on-line method for Cd and Pb pre-concentration and simultaneous determination in acid digested seafood by inductively coupled plasma optical emission spectrometry (ICP OES was developed. The on-line pre-concentration was based on the complex formation of the analytes with the ammonium salt of O,O-diethyldithiophosphate (DDTP and using the Amberlite XAD-4 resin as a solid support in a homemade column. Different conditions of the flow injection system, such as solutions flow rates, nebulizer pressure and eluent concentration were optimized. Three certified reference materials of lobster hepatopancreas, dogfish liver and fish protein, three samples of fish muscle and three samples of shrimp were digested with HNO3, H2O2 and H2SO4 in a microwave system under reflux. DDTP was added in the solutions obtained, and the mixture was injected in the FI system. Calibration curves for Cd and Pb were obtained using the standard solutions in the concentration range 0.05-0.5 µg mL-1 in the digestion medium, submitted to the same pre-concentration procedure. The quantification limits (3.3 x LOD for 5 min of pre-concentration time were 0.005 mg kg-1 Cd2+ and 0.1 mg kg-1 Pb2+ in the sample of fish or shrimp in natura, considering 1.0 g of the sample in a final volume of 50 mL. The agreement of the obtained concentrations with the certified ones (Student t-test, 95% confidence and the recoveries of spiked real samples, from 90 to 120%, demonstrated good accuracy. Precision was also adequate, with relative standard deviations from 2 to 13%. The method was accurate, precise and certainly could be applied to the digested samples of different natures.

  20. PHENIX on-line systems

    Energy Technology Data Exchange (ETDEWEB)

    Adler, S.S.; Allen, M.; Alley, G.; Amirikas, R.; Arai, Y.; Awes, T.C.; Barish, K.N.; Barta, F.; Batsouli, S.; Belikov, S.; Bennett, M.J.; Bobrek, M.; Boissevain, J.G.; Boose, S.; Britton, C.; Britton, L.; Bryan, W.L.; Cafferty, M.M.; Carey, T.A.; Chang, W.C.; Chi, C.Y.; Chiu, M.; Cianciolo, V.; Cole, B.A.; Constantin, P.; Cook, K.C.; Cunitz, H.; Desmond, E.J.; Ebisu, K.; Efremenko, Y.V.; El Chenawi, K.; Emery, M.S.; Engo, D.; Ericson, N.; Fields, D.E.; Frank, S.; Frantz, J.E.; Franz, A.; Frawley, A.D.; Fried, J.; Gannon, J.; Gee, T.F.; Gentry, R.; Giannotti, P.; Gustafsson, H.-A.; Haggerty, J.S.; Hahn, S.; Halliwell, J.; Hamagaki, H.; Hansen, A.G.; Hara, H.; Harder, J.; He, X.; Heistermann, F.; Hemmick, T.K.; Hibino, M.; Hill, J.C. E-mail: jhill@iastate.edu; Homma, K.; Jacak, B.V.; Jagadish, U.; Jia, J.; Kajihara, F.; Kametani, S.; Kamyshkov, Y.; Kandasamy, A.; Kang, J.H.; Kapustinsky, J.; Katou, K.; Kelley, M.A.; Kelly, S.; Kikuchi, J.; Kim, S.Y.; Kim, Y.G.; Kistenev, E.; Kotchetkov, D.; Kurita, K.; Lajoie, J.G.; Lenz, M.; Lenz, W.; Li, X.H.; Lin, S.; Liu, M.X.; Markacs, S.; Matathias, F.; Matsumoto, T.; Mead, J.; Mischke, R.E.; Mishra, G.C.; Moore, A.; Muniruzzamann, M.; Musrock, M.; Nagle, J.L.; Nandi, B.K.; Newby, J.; Nystrand, J.; O' Brien, E.; O' Connor, P.; Ohnishi, H.; Oskarsson, A.; Osterman, L.; Oyama, K.; Paffrath, L.; Pancake, C.E.; Pantuev, V.S.; Petridis, A.N.; Pisani, R.P.; Plagge, T.; Plasil, F.; Purschke, M.L.; Rankowitz, S.; Rao, R.; Rau, M.; Read, K.F.; Ryu, S.S.; Sakaguchi, T.; Sato, H.D.; Seto, R.; Shiina, T.; Silvermyr, D.; Simon-Gillo, J.; Simpson, M.; Sippach, W.; Skank, H.D.; Skutnik, S.; Sleege, G.A.; Smith, G.D.; Smith, M.; Stankus, P.W.; Steinberg, P.; Sugitate, T.; Sullivan, J.P.; Taketani, A.; Tamai, M.; Tanaka, Y.; Thomas, W.D.; Todd, R.; Toldo, F.; Turner, G.; Ushiroda, T.; Velkovska, J.; Hecke, H.W. van; Lith, M. van; Villatte, L.; Achen, W. von; Walker, J.W.; Wang, H.Q.; White, S.N.; Wintenberg, A.L.; Witzig, C.; Wood, L.[and others

    2003-03-01

    The PHENIX On-Line system takes signals from the Front End Modules (FEM) on each detector subsystem for the purpose of generating events for physics analysis. Processing of event data begins when the Data Collection Modules (DCM) receive data via fiber-optic links from the FEMs. The DCMs format and zero suppress the data and generate data packets. These packets go to the Event Builders (EvB) that assemble the events in final form. The Level-1 trigger (LVL1) generates a decision for each beam crossing and eliminates uninteresting events. The FEMs carry out all detector processing of the data so that it is delivered to the DCMs using a standard format. The FEMs also provide buffering for LVL1 trigger processing and DCM data collection. This is carried out using an architecture that is pipelined and deadtimeless. All of this is controlled by the Master Timing System (MTS) that distributes the RHIC clocks. A Level-2 trigger (LVL2) gives additional discrimination. A description of the components and operation of the PHENIX On-Line system is given and the solution to a number of electronic infrastructure problems are discussed.

  1. Modified sorbents for flue gas desulphurization

    Energy Technology Data Exchange (ETDEWEB)

    Bis, Z.; Radecki, M. [Czestochowa Technical Univ., Dabrowskiego (Poland). Dept. of Energy Engineering; Nowak, W.; Szymanek, A. [Czestochowa Technical Univ., Dabrowskiego (Poland). Dept. of Heting, Ventilation and Air Protection

    2002-07-01

    This paper presents a technological description of modified sorbents that are highly reactive and which offer possibilities for economic ash utilization from atmospheric circulating fluidized-bed boilers (ACFB). Effective methods to use solid combustion products are becoming a necessity to reduce emissions to the atmosphere. Desulphurization products and limestone are compounds derived from ash from fluidized bed and other boilers where dry, or self-dry methods, of desulphurization are used. The safe disposal or effective utilization of solid waste produced during simultaneous processes of combustion and waste gas desulphurization is a challenge because of the high cost of capturing sulphur from flue gases and the high cost of sorbents. Efforts are being made to find new kinds of sorbents so that their consumption can be lowered substantially. The economic use of solid wastes from combustion and desulphurization processes is also being investigated. This paper described the basic aspects of sulphur capture by calcined sorbents, and the mechanical activation of sorbents. 11 refs., 6 figs.

  2. Iron (II, III) oxide/multi-walled carbon nanotube composite as solid-phase extraction sorbent followed by ultra-high performance liquid chromatography tandem mass spectrometry for simultaneous determination of zearalenone and type A trichothecenes in Salviae miltiorrhizae Radix et Rhizoma (Danshen).

    Science.gov (United States)

    Jiang, Keqiu; Huang, Peng; Luan, Lianjun; Fan, Kai; Guo, Wenbo; Zhao, Zhihui; Wu, Yongjiang; Han, Zheng

    2017-01-27

    For the first time, a reliable solid-phase extraction (SPE) procedure using iron (II, III) oxide (Fe3O4)/multi-walled carbon nanotube (MWCNT) composite as sorbents was proposed for purification and enrichment of zearalenone (ZEA) and four type A trichothecenes (T-2 toxin (T-2), HT-2 toxin (HT-2), neosolaniol (NEO) and diacetoxyscirpenol (DAS)) in Salviae miltiorrhiza Radix et Rhizoma (Danshen). The Fe3O4/MWCNT composite was synthesized by assembling Fe3O4 with MWCNT by sonication through an "aggregation wrap" mechanism and several key parameters affecting the performance of SPE procedure such as the composition of sample loading solutions, washing and elution solvents were thoroughly investigated. After optimization, 2% acetonitrile aqueous solution as the loading solution, 5% methanol aqueous solution as the washing solution and acetone containing 0.5% formic acid as the elution solvent presented an excellent purification efficiency for the five targets in Danshen. Under the optimal sample pretreatment conditions followed by analysis with ultra-high performance liquid chromatography-tandem mass spectrometry, satisfactory linearity (R(2)≥0.991), high sensitivity (limit of quantification in the range of 1.20-4.80μgkg(-1)), good recovery (73.7-91.9%) and acceptable precision (RSD, 2.1-13.3%) were obtained. The applicability of the validated method was further verified in real Salviae miltiorrhiza Radix et Rhizoma samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Hydrogen sulfide removal from coal gas by the metal-ferrite sorbents made from the heavy metal wastewater sludge.

    Science.gov (United States)

    Tseng, Ting Ke; Chang, Han Ching; Chu, Hsin; Chen, Hung Ta

    2008-12-30

    The metal-ferrite (chromium-ferrite and zinc-ferrite) sorbents made from the heavy metal wastewater sludge have been developed for the hydrogen sulfide removal from coal gas. The high temperature absorption of hydrogen sulfide from coal gas with the metal-ferrite sorbent in a fixed bed reactor was conducted in this study. The metal-ferrite powders were the products of the ferrite process for the heavy metal wastewater treatment. The porosity analysis results show that the number of micropores of the sorbents after sulfidation and regeneration process decreases and the average pore size increases due to the acute endothermic and exothermic reactions during the sulfidation-regeneration process. The FeS, ZnS, and MnS peaks are observed on the sulfided sorbents, and the chromium extraction of the CFR6 can fulfill the emission standard of Taiwan EPA. The suitable sulfidation temperature range for chromium-ferrite sorbent is at 500-600 degrees C. In addition, effects of various concentrations of H2 and CO were also conducted in the present work at different temperatures. By increasing the H2 concentration, the sulfur sorption capacity of the sorbent decreases and an adverse result is observed in the case of increasing CO concentration. This can be explained via water-shift reaction.

  4. Determination of Cd in biological samples by flame AAS following on-line preconcentration by complexation with O,O-diethyldithiophosphate and solid phase extraction with Amberlite XAD-4.

    Science.gov (United States)

    Santos, Eder José Dos; Herrmann, Amanda Beatriz; Ribeiro, Anderson Schwingel; Curtius, Adilson José

    2005-01-30

    A method for the on-line preconcentration of Cd based on its complex formation with the ammonium salt of O,O-diethylditiophosphate (DDTP) and using the Amberlite XAD-4 resin as a solid support in a column is proposed. Cadmium was detected by flame atomic absorption spectrometry. Different conditions, such as complexing agent concentration, preconcentration time, solutions flow rates and nature and concentration of the eluent were optimized. Different detection limits (LODs) could be established by using different preconcentration times, between 30s and 5min, with corresponding LODs from 5 to 1mugL(-1), respectively. The method was validated by analyzing five biological certified samples. The relative standard deviation was usually around 3%, indicating a very good precision. The found concentrations values are in agreement with the certified ones, according to the t-test, for a confidence level of 95%. Enriched seawaters were also analyzed, and the recoveries were between 93 and 108%. The FI method is very simple and probably can be coupled to other measuring analytical techniques.

  5. Encapsulated liquid sorbents for carbon dioxide capture.

    Science.gov (United States)

    Vericella, John J; Baker, Sarah E; Stolaroff, Joshuah K; Duoss, Eric B; Hardin, James O; Lewicki, James; Glogowski, Elizabeth; Floyd, William C; Valdez, Carlos A; Smith, William L; Satcher, Joe H; Bourcier, William L; Spadaccini, Christopher M; Lewis, Jennifer A; Aines, Roger D

    2015-02-05

    Drawbacks of current carbon dioxide capture methods include corrosivity, evaporative losses and fouling. Separating the capture solvent from infrastructure and effluent gases via microencapsulation provides possible solutions to these issues. Here we report carbon capture materials that may enable low-cost and energy-efficient capture of carbon dioxide from flue gas. Polymer microcapsules composed of liquid carbonate cores and highly permeable silicone shells are produced by microfluidic assembly. This motif couples the capacity and selectivity of liquid sorbents with high surface area to facilitate rapid and controlled carbon dioxide uptake and release over repeated cycles. While mass transport across the capsule shell is slightly lower relative to neat liquid sorbents, the surface area enhancement gained via encapsulation provides an order-of-magnitude increase in carbon dioxide absorption rates for a given sorbent mass. The microcapsules are stable under typical industrial operating conditions and may be used in supported packing and fluidized beds for large-scale carbon capture.

  6. Topical Report 5: Sorbent Performance Report

    Energy Technology Data Exchange (ETDEWEB)

    Krutka, Holly; Sjostrom, Sharon

    2011-05-31

    ADA-ES has completed an extensive sorbent screening program funded primarily through DOE NETL cooperative agreement DE-NT0005649 with support from EPRI and industry cost-share participants. Tests were completed on simulated and actual flue gas. The overall project objective is to address the viability and accelerate development of a solid-based postcombustion CO2 capture technology that can be retrofit to the existing fleet of coal-fired power plants. An important component of the viability assessment was to evaluate the state of development of sorbents and measure key performance characteristics under realistic operating conditions.

  7. Simultaneous determination of six resorcylic acid lactones in feed using liquid chromatography-tandem mass spectrometry and multi-walled carbon nanotubes as a dispersive solid phase extraction sorbent.

    Science.gov (United States)

    Ying, Yong-Fei; Wu, Yin-Liang; Wen, Yi; Yang, Ting; Xu, Xiu-Qin; Wang, Yi-Zhen

    2013-09-13

    A simple and cost-effective pre-treatment procedure was developed for six resorcylic acid lactones (RALs) in feed using dispersive solid phase extraction (dSPE) with multi-walled carbon nanotubes (MWCNTs). The sample was analysed after purification by ultra-high performance liquid chromatography-negative electrospray ionisation tandem mass spectrometry (UHPLC-ESI-MS/MS). After extraction with acetonitrile/water (80:20, v/v) and dilution with water, a dSPE procedure was carried out with MWCNTs. The pH value of the extract, the extraction time for MWCNTs, the type and amount of MWCNTs and the type of eluent were optimised to increase the sample throughput and the sensitivity. The samples were quantified using the internal standard zearalenone-D6. The absolute recoveries of the target compounds from feed samples were most efficient when using 100mg of MWCNTs with an outer diameter of less than 8nm and a length of 10-30μm, and ethyl acetate was shown to be the most suitable solvent for desorbing the target compounds from the MWCNTs. The mean recoveries from fortified swine mixed feed samples ranged from 95.3% to 107.2% and had relative standard deviations lower than 10%; the limits of detection and quantification for RALs were in the ranges of 0.20-0.29μg/kg and 0.54-0.78μg/kg, respectively.

  8. Resolution of an intense sweetener mixture by use of a flow injection sensor with on-line solid-phase extraction. Application to saccharin and aspartame in sweets and drinks.

    Science.gov (United States)

    Capitán-Vallvey, L F; Valencia, M C; Arana Nicolás, E; García-Jiménez, J F

    2006-05-01

    An integrated solid-phase spectrophotometry-FIA method is proposed for simultaneous determination of the mixture of saccharin (1,2-benzisothiazol-3(2H)-one-1,1-dioxide; E-954) (SA) and aspartame (N-L-alpha-aspartyl-L-phenylalanine-1-methyl ester; E-951) (AS). The procedure is based on on-line preconcentration of AS on a C18 silica gel minicolumn and separation from SA, followed by measurement, at lambda = 210 nm, of the absorbance of SA which is transiently retained on the adsorbent Sephadex G-25 placed in the flow-through cell of a monochannel FIA setup using pH 3.0 orthophosphoric acid-dihydrogen phosphate buffer, 3.75x10(-3) mol L(-1), as carrier. Subsequent desorption of AS with methanol enables its determination at lambda = 205 nm. With a sampling frequency of 10 h(-1), the applicable concentration range, the detection limit, and the relative standard deviation were from 1.0 to 200.0 microg mL(-1), 0.30 microg mL(-1), and 1.0% (80 microg mL(-1), n = 10), respectively, for SA and from 10.0 to 200.0 microg mL(-1), 1.4 microg mL(-1), and 1.6% (100 microg mL(-1), n = 10) for AS. The method was used to determine the amounts of aspartame and saccharin in sweets and drinks. Recovery was always between 99 and 101%. The method enabled satisfactory determination of blends of SA and AS in low-calorie and dietary products and the results were compared with those from an HPLC reference method.

  9. Determination of steroidal oestrogens in tap water samples using solid-phase extraction on a molecularly imprinted polymer sorbent and quantification with gas chromatography-mass spectrometry (GC-MS).

    Science.gov (United States)

    Zacs, D; Perkons, I; Bartkevics, V

    2016-07-01

    An analytical method was established and validated for the analysis of steroidal oestrogens in tap water samples. Gas chromatography coupled to high-resolution mass spectrometry (GC-HRMS) and gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) were used for the identification/quantification of selected compounds and the analytical performance of these techniques was evaluated. Liquid-liquid extraction (LLE) and solid-phase extraction (SPE) with a molecularly imprinted polymer (MIP) stationary phase that was highly selective for oestrogens were used for the extraction of 100-mL aliquots of water samples. The recoveries of analytes with the described methods ranged from 92 to 114 %, while the repeatability in terms of relative standard deviations (RSDs) was in the range from 2.1 to 15.2 % (n = 5). It was concluded that SPE with MIP that was highly selective for oestrogens in combination with GC-HRMS detection is more preferable for the analysis of oestrogens in tap water samples. The typical oestrogen, 17β-estradiol (17β-E2), was detected above the method limit of quantification (m-LOQ) in 5 of 14 analysed tap water samples at concentrations from 0.09 to 0.15 ng L(-1). Despite that 17α-ethynylestradiol (17α-EE2) was not quantified in this study above m-LOQ, the presence of this chemical was qualitatively confirmed in some of the analysed samples.

  10. On-line solid phase extraction-high performance liquid chromatography–isotope dilution–tandem mass spectrometry approach to quantify N,N-diethyl-m-toluamide and oxidative metabolites in urine

    Energy Technology Data Exchange (ETDEWEB)

    Kuklenyik, Peter; Baker, Samuel E.; Bishop, Amanda M.; Morales-A, Pilar; Calafat, Antonia M., E-mail: aic7@cdc.gov

    2013-07-17

    Graphical abstract: -- Highlights: •A fast assay to quantify the concentrations of N,N-Diethyl-m-Toluamide and two urinary metabolites was developed •It uses online SPE, reversed phase HPLC and tandem mass spectrometry •The method is precise and accurate with limits of detection ≤1 ng mL{sup −1} -- Abstract: Human exposure to N,N-diethyl-m-toluamide (DEET) occurs because of the widespread use of DEET as an active ingredient in insect repellents. However, information on the extent of such exposure is rather limited. Therefore, we developed a fast on-line solid phase extraction–high performance liquid chromatography–isotope dilution tandem mass spectrometry (HPLC-MS/MS) method to measure in urine the concentrations of DEET and two of its oxidative metabolites: N,N-diethyl-3-(hydroxymethyl)benzamide and 3-(diethylcarbamoyl)benzoic acid (DCBA). To the best of our knowledge, this is the first HPLC-MS/MS method for the simultaneous quantification of DEET and its select metabolites in human urine. After enzymatic hydrolysis of the conjugated species in 0.1 mL of urine, the target analytes were retained and pre-concentrated on a monolithic column, separated from each other and from other urinary biomolecules on a reversed-phase analytical column, and detected by atmospheric pressure chemical ionization in positive ion mode. The limits of detection ranged from 0.1 ng mL{sup −1} to 1.0 ng mL{sup −1}, depending on the analyte. Accuracy ranged between 90.4 and 104.9%, and precision ranged between 5.5 and 13.1% RSD, depending on the analyte and the concentration. We tested the usefulness of this method by analyzing 75 urine samples collected anonymously in the Southeastern United States in June 2012 from adults with no known exposure to DEET. Thirty eight samples (51%) tested positive for at least one of the analytes. We detected DCBA most frequently and at the highest concentrations. Our results suggest that this method can be used for the analysis of a large

  11. On-line Monitoring of Extraction Process for Schisandrachinensis Using Near-Infrared Spectroscopy%基于近红外光谱的五味子提取过程在线检测方法研究

    Institute of Scientific and Technical Information of China (English)

    仲怿; 潘万芳; 朱捷强; 范骁辉; 康立源; 李正

    2014-01-01

    目的:利用近红外(NIR)光谱法,建立定量模型,实现五味子提取过程中关键指标的快速检测。方法:在线采集五味子提取液的近红外光谱,以高效液相色谱法和差重法获取参照,采用最小二乘回归法(PLSR)分别建立五味子醇甲、果糖、葡萄糖和可溶性固形物的定量模型。结果:定量模型的校正集相关系数R、校正均方根误差RMSEC、预测均方根误差RMSEP分别为:五味子醇甲0.99792、1.41、8.76,果糖0.99246、0.0919、0.333,葡萄糖0.99371、0.0954、0.448,可溶性固形物0.98723、3.07、11.2。结论:该方法快速、便捷,结果准确,适用于五味子提取过程的快速检测。%It is the objective of this study to establish quantitative models to detect quality indicators rapidly during theextraction process of Schisandrachinensis using using near-infrared (NIR) spectroscopy. NIR spectrum was collected on-line and PLSR models were developed for the contents of schisandrin , fructose, glucose and soluble solids, which were measured with HPLC and weight loss methods. For the cross validation of contents of schisandrin, fructose, glucose and soluble solids, the correlation coefficients were 0.99792, 0.99246, 0.99371 and 0.98723; RMSEC were 1.41, 0.0919, 0.0954 and 3.07; RMSEP were 8.76, 0.333, 0.448 and 11.2, respectively. In conclusion, NIR models were developed successfully to determine the quality indicators including the contents of schisandrin, fructose, glucose and soluble solids rapidly and accurately.

  12. Functionalized Organosilicate Sorbents for Air Purification

    Science.gov (United States)

    2013-12-23

    synthesized for reactive capture of targets. ADC-10 focused on incorporation of carbonyls for reactive removal of ammonia . CAR-40 focused on...16 Fig. 12 Ammonia breakthrough for E50 sorbents...23 Fig. 21 Ammonia breakthrough for the Cu DIX materials

  13. New high-capacity, calcium-based sorbents, calcium silicate sorbents. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Kenney, M.E.

    1996-02-28

    A search is being carried out for new calcium-based SO{sub 2} sorbents for induct injection. More specifically, a search is being carried out for induct injection calcium silicate sorbents that are highly cost effective. The current year objectives include the study of sorbents made by hydrating ordinary or Type I portland cement or portland cement clinker (a cement intermediate) under carefully selected conditions. Results of this study show that an excellent portland cement sorbent can be prepared by milling cement at 120{degrees}C at 600 rpm for 15 minutes with MgO-stabilized ZrO{sub 2} beads. They also show that clinker, which is cheaper than cement can be used interchangeably with cement as a starting material. Further, it is clear that while a high surface area may be a desirable property of a good sorbent, it is not a requisite property. Among the hydration reaction variables, milling time is highly important, reaction temperature is important and stirring rate and silicate-to-H{sub 2}O ratio are moderately important. The components of hydrated cement sorbent are various combinations of C-S-H, calcium silicate hydrate:Ca(OH){sub 2};AFm. a phase in hydrated cement.

  14. A Feature Extraction Algorithm of Cannon-ball Fuse Riveted Point Based on Line Scanning%基于行扫描的炮弹引信铆点特征提取

    Institute of Scientific and Technical Information of China (English)

    郝旺; 杨润泽; 尹晓春

    2011-01-01

    在炮弹引信铆点机器视觉识别中,有效消除图像中各种干扰、正确提取铆点特征是关键,解决好铆点特征的准确提取问题,是炮弹引信安全破除铆点的前提条件;根据铆点的结构特点,分析了产生各种干扰的原因及特点,在高斯滤波,阀值分割、形态学运算等基本运算的基础上,提出了一种基于行扫描的铆点特征提取方法;测试结果表明,提出的方法可行,铆点正确识别率达到90%以上,具有高效性和很好的鲁棒性的铆点特征提取,使得炮弹铆点的准确破除成为可能.%In the process of Cannon-ball Fuse Riveted point recognizing by machine vision, to eliminate the image interference effectively and to extract the riveted point feature accurately is the key point. The solution of Riveted point recognizing problem, is the condition of destroying Riveted point safely. Researching the reason of interference and its characteristic, after using basic image processing method by linear Gauss filtering, threshold segmentation, mathematical morphology, a line scanning algorithm is presented. This algorithm can resolve the problem of riveted point recognizing successfully. The recognizing accuracy ratio can reach 90 percents. To extract the riveted point feature effectively and robustly. make the operation of Fuse Riveted Point can be realized.

  15. The antimicrobial efficiency of silver activated sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Đolić, Maja B., E-mail: mirkovic.maja@gmail.com [Vinča Institute of Nuclear Sciences, University of Belgrade, P.O. Box 522, 11001 Belgrade (Serbia); Rajaković-Ognjanović, Vladana N. [Faculty of Civil Engineering, University of Belgrade, Bulevar Kralja Aleksandra 73, 11000 Belgrade (Serbia); Štrbac, Svetlana B. [ICTM-Institute of Electrochemistry, University of Belgrade, Njegoševa 12, 11001 Belgrade (Serbia); Rakočević, Zlatko Lj. [Vinča Institute of Nuclear Sciences, University of Belgrade, P.O. Box 522, 11001 Belgrade (Serbia); Veljović, Đorđe N.; Dimitrijević, Suzana I.; Rajaković, Ljubinka V. [Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, 11000 Belgrade (Serbia)

    2015-12-01

    Highlights: • Different sorbents were activated by Ag{sup +}-ions and modified sorbents were determined by sorption capacities, in range of values: 42.06–3.28 mg/g. • Granulated activated carbon (GAC), natural zeolit (Z) and titanium dioxide (T) activated by Ag{sup +}-ions were tested against E. coli, S. aureus and C. albicans. • The most successful bacteria removal was obtained using Ag/Z against S. aureus and E. coli, while the yeast cell reduction reached unsatisfactory effect for all three activated sorbents. • XRD, XPS and FE-SEM analysis showed that the chemical state of the silver activating agent affects the antimicrobial activity, as well as the structural properties of the material. • An overall microbial cell reduction, which is performed by separated antimicrobial tests on the Ag{sup +}-activated surface and Ag{sup +}-ions in aquatic solutions, is a consequence of both mechanisms. - Abstract: This study is focused on the surface modifications of the materials that are used for antimicrobial water treatment. Sorbents of different origin were activated by Ag{sup +}-ions. The selection of the most appropriate materials and the most effective activation agents was done according to the results of the sorption and desorption kinetic studies. Sorption capacities of selected sorbents: granulated activated carbon (GAC), zeolite (Z), and titanium dioxide (T), activated by Ag{sup +}-ions were following: 42.06, 13.51 and 17.53 mg/g, respectively. The antimicrobial activity of Ag/Z, Ag/GAC and Ag/T sorbents were tested against Gram-negative bacteria E. coli, Gram-positive bacteria S. aureus and yeast C. albicans. After 15 min of exposure period, the highest cell removal was obtained using Ag/Z against S. aureus and E. coli, 98.8 and 93.5%, respectively. Yeast cell inactivation was unsatisfactory for all three activated sorbents. The antimicrobial pathway of the activated sorbents has been examined by two separate tests – Ag{sup +}-ions desorbed from

  16. Inlfuence of Carbon Content on S Zorb Sorbent Activity

    Institute of Scientific and Technical Information of China (English)

    Xu Li

    2013-01-01

    The reaction activity of S Zorb sorbents with different sulfur contents was investigated, and the structure and composition of carbon-containing sorbents were characterized by XRD, FT-IR and TG-MS in order to delve into the kind and morphology of carbon on the sorbent. Test results have revealed that coke could be deposited on the S Zorb sorbent dur-ing the operating process, and the coke content was an important factor inlfuencing the reaction performance of the S Zorb sorbent. Retention of a deifnite amount of coke on the sorbent while securing the desulfurization activity of the S Zorb sor-bent would be conducive to the reduction of octane loss of reaction product.

  17. Analysis of polynuclear aromatic hydrocarbons in olive oil after solid-phase extraction using a dual-layer sorbent cartridge followed by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Stenerson, Katherine K; Shimelis, Olga; Halpenny, Michael R; Espenschied, Ken; Ye, Maochun M

    2015-05-27

    A simple and easy direct solid-phase extraction (SPE) method was developed for the analysis of polynuclear aromatic hydrocarbons (PAHs) in olive oil using a dual-layer cartridge containing activated Florisil and a mixture of octadecyl (C18)-bonded and zirconia-coated silicas. Undiluted olive oil was applied directly to the SPE cartridge, and the sample was eluted with acetonitrile solvent. Background in the extract was found to be low enough for either gas chromatography-mass spectrometry (GC-MS) or high-performance liquid chromatography with fluorescence detection (HPLC-FLD) analysis. Average recoveries for 16 different PAHs from spiked olive oil replicates were >75%, with intraday precisions of <20% relative standard deviation (% RSD). Detection limits ranged from 0.2 to 1.0 μg/kg and, specifically for the PAHs listed in EC Regulation 835/2011, benzo(a)anthracene, chrysene, benzo(b)fluoranthene, and benzo(a)pyrene, were from 0.3 to 0.7 μg/kg. The method was then applied to determine the PAH content present in commercial samples of refined versus extra-virgin olive oils.

  18. Synthesis of g-C3N4/Fe3O4 nanocomposites and application as a new sorbent for solid phase extraction of polycyclic aromatic hydrocarbons in water samples.

    Science.gov (United States)

    Wang, Man; Cui, Shihai; Yang, Xiaodi; Bi, Wentao

    2015-01-01

    An easy preparation of g-C3N4/Fe3O4 nanocomposites by chemical co-precipitation has been demonstrated. The as-prepared materials were characterized by X-ray diffraction, transmission electron microscopy, Fourier transform infrared spectroscopy and thermogravimetric analysis. The high affinity of g-C3N4 toward polycyclic aromatic hydrocarbons and the magnetic behavior of Fe3O4 were combined to provide an efficient and simple magnetic solid phase extraction (MSPE). The adsorption and desorption of polycyclic aromatic hydrocarbons on g-C3N4/Fe3O4 were examined. Different factors affecting the magnetic solid phase extraction of polycyclic aromatic hydrocarbons were assessed in terms of adsorption, desorption, and recovery. Under the optimized conditions, the proposed method showed good limits of detection (LOD, S/N=3) in the range of 0.05-0.1 ng mL(-1) and precision in the range of 1.8-5.3% (RSDs, n=3). This method was also successfully applied to the analysis of real water samples; good spiked recoveries over the range of 80.0-99.8% were obtained.

  19. 近红外在线检测技术在人参提取物生产中的应用%Application of Near-infrared Spectroscopy On-line Detection to Production Process of Ginseng Extract

    Institute of Scientific and Technical Information of China (English)

    张瑞; 王英平; 刘宏群; 许世泉; 闫梅霞; 赵景辉

    2012-01-01

    This experiment aims to use near-infrared spectroscopy to generate the spectrum of Chinese ginseng samples. The total ginseno-sides contents and near-infrared spectroscopy figure were determined in raw materials of ginseng and SS8 extract solutions. Raw materials of ginseng came from 93 different places, and born in different years. Using partial least squares (PLS), the methematical models were developed to correlate near infrared spectra and total ginsenosides contents. Method of cross-validation was adopted to evaluate these models, the results showed: Trie correlation coefficients of model were all above 0.95, the root mean square error of cross-validation (RMSEC V) values were 0.0716 and 0.032 7, ratio of deviation to performances (RPD) of model finally developed were 2.83 and 3.97 respectively. The model achieved the best prediction performance, and there is no significant difference between predictive contents and chemical reference values. The result indicates that NIR spectroscopy could be used in practice to fast determine the total ginsenoside contents of powder and extract solutions.%采用比色法和近红外漫反射、液体透射在线检测技术,分别测定93个不同产地、不同年生人参原材料固体样品和558个人参提取液样品的总皂苷含量和近红外光谱,结合偏最小二乘回归法,建立样品总皂苷含量与近红外光谱之间的数学模型.采用内部交叉检验对模型进行评价.评价结果显示:内部交叉检验的决定系数R2> 0.95,交义检验均方差(RMSECV)值分别为0.071 6和0.032 7,相对分析误差(RPD)分别为2.83和3.97.模型评价数据均有较好的表现,原材料、提取液检验样品近红外测定结果与化学参考值之间无显著性差异,近红外检测技术可以应用于人参原材料固体样品和人参提取液样品中总皂苷含量的快速测定.

  20. Application of Near-infrared Spectroscopy On -line Detection to Production Process of Atractylodes Japonica Extract%关苍术提取过程中近红外在线检测模型建立研究

    Institute of Scientific and Technical Information of China (English)

    张海波; 张瑞; 傅禹砜; 丁秀峰; 王英平

    2013-01-01

    Using near-infrared (NIR) spectroscopy to obtain the spectrum of atractylodes japonica sample ,and the atractylodin contents of the sample determined by colorimetric method .The sample contents 64 atractylodes japonica powders in different origin places and years ,and 128 extract solutions derived from the powders .Using partial least squares (PLS ) ,the calibration models were developed to correlate near infrared spectra and atractylodin contents .Using cross-validation evaluating the models ,the results showed:the correlation coefficients of model were 90.68 and 95.71 ,the root mean square error of cross-validation(RMSECV) values were 0.011 2 and 0.020 0 ,ratio of deviation to perfor-mances(RPD) of model finally developed were 3.43 and 3.86 respectively .The model achieved the best prediction performance ,and there is no significant difference between predictive contents and chemical values .The results indicated that NIR spectroscopy could be used in practice to fast determine the atractylodin contents of powder and extract solutions .%采用比色法和近红外漫反射、液体透射在线检测技术,分别测定64个关苍术原材料固体样品和128个关苍术提取液样品的苍术素含量和近红外光谱,结合偏最小二乘回归法,建立样品苍术素含量与近红外光谱之间的数学模型。采用内部交叉检验对模型进行评价,评价结果显示,决定系数 R2为90.68、95.71,交叉检验均方差(RMSECV )值分别为0.0112、0.0200,相对分析误差(RPD )分别为3.43、3.86。模型评价数据均有较好的表现,原材料、提取液检验样品近红外测定结果与化学参考值之间无显著性差异,近红外检测技术可以应用于关苍术原材料固体样品和关苍术提取液样品中苍术素含量的在线检测。

  1. Determination of 3,4-methylenedioxymethamphetamine and its five main metabolites in rat urine by solid-phase extraction and high performance liquid chromatography with on line mass spectrometry.

    Science.gov (United States)

    Menet, Marie-Claude; Fonsart, Julien; Hervé, Françoise; Fompeydie, Dominique; Galliot-Guilley, Martine; Noble, Florence; Scherrmann, Jean-Michel

    2010-10-15

    The consumption of psychostimulant amphetamine-like drugs has increased significantly in recent years. Some MDMA metabolites are probably involved in the neurotoxicity and neurodegeneration caused by prolonged use rather than MDMA itself. We recently developed a method to analyze MDMA and its five main metabolites in rat plasma [7]. We have now fully validated this method to the quantification of these drugs in rat urine. We extracted MDMA and its metabolites with Oasis WCX cartridges, separated them on a Nucleodur C18 analytical column and quantified them by ion-trap mass spectrometry. Linearity was excellent: 12.5-1250ng/mL urine for HMA, HMMA, MDA and MDMA, 25-2500ng/mL for HHMA, and 150-7500ng/mL for HHA (r(2)>0.993 for all analytes). The lower limits of quantification were 12.5ng/mL urine for MDMA, MDA, HMA and HMMA, 25ng/mL for HHMA and 150ng/mL for HHA. Reproducibility was good (intra-assay precision=1.7-6.1%; inter-assay precision=0.6-5.7%), as was accuracy (intra-assay deviation=0.1-4.8%; inter-assay deviation=0.7-7.9%). Average recoveries were around 85.0%, except for HHMA (66.2%) and HHA (53.0%) (CVurine samples taken over 24h from rats given subcutaneous MDMA.

  2. Sulfur dioxide removal by sol-gel sorbent derived CuO/Alumina sorbents in fixed bed adsorber

    Directory of Open Access Journals (Sweden)

    Zhong-Min Wang

    2017-02-01

    Full Text Available Nanostructured alumina supported copper oxide granular sorbents were prepared by the sol-gel method. The properties of the sol-gel derived sorbents were compared with a similar commercial sorbent which has been used in the pilot scale moving-bed copper oxide process for flue gas treatment. The crushing strength of the sol-gel derived sorbents is about 6–7 times that of the commercial samples, while the attrition rate of the former is at least 3 times smaller. At temperatures below 400 °C, SO2 sorption capacity of the sol-gel derived sorbent is about 3 times that of the commercial sorbent with a similar amount of CuO loading (7–9 wt%. The better mechanical properties and higher sulfation capacity of the sol-gel derived alumina supported copper oxide sorbents are due to their unique microstructure and the coating method for CuO.

  3. Seawater uranium sorbents: preparation from a mesoporous copolymer initiator by atom-transfer radical polymerization

    Energy Technology Data Exchange (ETDEWEB)

    Yue, Yanfeng; Mayes, Richard T.; Fulvio, Pasquale F.; Sun, Xiao-Guang [Chemical Sciences Division, Oak Ridge National Laboratory, Oak Ridge, TN (United States); Kim, Jungseung; Tsouris, Costas [Energy and Transportation Science Division, Oak Ridge National Laboratory, Oak Ridge, TN (United States); Chen, Jihua [Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge, TN (United States); Brown, Suree [Department of Chemistry, University of Tennessee, Knoxville, TN (United States); Dai, Sheng [Chemical Sciences Division, Oak Ridge National Laboratory, Oak Ridge, TN (United States); Department of Chemistry, University of Tennessee, Knoxville, TN (United States)

    2013-12-09

    Nanoporous template-free initiators for atom-transfer radical polymerization (ATRP) were synthesized with surface and framework initiator sites and tailorable pore structures. Polyacrylonitrile grown on one initiator was converted into polyamidoxime to generate a uranium sorbent for seawater extraction with a high uptake rate and capacity relative to those of nonwoven irradiation-grafted polyethylene-fiber composites. (Copyright copyright 2013 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  4. 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/....

  5. KINETICS OF HOT-GAS DESULFURIZATION SORBENTS FOR TRANSPORT REACTORS

    Energy Technology Data Exchange (ETDEWEB)

    K.C. Kwon

    2003-02-01

    Hot-gas desulfurization for the integrated gasification combined cycle (IGCC) process has been investigated by many researchers to remove effectively hydrogen sulfide with various metal oxide sorbents at elevated temperatures. Various metal oxide sorbents are formulated with metal oxides such as Fe, Co, Zn, and Ti. Initial reaction kinetics of formulated sorbents with hydrogen sulfide is studied in the presence of various amounts of moisture and hydrogen at various reaction temperatures. The objectives of this research are to study initial reaction kinetics for a sorbent-hydrogen sulfide heterogeneous reaction system, to investigate effects of concentrations of hydrogen sulfide, hydrogen, and moisture on dynamic absorption of H{sub 2}S into sorbents, and to evaluate effects of temperature and sorbent amounts on dynamic absorption of H{sub 2}S into sorbents. Experimental data on initial reaction kinetics of hydrogen sulfide with metal oxide sorbents were obtained with a 0.83-cm{sup 3} differential reactor. The reactivity of EX-SO3 was examined in this report. This sorbent was obtained from the Research Triangle Institute (RTI). The sorbent in the form of 110 {micro}m particles are reacted with 18000-ppm hydrogen sulfide at 350-550 C. The range of space time of reaction gas mixtures is 0.069-0.088 s. The range of reaction duration is 4-180 s.

  6. KINETICS OF HOT-GAS DESULFURIZATION SORBENTS FOR TRANSPORT REACTORS

    Energy Technology Data Exchange (ETDEWEB)

    K.C. Kwon

    2002-01-01

    Hot-gas desulfurization for the integrated gasification combined cycle (IGCC) process has been investigated by many researchers to remove effectively hydrogen sulfide with various metal oxide sorbents at elevated temperatures. Various metal oxide sorbents are formulated with metal oxides such as Fe, Co, Zn, and Ti. Initial reaction kinetics of formulated sorbents with hydrogen sulfide is studied in the presence of various amounts of moisture and hydrogen at various reaction temperatures. The objectives of this research are to study initial reaction kinetics for a sorbent-hydrogen sulfide heterogeneous reaction system, to investigate effects of concentrations of hydrogen sulfide, hydrogen, and moisture on dynamic absorption of H{sub 2}S into sorbents, and to evaluate effects of temperature and sorbent amounts on dynamic absorption of H{sub 2}S into sorbents. Experimental data on initial reaction kinetics of hydrogen sulfide with metal oxide sorbents were obtained with a 0.83-cm{sup 3} differential reactor. The reactivity of MCRH-67 was examined in this report. This sorbent was obtained from the Research Triangle Institute (RTI). The sorbent in the form of 130 mm particles are reacted with 18000-ppm hydrogen sulfide at 350-525 C. The range of space time of reaction gas mixtures is 0.069-0.088 s. The range of reaction duration is 4-180 s.

  7. Copper-based sorbents for hot coal gas desulfurization systems

    Energy Technology Data Exchange (ETDEWEB)

    Abbasian, J.; Slimane, R.B.; Zarnegar, M.K. [Inst. of Gas Technology, Des Plaines, IL (United States)] [and others

    1997-07-01

    High-temperature coal gas desulfurization has been recognized as essential in the development of emerging power generation technologies such as the Integrated Gasification Combined Cycle (IGCC), aiming to improve both the efficiency and environmental performance of power generation from coal. Hot gas desulfurization may be accomplished by using regenerable mixed metal oxides sorbents which can reduce the H{sub 2}S content of the coal gas to a few ppmv over many sulfidation/regeneration cycles. The focus of much of the current research on hot gas desulfurization has been on the use of zinc-based sorbents. Although these sorbents have been the subject of extensive pilot-scale and process development work, zinc-based sorbents have been shown to suffer from sulfate formation and zinc volatilization, leading to sorbent degradation over multicycle use, increasing sorbent replacement costs and the overall cost of hot gas desulfurization processes. A novel copper-chromite sorbent has been developed at IGT for hot coal gas desulfurization under the sponsorship of the Illinois Clean Coal Institute (ICCI). Results obtained so far indicate that this sorbent, in granular form (i.e., CuCr-29), has a much higher attrition resistance compared to the commercial granular zinc titanate sorbent, as well as excellent desulfurization efficiency. Furthermore, unlike most zinc titanate sorbents, the reactivity of IGT`s CuCr-29 sorbent gradually and consistently improved during the 20 cycles tested. The sorbent preparation techniques developed at IGT have been applied to produce highly reactive and attrition resistant sorbent pellets for moving-bed applications.

  8. High-throughput cytochrome P450 (CYP) inhibition screening via cassette probe-dosing strategy. I. Development of direct injection/on-line guard cartridge extraction/tandem mass spectrometry for the simultaneous detection of CYP probe substrates and their metabolites.

    Science.gov (United States)

    Bu, H Z; Magis, L; Knuth, K; Teitelbaum, P

    2000-01-01

    A highly efficient direct injection/on-line guard cartridge extraction/tandem mass spectrometry (DI-GCE/MS/MS) method utilizing electrospray polarity switching was developed for the simultaneous detection of probe substrates and marker metabolites of seven human hepatic cytochrome P450 (CYP) isozymes: CYP1A2, 2A6, 3A4, 2C9, 2C19, 2D6 and 2E1. Microsomal incubations were terminated with formic acid, centrifuged, and the resulting supernatants were injected for analysis by DI-GCE/MS/MS. This method employed an extremely short C(18) cartridge (4 mm in length) which allowed rapid cleanup of sample matrices while retaining the analytes an appropriate time (2. 0-2.2 min). From 1.5 to 2.7 min the effluent was directed to the mass spectrometer for detection otherwise diverted to waste. As a result of the efficient on-line extraction, matrix (e.g., salts and proteins) suppression was minimized. In addition, no visible source contamination was observed and system performance (chromatographic and mass spectrometric) did not significantly deteriorate after 500 consecutive injections. Electrospray polarity switching was strategically executed on a Micromass Quattro II mass spectrometer by establishing dummy ion transitions to protect the analytes from the interference of the overwhelming noise which was unavoidable for the first transition scanned following each polarity switch. This unique strategy led to the simultaneous detection of seven CYP probe substrates and seven corresponding marker metabolites (12 by positive mode and 2 by negative mode).

  9. 在线萃取流动注射分光光度法测定消毒食(饮)具烷基苯磺酸钠残留量%Determination of sodium alkylbenzene sulfonate residues in disinfected tableware by on-line extraction FI-spectrophotometry

    Institute of Scientific and Technical Information of China (English)

    郝莉鹏; 闵巍; 李宏亮

    2012-01-01

    目的:建立在线萃取流动注射分光光度法测定食(饮)具烷基苯磺酸钠残留量的方法.方法:100 ml蒸馏水冲洗消毒后食(饮)具制成样液,用在线萃取流动注射分光光度法进行测定.结果:方法检出限1.7 μg/100 cm2,烷基苯磺酸钠的浓度在0 mg/L ~1.00 mg/L有良好的线性(相关系数0.9995),实际样品的加标回收率为92% ~104%,相对标准偏差为3% ~8.5%.结论:本方法操作简便,准确度、精密度好,对操作人员的危害小,适用于消毒食(饮)具中烷基苯磺酸钠残留量的批量检测.%Objective: To establish on - line extraction FI - spectrophotometry for the determination of sodium al-kylbenzene sulfonate residues in disinfected tableware. Methods: The disinfected tableware was rinsed by 100 ml distilled water to obtain the sample solution. Then the sample solution was determined by on - line extraction FI -spectrophotometry. Results: The detection limit was 1. 7 μg/100 cm with linear range of 0 mg/L ~ 1. 00 mg/L ( r = 0.9995). The recoveries were 92% ~ 104% , RSD=3% -8.5%. Conclusion: This method is simple, sensitive, accurate and safe for the determination of sodium alkylbenzene sulfonate residues in disinfected tableware.

  10. Nanoporous carbon sorbent for molecular-sieve chromatography of lipoprotein complex

    Science.gov (United States)

    Kerimkulova, A. R.; Mansurova, B. B.; Gil'manov, M. K.; Mansurov, Z. A.

    2012-06-01

    The physicochemical characteristics of carbon sorbents are investigated. Electron microscopy data for the sorbent and separated lipoprotein complex are presented. It is found that the obtained carbon sorbent possess high porosity. Nanoporous carbon sorbents for the chromatography of molecular-sieve markers are obtained and tested. The applicability of nanoporous carbon sorbents for separation of lipoprotein complexes (LPC) is investigated.

  11. Are on-line currencies virtual banknotes?

    OpenAIRE

    Stephen F. Quinn; William Roberds

    2003-01-01

    The history of money is marked by innovations that have expanded the role of "inside money"-money created by the private sector. For instance, the past few years have seen the development of several types of on-line payment arrangements, some of which have been dubbed "on-line currencies." ; This article examines the likely success or failure of on-line currencies by means of a historical analogy. The discussion compares the introduction of on-line currencies to the debut of the bearer bankno...

  12. Layered solid sorbents for carbon dioxide capture

    Science.gov (United States)

    Li, Bingyun; Jiang, Bingbing; Gray, McMahan L; Fauth, Daniel J; Pennline, Henry W; Richards, George A

    2013-02-25

    A solid sorbent for the capture and the transport of carbon dioxide gas is provided having at least one first layer of a positively charged material that is polyethylenimine or poly(allylamine hydrochloride), that captures at least a portion of the gas, and at least one second layer of a negatively charged material that is polystyrenesulfonate or poly(acryclic acid), that transports the gas, wherein the second layer of material is in juxtaposition to, attached to, or crosslinked with the first layer for forming at least one bilayer, and a solid substrate support having a porous surface, wherein one or more of the bilayers is/are deposited on the surface of and/or within the solid substrate. A method of preparing and using the solid sorbent is provided.

  13. Adsorption of Ammonia on Regenerable Carbon Sorbents

    Science.gov (United States)

    Wójtowicz, Marek A.; Cosgrove, Jesph E.; Serio, Michael A..; Wilburn, Monique

    2015-01-01

    Results are presented on the development of reversible sorbents for the combined carbon dioxide, moisture, and trace-contaminant (TC) removal for use in Extravehicular Activities (EVAs), and more specifically in the Primary Life Support System (PLSS). The currently available life support systems use separate units for carbon dioxide, trace contaminants, and moisture control, and the long-term objective is to replace the above three modules with a single one. Data on sorption and desorption of ammonia, which is a major TC of concern, are presented in this paper. The current TC-control technology involves the use of a packed bed of acid-impregnated granular charcoal, which is non-regenerable, and the carbon-based sorbent under development in this project can be regenerated by exposure to vacuum at room temperature. In this study, several carbon sorbents were fabricated and tested for ammonia sorption. Ammonia-sorption capacity was related to carbon pore structure characteristics, and the temperature of oxidative carbon-surface treatment was optimized for enhanced ammonia-sorption performance.

  14. Supported-sorbent injection. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Nelson, S. Jr.

    1997-07-01

    A new retrofitable, wastefree acid-rain control concept was pilot-tested at Ohio Edison`s high-sulfur coal-fired R.E. Burger generating station at the 2-MWe level. During the project, moistened {open_quotes}supported{close_quotes} sorbents, made from a combination of lime and vermiculite or perlite, were injected into a humidified 6,500-acfm flue-gas slipstream. After the sorbents reacted with the sulfur dioxide in the flue gas, they were removed from ductwork with a cyclone and baghouse. The $1.0 million project was co-funded by Sorbent Technologies Corporation, the Ohio Edison Company, and the Ohio Coal Development Office. The project included a preliminary bench-scale testing phase, construction of the pilot plant, parametric studies, numerous series of recycle tests, and a long-term run. The project proceeded as anticipated and achieved its expected results. This duct injection technology successfully demonstrated SO{sub 2}-removal rates of 80 to 90% using reasonable stoichiometric injection ratios (2:1 Ca:S) and approach temperatures (20-25F). Under similar conditions, dry injection of hydrated lime alone typically only achieves 40 to 50% SO{sub 2} removal. During the testing, no difficulties were encountered with deposits in the ductwork or with particulate control, which have been problems in tests of other duct-injection schemes.

  15. Carbon Dioxide Capture from Flue Gas Using Dry, Regenerable Sorbents

    Energy Technology Data Exchange (ETDEWEB)

    David A. Green; Thomas O. Nelson; Brian S. Turk; Paul D. Box Raghubir P. Gupta

    2006-09-30

    This report describes research conducted between July 1, 2006 and September 30, 2006 on the use of dry regenerable sorbents for removal of carbon dioxide (CO{sub 2}) from coal combustion flue gas. Modifications to the integrated absorber/ sorbent regenerator/ sorbent cooler system were made to improve sorbent flow consistency and measurement reliability. Operation of the screw conveyor regenerator to achieve a sorbent temperature of at least 120 C at the regenerator outlet is necessary for satisfactory carbon dioxide capture efficiencies in succeeding absorption cycles. Carbon dioxide capture economics in new power plants can be improved by incorporating increased capacity boilers, efficient flue gas desulfurization systems and provisions for withdrawal of sorbent regeneration steam in the design.

  16. Role of Hansen solubility parameters in solid phase extraction.

    Science.gov (United States)

    Bielicka-Daszkiewicz, K; Voelkel, A; Pietrzyńska, M; Héberger, K

    2010-08-27

    The sorbent-eluent systems combined from eight polymeric sorbents and seven solvents as eluents were used for the extraction of phenol and its oxidation products from water samples. The individual interactions between sorbents, eluents and analytes were characterized by Hansen solubility parameters. Principal components analysis (PCA) was used for revealing the dominant interactions (dispersive, polar, and hydrogen bonding type) in sorbent-analyte-eluent systems. The importance of solubility parameters was also determined by a novel procedure based on sum of ranking differences (SRD). Although PCA and ranking by SRD are based on different principles and calculations, they have provided very similar results. The recovery in a given system has been predicted from the magnitudes of mutual interactions (sorbent-analyte, sorbent-eluent, analyte-eluent) by multiple linear regression.

  17. ADVANCED SORBENT DEVELOPMENT PROGRAM DEVELOPMENT OF SORBENTS FOR MOVING-BED AND FLUIDIZED-BED APPLICATIONS

    Energy Technology Data Exchange (ETDEWEB)

    R.E Ayala; V.S. Venkataramani; Javad Abbasian; Rachid B. Slimane; Brett E. Williams; Minoo K. Zarnegar; James R. Wangerow; Andy H. Hill

    2000-03-31

    The integrated gasification combined cycle (IGCC) power system using high-temperature coal gas cleanup is one of the most promising advanced technologies for the production of electric power from coal in an environmentally acceptable manner. Unlike conventional low-temperature cleanup systems that require costly heat exchangers, high-temperature coal gas cleanup systems can be operated near 482-538 C (900-1000 F) or higher, conditions that are a closer match with the gasifier and turbine components in the IGCC system, thus resulting is a more efficient overall system. GE is developing a moving-bed, high-temperature desulfurization system for the IGCC power cycle in which zinc-based regenerable sorbents are currently being used as desulfurization sorbents. Zinc titanate and other proprietary zinc-based oxides are being considered as sorbents for use in the Clean Coal Technology Demonstration Program at Tampa Electric Co.'s (TECo) Polk Power Station. Under cold startup conditions at TECo, desulfurization and regeneration may be carried out at temperatures as low as 343 C (650 F), hence a versatile sorbent is desirable to perform over this wide temperature range. A key to success in the development of high-temperature desulfurization systems is the matching of sorbent properties for the selected process operating conditions, namely, sustainable desulfurization kinetics, high sulfur capacity, and mechanical durability over multiple cycles. Additionally, the sulfur species produced during regeneration of the sorbent must be in a form compatible with sulfur recovery systems, such as sulfuric acid or elemental sulfur processes. The overall objective of this program is to develop regenerable sorbents for hydrogen sulfide removal from coal-derived fuel gases in the temperature range 343-538 C (650-1000 F). Two categories of reactor configurations are being considered: moving-bed reactors and fluidized-bed (bubbling and circulating) reactors. In addition, a cost

  18. ADVANCED SORBENT DEVELOPMENT PROGRAM; DEVELOPMENT OF SORBENTS FOR MOVING-BED AND FLUIDIZED-BED APPLICATIONS

    Energy Technology Data Exchange (ETDEWEB)

    AYALA, R E; VENKATARAMANI, V S

    1998-09-30

    The integrated gasification combined cycle (IGCC) power system using high-temperature coal gas cleanup is one of the most promising advanced technologies for the production of electric power from coal in an environmentally acceptable manner. Unlike conventional low-temperature cleanup systems that require costly heat exchangers, high-temperature coal gas cleanup systems can be operated near 482-538 °C (900-1000 °F) or higher, conditions that are a closer match with the gasifier and turbine components in the IGCC system, thus resulting is a more efficient overall system. GE is developing a moving-bed, high-temperature desulfurization system for the IGCC power cycle in which zinc-based regenerable sorbents are currently being used as desulfurization sorbents. Zinc titanate and other proprietary zinc-based oxides are being considered as sorbents for use in the Clean Coal Technology Demonstration Program at Tampa Electric Co.'s (TECo) Polk Power Station. Under cold startup conditions at TECo, desulfurization and regeneration may be carried out at temperatures as low as 343 °C (650 °F), hence a versatile sorbent is desirable to perform over this wide temperature range. A key to success in the development of high-temperature desulfurization systems is the matching of sorbent properties for the selected process operating conditions, namely, sustainable desulfurization kinetics, high sulfur capacity, and mechanical durability over multiple cycles. Additionally, the sulfur species produced during regeneration of the sorbent must be in a form compatible with sulfur recovery systems, such as sulfuric acid or elemental sulfur processes. The overall objective of this program is to develop regenerable sorbents for hydrogen sulfide removal from coal-derived fuel gases in the temperature range 343-538 °C (650-1000 °F). Two categories of reactor configurations are being considered: moving-bed reactors and fluidized-bed (bubbling and circulating) reactors. In addition, a

  19. Regenerable sorbent technique for capturing CO.sub.2 using immobilized amine sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Pennline, Henry W; Hoffman, James S; Gray, McMahan L; Fauth, Daniel J; Resnik, Kevin P

    2013-08-06

    The disclosure provides a CO.sub.2 absorption method using an amine-based solid sorbent for the removal of carbon dioxide from a gas stream. The method disclosed mitigates the impact of water loading on regeneration by utilizing a conditioner following the steam regeneration process, providing for a water loading on the amine-based solid sorbent following CO.sub.2 absorption substantially equivalent to the moisture loading of the regeneration process. This assists in optimizing the CO.sub.2 removal capacity of the amine-based solid sorbent for a given absorption and regeneration reactor size. Management of the water loading in this manner allows regeneration reactor operation with significant mitigation of energy losses incurred by the necessary desorption of adsorbed water.

  20. On line routing per mobile phone

    DEFF Research Database (Denmark)

    Bieding, Thomas; Görtz, Simon; Klose, Andreas

    2009-01-01

    On-line routing is concerned with building vehicle routes in an ongoing fashion in such a way that customer requests arriving dynamically in time are efficiently and effectively served. An indispensable prerequisite for applying on-line routing methods is mobile communication technology. Addition...

  1. Simple test guidelines for screening oilspill sorbents for toxicity

    Energy Technology Data Exchange (ETDEWEB)

    Blenkinsopp, S.A.; Sergy, G. [Environment Canada, Edmonton, AB (Canada); Doe, K.; Jackman, P. [Environment Canada, Moncton, NB (Canada); Huybers, A. [Harris Industrial Testing Services Ltd., Milford, NS (Canada)

    1998-09-01

    Environment Canada`s Emergencies Science Division has established a program to develop a standard test method suitable for evaluating the toxicity of common sorbent materials. Sorbents are used to absorb or adsorb spilled oil and other hazardous materials. They vary widely in composition and packaging. They are often treated with oleophilic and hydrophobic compounds to improve performance and have been used in large quantities during oil spills. Until now, their potential toxicity has never been considered. Three tests have been evaluated to determine how appropriate they are in screening the toxicity of sorbents. Seven toxicity test recommendations for sorbents were presented. 7 refs., 3 tabs., 2 figs.

  2. Enhanced durability and reactivity for zinc ferrite desulfurization sorbent

    Energy Technology Data Exchange (ETDEWEB)

    Jha, M.C.; Berggren, M.H.

    1988-11-14

    AMAX Research Development Center (AMAX R D) has been investigating methods for enhancing the reactivity and durability of the zinc ferrite desulfurization sorbent. Zinc ferrite sorbents are intended for use in desulfurization of hot coal gas in integrated gasification combined cycle (IGCC) or molten carbonate fuel cell (MCFC) applications. For the present program, the reactivity of the sorbent may be defined as its sulfur sorption capacity at the breakthrough point and at saturation in a bench-scale, fixed-bed reactor. Durability may be defined as the ability of the sorbent to maintain important physical characteristics such As size, strength, and specific surface area during 10 cycles of sulfidation and oxidation.

  3. Study of physical chemical properties of nanostructured carbon sorbent for cleanup of biomolecules

    OpenAIRE

    Almagul Kerimkulova; M. Koldasbekova; Аmіr Kenzhehan; Moldir Kerimkulova; Zulkhair Mansurov; Murat Gilmanov

    2012-01-01

    The technology of nanostructured carbon sorbent. Optimized the conditions of carbonization of plant material and studied the basic structural and physicochemical properties of the sorbent. Studied the molecular-sieve and adsorption characteristics of the sorbent.

  4. Study of physical chemical properties of nanostructured carbon sorbent for cleanup of biomolecules

    Directory of Open Access Journals (Sweden)

    Almagul Kerimkulova

    2012-03-01

    Full Text Available The technology of nanostructured carbon sorbent. Optimized the conditions of carbonization of plant material and studied the basic structural and physicochemical properties of the sorbent. Studied the molecular-sieve and adsorption characteristics of the sorbent.

  5. Determination of trace metal ions via on-line separation and preconcentration by means of chelating Sepharose beads in a sequential injection lab-on-valve (SI-LOV) system coupled to electrothermal atomic absorption spectrometric detection

    DEFF Research Database (Denmark)

    Long, Xiangbao; Hansen, Elo Harald; Miró, Manuel

    2005-01-01

    The analytical performance of an on-line sequential injection lab-on-valve (SI-LOV) system using chelating Sepharose beads as sorbent material for the determination of ultra trace levels of Cd(II), Pb(II) and Ni(II) by electrothermal atomic absorption spectrometry (ETAAS) is described and discussed...

  6. Optimizing the Costs of Solid Sorbent-Based CO2 Capture Process Through Heat Integration

    Energy Technology Data Exchange (ETDEWEB)

    Sjostrom, Sharon [Ada-Es, Inc., Highlands Ranch, CO (United States)

    2016-03-18

    The focus of this project was the ADAsorb™ CO2 Capture Process, a temperature-swing adsorption process that incorporates a three-stage fluidized bed as the adsorber and a single-stage fluidized bed as the regenerator. ADAsorb™ system was designed, fabricated, and tested under DOE award DEFE0004343. Two amine-based sorbents were evaluated in conjunction with the ADAsorb™ process: “BN”, an ion-exchange resin; and “OJ”, a metal organic framework (MOF) sorbent. Two cross heat exchanger designs were evaluated for use between the adsorber and regenerator: moving bed and fluidized bed. The fluidized bed approach was rejected fairly early in the project because the additional electrical load to power blowers or fans to overcome the pressure drop required for fluidization was estimated to be nominally three times the electrical power that could be generated from the steam saved through the use of the cross heat exchanger. The Energy Research Center at Lehigh University built and utilized a process model of the ADAsorb™ capture process and integrated this model into an existing model of a supercritical PC power plant. The Lehigh models verified that, for the ADAsorb™ system, the largest contributor to parasitic power was lost electrical generation, which was primarily electric power which the host plant could not generate due to the extraction of low pressure (LP) steam for sorbent heating, followed by power for the CO2 compressor and the blower or fan power required to fluidize the adsorber and regenerator. Sorbent characteristics such as the impacts of moisture uptake, optimized adsorption and regeneration temperature, and sensitivity to changes in pressure were also included in the modeling study. Results indicate that sorbents which adsorb more than 1-2% moisture by weight are unlikely to be cost competitive unless they have an extremely high CO2 working capacity that well exceeds 15% by weight. Modeling also revealed

  7. 在线固相萃取-超高效液相色谱-串联质谱法测定乳制品中双酚A等4种内分泌干扰物%Determination of 4 Environmental Endocrine Disruptors Involving Bisphenol A in Dairy Products by On-line Solid Phase Extraction Coupled with Liquid Chromatography-Tandem Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    张品; 张晶; 陈洁君; 段鹤君; 邵兵

    2014-01-01

    A simple analytical method by means of on-line solid phase extraction followed liquid chromatography-tandem mass spectrometry ( SPE-LC-MS/MS) was developed for the simultaneous quantitation of 4 endocrine disruptors ( triclosan, triclocarban, bisphenol A and nonylphenol) in dairy products. Infant formula and milk samples were dissolved in acetic acid buffer and hydrolyzed by β-glucuronidase/arylsulfatase. Acetonitrile was used as the extract. Then, the mixture was freeze-centrifuged for 10 min and the supernatant was diluted with water, and analyzed via on-line SPE-LC-MS/MS. The sample extracts were concentrated by an Xbridge C8 cartridge and separated on a BEH C18 column with a gradient mobile phase of methanol and water; then analyzed by triple quadrupole mass spectrometry. Mass acquisition was conducted under negative electrospray ionization mode. Quantification was performed by isotopic internal standard calibration. Acceptable linearity (R2>0. 99) was achieved over the range of 0. 005-5. 0 μg/L, with limits of quantification of 0. 03-1. 0μg/kg. Average recoveries of four target compounds (spiked at three concentration levels) ranged from 80. 2%-106. 7%,with relative standard deviation less than 15%. Due to its rapidity, simplicity, and high sensitivity, the method is suitable for the analysis of endocrine disruptors in dairy products. It has been applied in the analysis of raw milk and milk products collected in Beijing. As a result, nonylphenol was found with a high detectable frequency.%建立了乳制品中三氯生、三氯卡班、双酚A和壬基酚4种内分泌干扰物的在线固相萃取超高压液相色谱-串联质谱(On-line SPE LC-MS/MS)检测方法。液态乳制品或奶粉样品中加入乙酸缓冲液,目标物经β-葡糖醛酸苷肽酶/芳基磺酸酯酶酶解后,用乙腈提取,冷冻离心10 min后,取上清液,用水稀释,在线固相萃取串联质谱法测定。样品溶液经Xbridge C8柱富集,BEH C18色谱柱分离,甲醇和

  8. Determination of Hg{sup 2+} by on-line separation and pre-concentration with atmospheric-pressure solution-cathode glow discharge atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li, Qing [Shanghai Institute of Ceramics, Chinese Academy of Science, Shanghai 200050 (China); Zhang, Zhen [Shanghai Institute of Ceramics, Chinese Academy of Science, Shanghai 200050 (China); School of Materials Science and Engineering, Shanghai University, Shanghai 200072 (China); Wang, Zheng, E-mail: wangzheng@mail.sic.ac.cn [Shanghai Institute of Ceramics, Chinese Academy of Science, Shanghai 200050 (China)

    2014-10-03

    Highlights: • A modified SBA-15 mesoporous silica (SH-SBA-15) was synthesized as a sorbent. • On-line SPE combined with SCGD-AES based on FIA was used to detect Hg{sup 2+} firstly. • A simple, low-cost Hg{sup 2+} analysis in a complex matrix was established. • The sensitive detection of Hg{sup 2+} was achieved with a detection limit of 0.75 μg L{sup −1}. - Abstract: A simple and sensitive method to determine Hg{sup 2+} was developed by combining solution-cathode glow discharge atomic emission spectrometry (SCGD-AES) with flow injection (FI) based on on-line solid-phase extraction (SPE). We synthesized L-cysteine-modified mesoporous silica and packed it in an SPE microcolumn, which was experimentally determined to possess a good mercury adsorption capacity. An enrichment factor of 42 was achieved under optimized Hg{sup 2+} elution conditions, namely, an FI flow rate of 2.0 mL min{sup −1} and an eluent comprised of 10% thiourea in 0.2 mol L{sup −1} HNO{sub 3}. The detection limit of FI–SCGD-AES was determined to be 0.75 μg L{sup −1}, and the precision of the 11 replicate Hg{sup 2+} measurements was 0.86% at a concentration of 100 μg L{sup −1}. The proposed method was validated by determining Hg{sup 2+} in certified reference materials such as human hair (GBW09101b) and stream sediment (GBW07310)

  9. Method of making ionic liquid mediated sol-gel sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Malik, Abdul; Shearrow, Anne M.

    2017-01-31

    Ionic liquid (IL)-mediated sol-gel hybrid organic-inorganic materials present enormous potential for effective use in analytical microextraction. One obstacle to materializing this prospect arises from high viscosity of ILs significantly slowing down sol-gel reactions. A method was developed which provides phosphonium-based, pyridinium-based, and imidazolium-based IL-mediated advanced sol-gel organic-inorganic hybrid materials for capillary microextraction. Scanning electron microscopy results demonstrate that ILs can serve as porogenic agents in sol-gel reactions. IL-mediated sol-gel coatings prepared with silanol-terminated polymers provided up to 28 times higher extractions compared to analogous sol-gel coatings prepared without any IL in the sol solution. This study shows that IL-generated porous morphology alone is not enough to provide effective extraction media: careful choice of the organic polymer and the precursor with close sol-gel reactivity must be made to ensure effective chemical bonding of the organic polymer to the created sol-gel material to be able to provide the desired sorbent characteristics.

  10. CARBONIZED FIBROUS RESIN AS A NEW SORBENT FOR SAMPLING POLYCYCLIC AROMATIC HYDROCARBONS (PAHS) IN AMBIENT AIR

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    A new sampling method of ambient air analysis using carbonized fibrous resin as asorbent for polycyclic aromatic hydrocarbons (PAHs) was reported.The physical and chemical properties of the carbonized fibrous resins were measured. Thesample pretreatment with ultrasonic extraction and subsequent clean-up ehition through a silica gelcolumn was optimized. The suitable ultrasonic extraction conditions were selected as follows: resinweight was 1.5 g, ultrasonic extraction time 20 min, volume of extraction solvent 100 mi andextraction operation times 2~3. The concentrated extractable organic matter was submitted to nextstep of clean-up procedure of adsorption chromatography on silica gel column/n-hexane and amixture of dichloromethene:n-hexane solution 2:3 (v/v). The PAHs fractions in the real samplesfrom Changzhou, China were particularly analyzed using GC-MS data system and the data of massspectra, retention times and scan numbers of the real samples were compared with that of thestandards of 16 PAHs listed by the US EPA as "priority pollutants" of the environment. Theanalysis of the real samples indicates that the carbonized fibrous resin is a good sorbent. Thepretreatment of samples of ambient air with carbonized fibrous resin as a sorbent for P,AHs isproved to be reliable and might be used for the procedure of the determination of PAHs inatmospheric environment.

  11. On-line generalized Steiner problem

    Energy Technology Data Exchange (ETDEWEB)

    Awerbuch, B.; Azar, Y.; Bartal, Y. [Tel Aviv Univ. (Israel)

    1996-12-31

    The Generalized Steiner Problem (GSP) is defined as follows. We are given a graph with non-negative weights and a set of pairs of vertices. The algorithm has to construct minimum weight subgraph such that the two nodes of each pair are connected by a path. We consider the on-line generalized Steiner problem, in which pairs of vertices arrive on-line and are needed to be connected immediately. We give a simple O(log{sup 2} n) competitive deterministic on-line algorithm. The previous best online algorithm (by Westbrook and Yan) was O({radical}n log n) competitive. We also consider the network connectivity leasing problem which is a generalization of the GSP. Here edges of the graph can be either bought or leased for different costs. We provide simple randomized O(log{sup 2} n) competitive algorithm based on the on-line generalized Steiner problem result.

  12. The war against on-line piracy

    OpenAIRE

    Harris, Julian

    2011-01-01

    A summary by Julian Harris, Deputy General Editor Amicus Curiae, of US attempts to control what it identifies as rogue Internet sites engaged in on-line piracy and opposition to such legislative moves.

  13. Development of Sorbents for Extraction and Stabilization of Nucleic Acids

    Science.gov (United States)

    2016-09-13

    groups [86]. Methods used to displace these interactions, as well as those used to displace RNA from negatively charged membranes [87], were...Detection of mRNA by RT-PCR from Preserved Prokaryotic Samples,” FEMS Microbiology Letters 201, 127–132 (2001). 25. S.D. Blacksell, S. Khounsy, and H.A...53. I.I. Slowing, B.G. Trewyn, and V.S.Y. Lin, “Mesoporous Silica Nanoparticles for Intracellular Delivery of Membrane -Impermeable Proteins

  14. Development of Sorbents for Extraction and Stabilization of Nucleic Acids

    Science.gov (United States)

    2016-09-13

    Supported Lipid Bilayers,” ACS Nano 6, 2174–2188 (2012). 61. Z. Li, J.C. Barnes, A. Bosoy, J.F. Stoddart, and J.I. Zink, “Mesoporous Silica Nanoparticles in...2013. 76. J. Kobler, K. Möller, and T. Bein, “Colloidal Suspensions of Functionalized Mesoporous Silica Nanoparticles,” ACS Nano 2, 791–799 (2008

  15. New high-capacity, calcium-based sorbents, calcium silicate sorbents. Final report, 1993--August 31, 1994

    Energy Technology Data Exchange (ETDEWEB)

    Kenney, M.C.; Chiang, R.K.; Fillgrove, K.L. [Case Western Reserve Univ., Cleveland, OH (United States)

    1995-02-01

    A search is being carried out for new calcium-based S0{sub 2} sorbents for induct injection. More specifically, a search is being carried out for induct injection calcium silicate sorbents that are highly cost effective. The objectives for the current year include the study of sorbents made from Ca(OH){sub 2}, from mixtures of Ca(OH){sub 2} and SiO{sub 2}, and from portland cement. They also include the study of sorbents made from model compounds. During this year, sorbents prepared from Ca(OH){sub 2} and from mixtures of Ca(OH){sub 2} and fumed SiO{sub 2} were investigated. The results show that very good SiO{sub 2}-modified Ca(OH){sub 2} sorbents in which the Si-to-Ca reactant ratio is low can be prepared from Ca(OH){sub 2} and fumed SiO{sub 2}. Sorbents prepared from Ca(OH){sub 2} and natural SiO{sub 2} or natural SiO{sub 2} sources were also studied. The results obtained show that very good SiO{sub 2}-modified Ca(OH){sub 2} sorbents and calcium silicate hydrate sorbents, C-S-H sorbents, can be prepared from Ca(OH){sub 2} and diatomite, pumice or perlite, minerals that are readily available. In addition. sorbents prepared from Ca{sub 3}SiO{sub 5} and {beta}-Ca{sub 2}SiO{sub 4} and from mixtures of these compounds and SiO{sub 2} were studied. The results secured demonstrate that very good C-S-H rich sorbents can be prepared from these compounds and from mixtures of them with SiO{sub 2}. They also provide information useful for interpreting the cement sorbent results. Sorbents prepared from cement and from mixtures of cement and natural SiO{sub 2} or SiO{sub 2} sources were investigated as well. The results secured show that cement and mixtures of it with diatomite, pumice or perlite rapidly yield excellent sorbents with the proper reaction conditions.

  16. On-Line Acquisitions by LOLITA

    Directory of Open Access Journals (Sweden)

    Frances G. Spigai

    1970-12-01

    Full Text Available The on-line acquisition program (LOLITA in use at the Oregon State University Library is described in terms of development costs, equipment requirements, and overall design philosophy. In particular, the record format and content of records in the on-order file, and the on-line processing of these records (input, search, correction, output using a cathode ray tube display terminal are detailed.

  17. ACSEPP On-Line Electronic Payment Protocol

    Institute of Scientific and Technical Information of China (English)

    WANG Shao-bin; ZHU Xian; HONG Fan

    2004-01-01

    With analyzing the existing on-line electronic payment protocols, this paper presents a new on-line electronic payment protocol named ACSEPP: Anonymous, Convenient and Secure Electronic Payment Protocol.Its aim is to design a practical electronic payment protocol which is both secure and convenient.Without using PKI_CA frame, it realized the anonymity of consumer and merchant, the convenient of handling, the low cost of maintenance and the security.

  18. Highly attrition resistant sorbents for desulfurization of hot coal gases

    Energy Technology Data Exchange (ETDEWEB)

    Slimane, R.B.; Abbasian, J.; Zarnegar, M.K. [Institute of Gas Technology, Des Plaines, IL (United States)] [and others

    1998-04-01

    One of the main obstacles in the commercialization of high-temperature desulfurization systems for Integrated Gasification Combined Cycle (IGCC) power generation processes is the development of regenerable sulfur sorbents with suitable physical and chemical characteristics. The focus of much of the current research on sorbent development has been on the use of zinc-based sorbents. These sorbents have been the subject of extensive pilot-scale and process development work; however, they have been shown to suffer from sulfate formation and zinc volatilization, leading to sorbent degradation over multi-cycle use. Therefore, investigation of non-zinc based sorbents is a logical approach to develop an effective alternative. An effective alternative to zinc-based sorbents could be manganese-based sorbents which have recently been shown to withstand high temperature ({ge} 750{degrees}C) operation and also maintain structural and reactive integrity over many cycles. However, because of process equipment limitations and other process variables such as fuel gas alkali content, a number of investigators have recently argued that the benefit to be gained by lower temperature application may outweigh the slight loss of efficiency, resulting in lower overall cost of electricity. Desulfurization temperatures {le} 538{degrees}C have been recommended to provide the best compromise between process equipment limitations and higher temperature operation.

  19. Development of advanced sorbents for hot gas desulfurization

    Energy Technology Data Exchange (ETDEWEB)

    Abbasian, J.; Slimane, R.B.; Wangerow, J.R. [Inst. of Gas Technology, Des Plaines, IL (United States); Cicero, D.C. [Dept. of Energy, Morgantown, WV (United States). Morgantown Energy Technology Center

    1996-12-31

    Integrated Gasification Combined-Cycle (IGCC) processes are among the leading contenders for the production of electricity from coal. Coal gas desulfurization to sufficiently low levels at elevated temperatures (T > 350 C) is now recognized as crucial to efficient and economic coal utilization in advanced IGCC processes. The implementation of hot coal gas desulfurization relies heavily on the development of regenerable sorbent materials which can efficiently reduce H{sub 2}S from several thousand ppmv levels down to a few ppmv over many cycles of sulfidation/regeneration. Zinc-based sorbents, such as zinc titanate, are currently the leading candidate sorbents, however, they have been shown to suffer from zinc volatilization at elevated temperatures leading to sorbent deterioration, increasing sorbent replacement costs, and the overall cost of hot gas cleanup. This paper discusses the results obtained in an ongoing investigation geared towards developing advanced mixed-metal oxide sorbents for desulfurization of coal-derived fuel gases in the temperature range of 350 to 550 C. The paper focuses on the study related to the development of durable sorbents and addresses thermodynamic considerations, sulfidation kinetics, regenerability, and long term durability of a number of novel sorbents.

  20. Development of advanced hot-gas desulfurization sorbents. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Jothimurugesan, K.; Adeyiga, A.A.; Gangwal, S.K.

    1997-10-01

    The objective of this project was to develop hot-gas desulfurization sorbent formulations for relatively lower temperature application, with emphasis on the temperature range from 343--538 C. The candidate sorbents include highly dispersed mixed metal oxides of zinc, iron, copper, cobalt, nickel and molybdenum. The specific objective was to develop suitable sorbents, that would have high and stable surface area and are sufficiently reactive and regenerable at the relatively lower temperatures of interest in this work. Stability of surface area during regeneration was achieved by adding stabilizers. To prevent sulfation, catalyst additives that promote the light-off of the regeneration reaction at lower temperature was considered. Another objective of this study was to develop attrition-resistant advanced hot-gas desulfurization sorbents which show stable and high sulfidation reactivity at 343 to 538 C and regenerability at lower temperatures than leading first generation sorbents.

  1. Monitoring solid oxide CO2 capture sorbents in action.

    Science.gov (United States)

    Keturakis, Christopher J; Ni, Fan; Spicer, Michelle; Beaver, Michael G; Caram, Hugo S; Wachs, Israel E

    2014-12-01

    The separation, capture, and storage of CO2 , the major greenhouse gas, from industrial gas streams has received considerable attention in recent years because of concerns about environmental effects of increasing CO2 concentration in the atmosphere. An emerging area of research utilizes reversible CO2 sorbents to increase conversion and rate of forward reactions for equilibrium-controlled reactions (sorption-enhanced reactions). Little fundamental information, however, is known about the nature of the sorbent surface sites, sorbent surface-CO2 complexes, and the CO2 adsorption/desorption mechanisms. The present study directly spectroscopically monitors Na2 O/Al2 O3 sorbent-CO2 surface complexes during adsorption/desorption with simultaneous analysis of desorbed CO2 gas, allowing establishment of molecular level structure-sorption relationships between individual surface carbonate complexes and the CO2 working capacity of sorbents at different temperatures.

  2. CARBON DIOXIDE CAPTURE FROM FLUE GAS USING DRY REGENERABLE SORBENTS

    Energy Technology Data Exchange (ETDEWEB)

    David A. Green; Thomas Nelson; Brian S. Turk; Paul Box; Weijiong Li; Raghubir P. Gupta

    2005-07-01

    This report describes research conducted between April 1, 2005 and June 30, 2005 on the use of dry regenerable sorbents for removal of carbon dioxide from flue gas from coal combustion and synthesis gas from coal gasification. Supported sodium carbonate sorbents removed up to 76% of the carbon dioxide from simulated flue gas in a downflow cocurrent flow reactor system, with an approximate 15 second gas-solid contact time. This reaction proceeds at temperatures as low as 25 C. Lithium silicate sorbents remove carbon dioxide from high temperature simulated flue gas and simulated synthesis gas. Both sorbent types can be thermally regenerated and reused. The lithium silicate sorbent was tested in a thermogravimetric analyzer and in a 1-in quartz reactor at atmospheric pressure; tests were also conducted at elevated pressure in a 2-in diameter high temperature high pressure reactor system. The lithium sorbent reacts rapidly with carbon dioxide in flue gas at 350-500 C to absorb about 10% of the sorbent weight, then continues to react at a lower rate. The sorbent can be essentially completely regenerated at temperatures above 600 C and reused. In atmospheric pressure tests with synthesis gas of 10% initial carbon dioxide content, the sorbent removed over 90% of the carbon dioxide. An economic analysis of a downflow absorption process for removal of carbon dioxide from flue gas with a supported sodium carbonate sorbent suggests that a 90% efficient carbon dioxide capture system installed at a 500 MW{sub e} generating plant would have an incremental capital cost of $35 million ($91/kWe, assuming 20 percent for contingencies) and an operating cost of $0.0046/kWh. Assuming capital costs of $1,000/kW for a 500 MWe plant the capital cost of the down flow absorption process represents a less than 10% increase, thus meeting DOE goals as set forth in its Carbon Sequestration Technology Roadmap and Program Plan.

  3. Dimensional Description of On-line Wear Debris Images for Wear Characterization

    Institute of Scientific and Technical Information of China (English)

    WU Tonghai; PENG Yeping; DU Ying; WANG Junqun

    2014-01-01

    As one of the most wear monitoring indicator, dimensional feature of individual particles has been studied mostly focusing on off-line analytical ferrograph. Recent development in on-line wear monitoring with wear debris images shows that merely wear debris concentration has been extracted from on-line ferrograph images. It remains a bottleneck of obtaining the dimension of on-line particles due to the low resolution, high contamination and particle’s chain pattern of an on-line image sample. In this work, statistical dimension of wear debris in on-line ferrograph images is investigated. A two-step procedure is proposed as follows. First, an on-line ferrograph image is decomposed into four component images with different frequencies. By doing this, the size of each component image is reduced by one fourth, which will increase the efficiency of subsequent processing. The low-frequency image is used for extracting the area of wear debris, and the high-frequency image is adopted for extracting contour. Second, a statistical equivalent circle dimension is constructed by equaling the overall wear debris in the image into equivalent circles referring to the extracted total area and premeter of overall wear debris. The equivalent circle dimension, reflecting the statistical dimension of larger wear debris in an on-line image, is verified by manual measurement. Consequently, two preliminary applications are carried out in gasoline engine bench tests of durability and running-in. Evidently, the equivalent circle dimension, together with the previously developed concentration index, index of particle coverage area (IPCA), show good performances in characterizing engine wear conditions. The proposed dimensional indicator provides a new statistical feature of on-line wear particles for on-line wear monitoring. The new dimensional feature conveys profound information about wear severity.

  4. Highly attrition resistant sorbents for desulfurization of hot coal gases

    Energy Technology Data Exchange (ETDEWEB)

    Slimane, R.B.; Abbasian, J.; Zarnegar, M.K.; Wangerow, J.R.; Carty, R.H.

    1998-07-01

    One of the main obstacles in the commercialization of high-temperature desulfurization systems for Integrated Gasification Combined Cycle (IGCC) power generation processes is the development of regenerable sulfur sorbents with suitable physical and chemical characteristics. The focus of much of the current research on sorbent development has been on the use of zinc-based sorbents. These sorbents have been the subject of extensive pilot-scale and process development work; however, they have been shown to suffer from sulfate formation and zinc volatilization, leading to sorbent degradation over multi-cycle use. Therefore, investigation of non-zinc based sorbents is a logical approach to develop an effective alternative. An effective alternative to zinc-based sorbents could be manganese-based sorbents which have recently been shown to withstand high temperature ({gt} 750 C) operation and also maintain structural and reactive integrity over many cycles. However, because of process equipment limitations and other process variables such as fuel gas alkali content, a number of investigators have recently argued that the benefit to be gained by lower temperature application may outweigh the slight loss of efficiency, resulting in lower overall cost of electricity. Desulfurization temperatures {lt} 538 C have been recommended to provide the best compromise between process equipment limitations and higher temperature operation. This paper reports on an on-going research program to develop novel, highly reactive, attrition-resistant, and regenerable manganese-based sorbents for the removal of hydrogen sulfide (H{sub 2}S) from coal-derived fuel gases at temperatures of 316 to 538 C and pressures up to 300 psig. The primary focus of this study is placed on the preparation (method and composition), characterization, and evaluation of a number of sorbent formulations to identify the most suitable manganese-based sorbent. The manganese-based sorbent formulations prepared to

  5. Formación on line

    Directory of Open Access Journals (Sweden)

    O. Grau-Perejoan

    Full Text Available La formación on line es una modalidad de enseñanza a distancia basada en las nuevas tecnologías. En este artículo se pretende hacer una introducción a base de describir a grandes rasgos sus características principales: asincronía, no presencialidad, comunicación escrita, función del profesor on line, así como los retos, los riesgos, las ventajas y los inconvenientes que plantea. Se exponen las diferencias entre la formación on line y la formación presencial, de manera que los docentes puedan adaptar de la mejor manera posible sus propuestas formativas a la modalidad on line. Se introduce el importantísimo papel de la planificación y de la fase de diseño y, finalmente, se repasan conceptos útiles para comprender mejor el mundo de la formación on line como son los conceptos entorno virtual de aprendizaje (EVA o Blended Learning (B-Learning.

  6. Efficient Theoretical Screening of Solid Sorbents for CO2 Capture Applications*

    Energy Technology Data Exchange (ETDEWEB)

    Duan, Yuhua; Luebke, David; Pennline, Henry

    2012-03-31

    By combining thermodynamic database mining with first principles density functional theory and phonon lattice dynamics calculations, a theoretical screening methodology to identify the most promising CO2 sorbent candidates from the vast array of possible solid materials has been proposed and validated. The ab initio thermodynamic technique has the advantage of allowing identification of thermodynamic properties of CO2 capture reactions without any experimental input beyond crystallographic structural information of the solid phases involved. For a given solid, the first step is to attempt to extract thermodynamic properties from thermodynamic databases and the available literatures. If the thermodynamic properties of the compound of interest are unknown, an ab initio thermodynamic approach is used to calculate them. These properties expressed conveniently as chemical potentials and heat of reactions, which obtained either from databases or from calculations, are further used for computing the thermodynamic reaction equilibrium properties of the CO2 absorption/desorption cycles. Only those solid materials for which lower capture energy costs are predicted at the desired process conditions are selected as CO2 sorbent candidates and are further considered for experimental validations. Solid sorbents containing alkali and alkaline earth metals have been reported in several previous studies to be good candidates for CO2 sorbent applications due to their high CO2 absorption capacity at moderate working temperatures. In addition to introducing our computational screening procedure, in this presentation we will summarize our results for solid systems composed by alkali and alkaline earth metal oxides, hydroxides, and carbon- ates/bicarbonates to validate our methodology. Additionally, applications of our computational method to mixed solid systems of Li2O with SiO2/ZrO2 with different mixing ratios, our preliminary results showed that increasing the Li2O/SiO2 ratio in

  7. A generalized theory of chromatography and multistep liquid extraction

    Science.gov (United States)

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

    2017-03-01

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

  8. Sorbent-based Oxygen Production for Energy Systems

    Energy Technology Data Exchange (ETDEWEB)

    Sethi, Vijay [Western Research Inst. (WRI), Laramie, WY (United States)

    2017-01-31

    Project DE-FE0024075 deals with the development of a moderate-temperature sorbent-based oxygen production technology. Sorbent-based oxygen production process utilizes oxygen-storage properties of Perovskites to (1) adsorb oxygen from air in a solid sorbent, and (2) release the adsorbed oxygen into a sweep gas such as CO2 and/or steam for gasification systems or recycled flue gas for oxy-combustion systems. Pure oxygen can be produced by the use of vacuum instead of a sweep gas to affect the pressure swing. By developing more efficient and stable, higher sorption capacity, newer class of materials operating at moderate temperatures this process represents a major advancement in air separation technology. Newly developed perovskite ceramic sorbent materials with order-disorder transition have a higher O2 adsorption capacity, potentially 200 °C lower operating temperatures, and up to two orders of magnitude faster desorption rates than those used in earlier development efforts. The performance advancements afforded by the new materials lead to substantial savings in capital investment and operational costs. Cost of producing oxygen using sorbents could be as much as 26% lower than VPSA and about 13% lower than a large cryogenic air separation unit. Cost advantage against large cryogenic separation is limited because sorbent-based separation numbers up sorbent modules for achieving the larger capacity.

  9. On line routing per mobile phone

    DEFF Research Database (Denmark)

    Bieding, Thomas; Görtz, Simon; Klose, Andreas

    2009-01-01

    . Additionally it is of utmost importance that the employed communication system is suitable integrated with the firm’s enterprise application system and business processes. On basis of a case study, we describe in this paper a system that is cheap and easy to implement due to the use of simple mobile phones......On-line routing is concerned with building vehicle routes in an ongoing fashion in such a way that customer requests arriving dynamically in time are efficiently and effectively served. An indispensable prerequisite for applying on-line routing methods is mobile communication technology...

  10. Educational On-Line Gaming Propensity

    DEFF Research Database (Denmark)

    Sudzina, Frantisek; Razmerita, Liana; Kirchner, Kathrin

    2014-01-01

    Educational on-line games are promising for new generations of students who are grown up digital. Th e new generations of students are technology savvy and spend lots of time on the web and on social networks. Based on an exploratory study, this article investigates the factors that infl uence...... students’ willingness to participate in serious games for teaching/learning. Th is study investigates the relationship between students’ behavior on Facebook, Facebook games, and their attitude toward educational on-line games. Th e results of the study reveal that the early adopters of educational games...

  11. Enhanced durability and reactivity for zinc ferrite desulfurization sorbent

    Energy Technology Data Exchange (ETDEWEB)

    Berggren, M.H.; Jha, M.C.

    1989-10-01

    AMAX Research Development Center (AMAX R D) investigated methods for enhancing the reactivity and durability of zinc ferrite desulfurization sorbents. Zinc ferrite sorbents are intended for use in desulfurization of hot coal gas in integrated gasification combined cycle (IGCC) or molten carbonate fuel cell (MCFC) applications. For this program, the reactivity of the sorbent may be defined as its sulfur sorption capacity at the breakthrough point and at saturation in a bench-scale, fixed-bed reactor. Durability may be defined as the ability of the sorbent to maintain important physical characteristics such as size, strength, and specific surface area during 10 cycles of sulfidation and oxidation. Two base case sorbents, a spherical pellet and a cylindrical extrude used in related METC-sponsored projects, were used to provide a basis for the aimed enhancement in durability and reactivity. Sorbent performance was judged on the basis of physical properties, single particle kinetic studies based on thermogravimetric (TGA) techniques, and multicycle bench-scale testing of sorbents. A sorbent grading system was utilized to quantify the characteristics of the new sorbents prepared during the program. Significant enhancements in both reactivity and durability were achieved for the spherical pellet shape over the base case formulation. Overall improvements to reactivity and durability were also made to the cylindrical extrude shape. The primary variables which were investigated during the program included iron oxide type, zinc oxide:iron oxide ratio, inorganic binder concentration, organic binder concentration, and induration conditions. The effects of some variables were small or inconclusive. Based on TGA studies and bench-scale tests, induration conditions were found to be very significant.

  12. Efficient separations and processing crosscutting program: Develop and test sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Bray, L.A.

    1995-09-01

    This report summarizes work performed during FY 1995 under the task {open_quotes}Develop and Test Sorbents,{close_quotes} the purpose of which is to develop high-capacity, selective solid extractants to recover cesium, strontium, and technetium from nuclear wastes. This work is being done for the Efficient Separations and Processing Crosscutting Program (ESP), operated by the U.S. Department of Energy`s Office of Environmental Management`s Office of Technology Development. The task is under the direction of staff at Pacific Northwest Laboratory (PNL) with key participation from industrial and university staff at 3M, St. Paul, Minnesota; IBC Advanced Technologies, Inc., American Forks, Utah; AlliedSignal, Inc., Des Plaines, Illinois, and Texas A&M University, College Station, Texas. 3M and IBC are responsible for ligand and membrane technology development; AlliedSignal and Texas A&M are developing sodium titanate powders; and PNL is testing the materials developed by the industry/university team members. Major accomplishments for FY 1995 are summarized in this report.

  13. Molecularly imprinted sol-gel nanofibers based solid phase microextraction coupled on-line with high performance liquid chromatography for selective determination of acesulfame.

    Science.gov (United States)

    Moein, Mohammad Mahdi; Javanbakht, Mehran; Karimi, Mohammad; Akbari-adergani, Behrouz

    2015-03-01

    Sol-gel based molecularly imprinted polymer (MIP) nanofiber was successfully fabricated by electrospinning technique on the surface of a stainless steel bar. The manufactured tool was applied for on-line selective solid phase microextraction (SPME) and determination of acesulfame (ACF) as an artificial sweetener with high performance liquid chromatography (HPLC). The selective ability of method for the extraction of ACF was investigated in the presence of some selected sweeteners such as saccharine (SCH), aspartame (ASP) and caffeine (CAF). Electrospinning of MIP sol-gel solution on the stainless steel bar provided an unbreakable sorbent with high thermal, mechanical, and chemical stability. Moreover, application of the MIP-SPME tool revealed a unique approach for the selective microextraction of the analyte in beverage samples. In this work, 3-(triethoxysilyl)-propylamine (TMSPA) was chosen as a precursor due to its ability to imprint the analyte by hydrogen bonding, Van der Walls, and dipole-dipole interactions. Nylon 6 was also added as a backbone and support for the precursor in which sol could greatly growth during the sol-gel process and makes the solution electrospinable. Various effective parameters in the extraction efficiency of the MIP-SPME tool such as loading time, flow rate, desorption time, selectivity, and the sample volume were evaluated. The linearity for the ACF in beverage sample was in the range of 0.78-100.5 ng mL(-1). Limit of detection (LOD) and quantification (LOQ) were 0.23 and 0.78 ng mL(-1) respectively. The RSD values (n=5) were all below 3.5%at the 20 ng mL(-1) level.

  14. ON-LINE DOCUMENTS CONTENT MANAGEMENT

    Directory of Open Access Journals (Sweden)

    VASILESCU RAMONA VIOLETA

    2010-05-01

    Full Text Available This paper outlines the steps and technologies used in developing an on-line application server with many desktop clients, and with high power processing for a wide range of input documents to obtain searchable documents on the highest portability standards, PDF and PDF /A.

  15. 流动注射在线萃取法测定饮用水中阴离子合成洗涤剂%Flow injection on-line extraction method for the determination of anionic synthetic detergent in drinking water

    Institute of Scientific and Technical Information of China (English)

    郑丽红

    2015-01-01

    Objective To discuss the use of flow injection on-line extraction method for testing the concentration of an-ionic synthetic detergent in drinking water. Methods Based on the principle that component of anionic synthetic deter-gent could form ion pair complexes with alkaline methylene blue, flow injection analysis instrument (QC8500) was used to test the concentration of anionic synthetic detergent in water. The method's detection limit, precision and accuracy were examined firstly, then the concentration in samples were tested, and lastly compared the result with that of nation-al standard method. Results The linear range of standard curve was 0.025-1.00 mg/L (r=0.9996), relative standard de-viation was 2.04%-4.35%, the detection limit was 5.2 μg/L, and the labeled recovery rate was 95.5%-105.3%. Con-clusion Flow injection on-line extraction method is simple, rapid, stable, accurate and sensitive, which is suitable for the determination of anionic synthetic detergent in drinking water.%目的:探讨使用流动注射在线萃取法测定饮用水中阴离子合成洗涤剂含量的方法。方法利用阴离子合成洗涤剂中的主要成分可与碱性亚甲基蓝形成离子对络合物的原理,采用QC8500型流动注射仪对水中阴离子合成洗涤剂含量进行定量分析。本研究分别对方法的检出限、精确度、准确度进行了测定,并对饮用水样品进行检测,最后将检测结果与国家标准方法所得结果进行了比较。结果方法线性范围为0.025~1.00 mg/L,相关系数r值为0.9996,相对标准偏差为2.04%~4.35%,最低检出限为5.2μg/L,回收率为95.5%~105.3%。结论使用流动注射在线萃取法测定饮用水中阴离子合成洗涤剂,方便、快捷、稳定、准确、灵敏度高,符合阴离子合成洗涤剂的检测要求。

  16. Sorbents based on xerogels of zirconium, aluminum and manganese oxyhydroxides

    National Research Council Canada - National Science Library

    R.V. Smotraiev; E.O. Sorochkina; А.V. Dzuba; Y.D. Galivets

    2016-01-01

    ...: The aim of this work is to determine the impact of aluminum and manganese ions additives on surface and sorption properties of zirconium oxyhydroxide based sorbents during their production process...

  17. Novel Sorbent to Clean Up Biogas for CHPs

    Energy Technology Data Exchange (ETDEWEB)

    Alptekin, Gökhan O. [TDA Research, Incorporated, Wheat Ridge, CO (United States); Jayataman, Ambalavanan [TDA Research, Incorporated, Wheat Ridge, CO (United States); Schaefer, Matthew [TDA Research, Incorporated, Wheat Ridge, CO (United States); Ware, Michael [TDA Research, Incorporated, Wheat Ridge, CO (United States); Hunt, Jennifer [FuelCell Energy, Inc., Danbury, CT (United States); Dobek, Frank [FuelCell Energy, Inc., Danbury, CT (United States)

    2015-05-30

    In this project, TDA Research Inc. (TDA) has developed low-cost (on a per unit volume of gas processed basis), high-capacity expendable sorbents that can remove both the H2S and organic sulfur species in biogas to the ppb levels. The proposed sorbents will operate downstream of a bulk desulfurization system as a polishing bed to provide an essentially sulfur-free gas to a fuel cell (or any other application that needs a completely sulfur-free feed). Our sorbents use a highly dispersed mixed metal oxides active phase with desired modifiers prepared over on a mesoporous support. The support structure allows the large organic sulfur compounds (such as the diethyl sulfide and dipropyl sulfide phases with a large kinetic diameter) to enter the sorbent pores so that they can be adsorbed and removed from the gas stream.

  18. Oil sorbents from plastic wastes and polymers: A review.

    Science.gov (United States)

    Saleem, Junaid; Adil Riaz, Muhammad; Gordon, McKay

    2018-01-05

    A large volume of the waste produced across the world is composed of polymers from plastic wastes such as polyethylene (HDPE or LDPE), polypropylene (PP), and polyethylene terephthalate (PET) amongst others. For years, environmentalists have been looking for various ways to overcome the problems of such large quantities of plastic wastes being disposed of into landfill sites. On the other hand, the usage of synthetic polymers as oil sorbents in particular, polyolefins, including polypropylene (PP) and polyethylene (PE) have been reported. In recent years, the idea of using plastic wastes as the feed for the production of oil sorbents has gained momentum. However, the studies undertaking such feasibility are rather scattered. This review paper is the first of its kind reporting, compiling and reviewing these various processes. The production of an oil sorbent from plastic wastes is being seen to be satisfactorily achievable through a variety of methods Nevertheless, much work needs to be done regarding further investigation of the numerous parameters influencing production yields and sorbent qualities. For example, differences in results are seen due to varying operating conditions, experimental setups, and virgin or waste plastics being used as feeds. The field of producing oil sorbents from plastic wastes is still very open for further research, and seems to be a promising route for both waste reduction, and the synthesis of value-added products such as oil sorbents. In this review, the research related to the production of various oil sorbents based on plastics (plastic waste and virgin polymer) has been discussed. Further oil sorbent efficiency in terms of oil sorption capacity has been described. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Hot coal gas desulfurization with manganese-based sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Lynch, D.; Hepworth, M.T.

    1993-09-01

    The focus of work being performed on Hot Coal Gas Desulfurization is primarily in the use of zinc ferrite and zinc titanate sorbents; however, prior studies at the US Steel Fundamental Research Laboratories in Monroeville, PA, by E.T. Turkdogan indicated that an alternate sorbent, manganese dioxide-containing ore in mixture with alumina (75 wt % ore + 25 wt % Al{sub 2}/O{sub 3}) may be a viable alternative to zinc-based sorbents. Manganese, for example, has a lower vapor pressure in the elemental state than zinc hence it is not as likely to undergo depletion from the sorbent surface upon loading and regeneration cycles. Also manganese oxide is less readily reduced to the elemental state than iron hence the range of reduction potentials for oxygen is somewhat greater than for zinc ferrite. In addition, thermodynamic analysis of the manganese-oxygen-sulfur system shows it to be less amenable to sulfation than zinc ferrite. Potential also exists for utilization of manganese higher temperatures than zinc ferrite or zinc titanate. This presentation gives the thermodynamic background for consideration of manganese-based sorbents as an alternative to zinc ferrite. To date the work which has been in progress for nine months is limited at this stage to thermogravimetric testing of four formulations of manganese-alumina sorbents to determine the optimum conditions of pelletization and induration to produce reactive pellets.

  20. Educational On-Line Gaming Propensity

    DEFF Research Database (Denmark)

    Sudzina, Frantisek; Razmerita, Liana; Kirchner, Kathrin

    2014-01-01

    Educational on-line games are promising for new generations of students who are grown up digital. Th e new generations of students are technology savvy and spend lots of time on the web and on social networks. Based on an exploratory study, this article investigates the factors that infl uence...... students’ willingness to participate in serious games for teaching/learning. Th is study investigates the relationship between students’ behavior on Facebook, Facebook games, and their attitude toward educational on-line games. Th e results of the study reveal that the early adopters of educational games...... are likely to be students, who are young, have only a few Facebook connections, who currently play Facebook game(s). Furthermore, the study emphasizes that there may be differences between students coming from various countries....

  1. New Trends in on-line Marketing

    OpenAIRE

    Palkovič, Lukáš

    2011-01-01

    This bachelor thesis deals with new trend of internet marketing, it focuses especially on viral marketing. The theoretical part charasterizes the process of viral campaigns, furthermore deals with the components and aspects of on-line environment. Another separated chapter presents social networks, their place in viral marketing and at last but not least the viral video making process. The practical part contains different analyses of specific viral campaigns. The next and equally the last pa...

  2. Connecting to On-line Data

    Science.gov (United States)

    Eichhorn, G.; Astrophysics Datacenter Executive Committee (ADEC)

    2004-05-01

    The Astrophysics Datacenter Executive Committee (ADEC) is coordinating the development of a system to facilitate the linking to on-line data. This system has three components: 1. Unique dataset identifiers. 2. A verification system for identifiers. 3. Permanent links to on-line data sets. 1. The ADEC has agreed on a naming scheme for data sets that allows for the unique identification of any data set. The ADEC data centers will clearly mark their data with these identifiers to allow the generation of links to these data. 2. Each data center has a utility that can check whether a data set identifier is a valid identifier at that center. A central verifier allows third parties access to these individual verifiers through a single portal. 3. The central verifier also provides permanent links to data sets through a central link forwarding system. This makes it possible to move data sets between data centers while maintaining the permanent links. The ADEC plans to first use this system to implement the linking from the literature to on-line data in a collaboration with the AAS and the University of Chicago Press for the AAS journals.

  3. New Sorbents for Removing Arsenic From Water

    Science.gov (United States)

    McConchie, D. M.; Genc-Fuhrman, H.; Clark, M. W.; Caldicott, W.; Davies-McConchie, F. G.

    2004-12-01

    Elevated concentrations of arsenic in the drinking water used in many countries, including some of the poorest developing countries, and recognition that consuming this water can have serious consequences for human health, have led to increased investigations of ways to obtain safe water supplies. Finding new groundwater resources is a possible solution but this is a costly strategy that has no guarantee of success, particularly in areas where water is already a scarce commodity. The alternative is to treat water that is already available, but existing technologies are usually too expensive, too difficult to operate and maintain, or not completely effective when used in less developed countries or remote areas. There is therefore, an urgent need to find a simple and effective but inexpensive sorbent for arsenic that can be used to treat large volumes of water under less than ideal conditions. In this paper we present the results of field and laboratory trials that used a new, highly cost-effective, sorbent to remove arsenic from contaminated water. BauxsolT is the name given to the cocktail of minerals prepared by treating caustic bauxite refinery residues with Mg and Ca to produce a substance with a reaction pH of about 8.5, a high acid neutralizing capacity and an excellent ability to trap trace metals, metalloids and some other ionic species. The trapped ions are tightly bound by processes that include; precipitation of low solubility neoformational minerals, isomorphous substitution, solid-state diffusion, and adsorption; it is also an excellent flocculant. Although ordinary BauxsolT has an excellent ability to bind arsenate, and to a lesser extent arsenite, this ability can be further increased for particular water types by using activated BauxsolT or BauxsolT combined with small amounts of other reagents. Field trials conducted at the Gilt Edge Mine, South Dakota, showed that the addition of BauxsolT to highly sulfidic waste rock reduced the arsenic

  4. 羧基化多壁碳纳米管固相萃取-液相色谱-串联质谱法测定环境水体中四溴双酚A和双酚A%Determination of tetrabromobisphenol A and bisphenol A in environmental water using carboxylated multiwalled carbon nanotubes as sorbent for solid-phase extraction combined with liquid chromatography-tandem mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    寇立娟; 梁荣宁

    2014-01-01

    A method for the determination of tetrabromobisphenol A and bisphenol A in environ-mental water using carboxyl-functionalized multiwalled carbon nanotubes as solid-phase extraction sorbent and liquid chromatography-tandem mass spectrometry was established. Com-parison of three nanomaterials including multiwalled carbon nanotubes,C60 and carboxyl-func-tionalized multiwalled carbon nanotubes used as solid-phase extraction sorbents was made. After preconcentration by solid-phase extraction,tetrabromobisphenol A and bisphenol A were separa-ted on a Thermo Scientific Hypersil C18 column(150 mm×4. 6 mm,3 μm)and then detected by tandem mass spectrometry in negative electrospray ionization(ESI)mode. The results showed a good linear response in the concentration range of 0. 02-1. 0 mg / L for tetrabromobisphenol A and bisphenol A,and the limits of detection(S / N = 3)were 0. 04 μg / L and 0. 2 μg / L for tetrabromo-bisphenol A and bisphenol A,respectively. The application of the proposed approach has been carried out for the determination of tetrabromobisphenol A and bisphenol A in spiked lake water and sea water samples. The recoveries varied from 82% to 99% with the relative standard devia-tions below 5. 0%. The proposed method can be used for the determination of tetrabromobisphe-nol A and bisphenol A at trace level in complex environmental samples.%建立了羧基化碳纳米管固相萃取-液相色谱-串联质谱联用检测环境水体中四溴双酚 A 和双酚 A 的方法。比较了多壁碳纳米管、C60和羧基化多壁碳纳米管作为固相吸附剂对水体中四溴双酚 A 和双酚 A 的吸附效率。固相萃取浓缩后的样品经 Thermo Scientific Hypersil C18色谱柱(150 mm×4.6 mm,3μm)分离,采用串联质谱负离子模式进行检测。结果表明,四溴双酚 A 和双酚 A 在0.02~1.0 mg / L 范围内具有良好的线性关系( r2≥0.99),空白样品中的检出限(S / N =3)分别为0.04μg / L 和0.2μg / L。

  5. Evaluation of Sorbent Injection for Mercury Control

    Energy Technology Data Exchange (ETDEWEB)

    Sharon Sjostrom

    2006-04-30

    The power industry in the U.S. is faced with meeting new regulations to reduce the emissions of mercury compounds from coal-fired plants. These regulations are directed at the existing fleet of nearly 1,100 boilers. These plants are relatively old with an average age of over 40 years. Although most of these units are capable of operating for many additional years, there is a desire to minimize large capital expenditures because of the reduced (and unknown) remaining life of the plant to amortize the project. Injecting a sorbent such as powdered activated carbon into the flue gas represents one of the simplest and most mature approaches to controlling mercury emissions from coal-fired boilers. This is the final site report for tests conducted at DTE Energy's Monroe Power Plant, one of five sites evaluated in this DOE/NETL program. The overall objective of the test program was to evaluate the capabilities of activated carbon injection at five plants: Sunflower Electric's Holcomb Station Unit 1, AmerenUE's Meramec Station Unit 2, Missouri Basin Power Project's Laramie River Station Unit 3, Detroit Edison's Monroe Power Plant Unit 4, and AEP's Conesville Station Unit 6. These plants have configurations that together represent 78% of the existing coal-fired generation plants. The goals for the program established by DOE/NETL were to reduce the uncontrolled mercury emissions by 50 to 70% at a cost 25 to 50% lower than the target established by DOE of $60,000/lb mercury removed. The results from Monroe indicate that using DARCO{reg_sign} Hg would result in higher mercury removal (80%) at a sorbent cost of $18,000/lb mercury, or 70% lower than the benchmark. These results demonstrate that the goals established by DOE/NETL were exceeded during this test program. The increase in mercury removal over baseline conditions is defined for this program as a comparison in the outlet emissions measured using the Ontario Hydro method during the baseline

  6. Enhanced durability of desulfurization sorbents for fluidized-bed applications

    Energy Technology Data Exchange (ETDEWEB)

    Gupta, R.P.; Gangwal, S.K.

    1992-11-01

    To extend the operating temperature range and further improve the durability of fluidizable sorbents, zinc titanate, another leading regenerable sorbent, was selected for development in the later part of this project. A number of zinc titanate formulations were prepared in the 50 to 300 [mu]m range using granulation and spray drying methods. Important sorbent preparation variables investigated included zinc to titanium ratio, binder type, binder amount, and various chemical additives such as cobalt and molybdenum. A number of sorbents selected on the basis of screening tests were subjected to bench-scale testing for 10 cycles at high temperature, high pressure (HTHP) conditions using the reactor system designed and constructed during the base program. This reactor system is capable of operation either as a 2.0 in. or 3.0 in. I.D. bubbling bed and is rated up to 20 atm operation at 871[degrees]C. Bench-scale testing variables included sorbent type, temperature (550 to 750[degrees]C), gas type (KRW or Texaco gasifier gas), steam content of coal gas, and fluidizing gas velocity (6 to 15 cm/s). The sorbents prepared by spray drying showed poor performance in terms of attrition resistance and chemical reactivity. On the other hand, the granulation method proved to be very successful. For example, a highly attrition-resistant zinc titanate formulation, ZT-4, prepared by granulation exhibited virtually no zinc loss and demonstrated a constant high reactivity and sulfur capacity over 10 cycles, i.e., approximately a 60 percent capacity utilization, with Texaco gas at 750[degrees]C, 15 cm/s fluidizing velocity and 15 atm pressure. The commercial potential of the granulation method for zinc titanate manufacture was demonstrated by preparing two 80 lb batches of sorbent with zinc to titanium mol ratios of 0.8 and 1.5.

  7. Enhanced durability of desulfurization sorbents for fluidized-bed applications

    Energy Technology Data Exchange (ETDEWEB)

    Gupta, R.P.; Gangwal, S.K.

    1992-11-01

    To extend the operating temperature range and further improve the durability of fluidizable sorbents, zinc titanate, another leading regenerable sorbent, was selected for development in the later part of this project. A number of zinc titanate formulations were prepared in the 50 to 300 {mu}m range using granulation and spray drying methods. Important sorbent preparation variables investigated included zinc to titanium ratio, binder type, binder amount, and various chemical additives such as cobalt and molybdenum. A number of sorbents selected on the basis of screening tests were subjected to bench-scale testing for 10 cycles at high temperature, high pressure (HTHP) conditions using the reactor system designed and constructed during the base program. This reactor system is capable of operation either as a 2.0 in. or 3.0 in. I.D. bubbling bed and is rated up to 20 atm operation at 871{degrees}C. Bench-scale testing variables included sorbent type, temperature (550 to 750{degrees}C), gas type (KRW or Texaco gasifier gas), steam content of coal gas, and fluidizing gas velocity (6 to 15 cm/s). The sorbents prepared by spray drying showed poor performance in terms of attrition resistance and chemical reactivity. On the other hand, the granulation method proved to be very successful. For example, a highly attrition-resistant zinc titanate formulation, ZT-4, prepared by granulation exhibited virtually no zinc loss and demonstrated a constant high reactivity and sulfur capacity over 10 cycles, i.e., approximately a 60 percent capacity utilization, with Texaco gas at 750{degrees}C, 15 cm/s fluidizing velocity and 15 atm pressure. The commercial potential of the granulation method for zinc titanate manufacture was demonstrated by preparing two 80 lb batches of sorbent with zinc to titanium mol ratios of 0.8 and 1.5.

  8. Durable metal oxide-based sorbents for coal gas desulfurization

    Energy Technology Data Exchange (ETDEWEB)

    Abbasian, J.; Slimane, R.B.; Wangerow, J.R.; Zarnegar, M.K. [Inst. of Gas Technology, Des Plaines, IL (United States); Cicero, D.C. [Dept. of Energy, Morgantown, WV (United States). Federal Energy Technology Center

    1998-12-31

    Development of high temperature desulfurization regenerable sorbents for the Integrated Gasification Combined Cycle (IGCC) process has been pursued over the last two decades, primarily using various combinations of transition metal oxides. The primary focus has been directed toward applications above 550 C, restricting the choice of metal oxides to those that possess favorable thermodynamic equilibria. These efforts led to the emergence of zinc-based sorbents, such as zinc titanate, as the leading candidates. Recent studies have indicated that desulfurization system components become prohibitively expensive with increasing operating temperature and that the overall process efficiency gains of conducting desulfurization above 550 C may not be sufficient to justify operation at such high temperatures. The optimum desulfurization temperature appears to be in the range of 350 to 550 C, where technical viability and process efficiency result in lower overall process cost. In addition, because of the more favorable thermodynamic equilibria in the lower temperature range, a large number of metal oxides can be considered for coal gas desulfurization, increasing the likelihood of developing suitable sorbents. This paper reports on the results obtained in an on-going study at the Institute of Gas Technology (IGT), for the development of durable mixed-metal oxide sorbents for fluidized-bed desulfurization of coal-derived fuel gases in the temperature range of 350 to 550 C. The sorbent formulations prepared, their sulfidation performance and regenerability, and the physical and chemical properties of a select group of sorbents are presented and discussed. The results from multi-cycle evaluation tests of a few sorbents in a bench-scale high-pressure high-temperature fluidized-bed reactor are also presented.

  9. Specificity of noble metals dynamic sorption preconcentration on reversed-phase sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Fedyunina, N.N.; Seregina, I.F.; Ossipov, K.; Dubenskiy, A.S. [Chemistry Department, Analytical Chemistry Division, Lomonosov Moscow State University, 1-3 Leninskie Gory, 119991 Moscow (Russian Federation); Tsysin, G.I. [Chemistry Department, Analytical Chemistry Division, Lomonosov Moscow State University, 1-3 Leninskie Gory, 119991 Moscow (Russian Federation); Institute for Spectroscopy, Russian Academy of Sciences, 5 Fizicheskaya Street, 142190 Moscow, Troitsk (Russian Federation); Bolshov, M.A., E-mail: mbolshov@mail.ru [Chemistry Department, Analytical Chemistry Division, Lomonosov Moscow State University, 1-3 Leninskie Gory, 119991 Moscow (Russian Federation)

    2013-10-10

    Graphical abstract: -- Highlights: •StrataX and StrataX-AW for PGMs’ preconcentration were used for the first time. •Steric structure of chlorocomplexes plays critical role in the sorption mechanism. •The conditions of quantitative and reversible sorption of Ir on StrataX-AW were found. •The quantitative and reversible schemes for Pd, Pt, Au and Ir are developed. -- Abstract: The reversible sorption preconcentration of noble metals (NMs) using different schemes “sorbent–reagent–eluent” was investigated. The extraction of Au, Pd, Pt, Ir, Rh and Ru chlorocomplexes from hydrochloric acid solutions on hyper-crosslinked polysterene MN-200 in the form of ion associates with tributylamine (TBA) and 4-(n-octyl)diethylenetriamine (ODETA) was investigated. It was found that Pd, Pt and Au were quantitatively and reversibly extracted using TBA on hyper-crosslinked polysterene; the appropriate eluent for desorption was 1 M solution of HCl in ethanol. Ir, Rh and Ru under these conditions were not sorbed quantitatively. It was found that sorbent hydrophobicity is not the main characteristic that defines the efficiency of sorption of a particular NM ion associate. Different efficiencies of hyper-crosslinked polysterene MN-200 for sorption of square-planar chlorcomplexes of Pt, Pd and Au and octahedral complexes of Ir, Rh and Ru were found. For the first time, the sorbents with their own N-atoms – StrataX and StrataX-AW – were used for the sorption of Ir, Rh and Ru. Using these sorbents, the sorption of Ir was increased up to 95%, and the sorption of Ru and Rh was increased to about 40%. We can explain these results by nonspecific interaction of chlorcomplexes of Ir, Rh and Ru with ethylenediamine groups of the sorbent. Weak bases with large anions may be applied for desorption of Ir, Rh and Ru. Two schemes of dynamic sorption preconcentration of NMs from hydrochloric acid solutions were proposed – hyper-crosslinked polysterene MN-200 for the determination

  10. Selective extraction and determination of neonicotinoid insecticides in wine by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Rodríguez-Cabo, T; Casado, J; Rodríguez, I; Ramil, M; Cela, R

    2016-08-19

    A simplified, high throughput procedure for the determination of five neonicotinoid insecticides in red and white wines, using liquid chromatography (LC)-tandem mass spectrometry (MS/MS), is presented. The effects of different experimental parameters (extraction sorbent, solvent elution and clean-up conditions) in the efficiency and the selectivity of the sample preparation process were assessed through calculation of the extraction yields and the matrix effects (MEs). Wines (10mL) were concentrated using OASIS HLB cartridges, on-line connected to Florisil clean-up cartridges, with acetonitrile serving as the elution solvent. The extract (5mLvol) was concentrated to 1mL and injected in the LC-ESI-MS/MS system. The optimized procedure provided quantitative extraction yields at the same time that the efficiency of ESI ionization remained unchanged between standards and sample extracts. Overall recoveries, calculated against authentic standards in ACN, varied between 77 and 119% and the attained limits of quantification remained below 0.2ngmL(-1). Analysis of commercial wines revealed imidacloprid residues in more than 50% of processed samples, with a maximum level of 14ngmL(-1). Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Total on-line purchasing system (TOPS)

    Energy Technology Data Exchange (ETDEWEB)

    Collins, N.

    1995-11-01

    The Information Management Division (IMD) at LLNL is developing a new purchasing system for the Procurement Department. The first major development of this new system is called, {open_quotes}Total On-Line Purchasing System{close_quotes} (TOPS). TOPS will help speed up the requisitioning process by having requisitions electronically entered by requesters and electronically sent to buyers to be put on Purchase Orders. The new purchasing system will use Electronic Commerce (EC)/Electronic Data Interchange (EDI), to help increase transaction flows for shipping notices, RFQs, Quotes, Purchase Orders, and Invoices. ANSI X.12 is the EDI standard that this new EC will use.

  12. On-Line Core Thermal-Hydraulic Model Improvement

    Energy Technology Data Exchange (ETDEWEB)

    In, Wang Kee; Chun, Tae Hyun; Oh, Dong Seok; Shin, Chang Hwan; Hwang, Dae Hyun; Seo, Kyung Won

    2007-02-15

    The objective of this project is to implement a fast-running 4-channel based code CETOP-D in an advanced reactor core protection calculator system(RCOPS). The part required for the on-line calculation of DNBR were extracted from the source of the CETOP-D code based on analysis of the CETOP-D code. The CETOP-D code was revised to maintain the input and output variables which are the same as in CPC DNBR module. Since the DNBR module performs a complex calculation, it is divided into sub-modules per major calculation step. The functional design requirements for the DNBR module is documented and the values of the database(DB) constants were decided. This project also developed a Fortran module(BEST) of the RCOPS Fortran Simulator and a computer code RCOPS-SDNBR to independently calculate DNBR. A test was also conducted to verify the functional design and DB of thermal-hydraulic model which is necessary to calculate the DNBR on-line in RCOPS. The DNBR margin is expected to increase by 2%-3% once the CETOP-D code is used to calculate the RCOPS DNBR. It should be noted that the final DNBR margin improvement could be determined in the future based on overall uncertainty analysis of the RCOPS.

  13. Fully On-line Introductory Physics with a Lab

    Science.gov (United States)

    Schatz, Michael

    We describe the development and implementation of a college-level introductory physics (mechanics) course and laboratory that is suited for both on-campus and on-line environments. The course emphasizes a ``Your World is Your Lab'' approach whereby students first examine and capture on video (using cellphones) motion in their immediate surroundings, and then use free, open-source software both to extract data from the video and to apply physics principles to build models that describe, predict, and visualize the observations. Each student reports findings by creating a video lab report and posting it online; these video lab reports are then distributed to the rest of the class for peer review. In this talk, we will discuss the student and instructor experiences in courses offered to three distinct audiences in different venues: (1) a Massively Open On-line Course (MOOC) for off-campus participants, (2) a flipped/blended course for on-campus students, and, most recently, (3) a fully-online course for off-campus students.

  14. Fast Analysis of Vitamin A and E in Animal Derived Foods by On-Line Solid Phase Extraction Coupled with High Performance Liquid Chromatography%在线固相萃取-高效液相色谱联用测定动物源食品中的维生素A、E

    Institute of Scientific and Technical Information of China (English)

    谢云峰; 王浩; 刘佟; 任丹丹; 杨永坛

    2014-01-01

    采用固相萃取与双梯度高效液相色谱联用技术,建立了一种在线固相萃取-高效液相色谱同时测定动物源食品中维生素A、E的分析方法。样品于80℃下皂化反应30 min,经离心沉淀后引入一维C8固相萃取柱,采用60%( V/V)甲醇溶液对目标物进行在线富集净化,然后通过阀切换将其转移至二维液相分析系统进行分离检测。考察了萃取填料、上样溶剂及洗脱条件对猪肝、鸡蛋和配方乳粉的维生素A、E富集和基质净化效果。结果表明,在优化条件下,方法线性范围为0.02~20 mg/L,线性相关系数R2≥0.9998,对维生素A、E的检出限(S/N=3)为3.0~30.0μg/L,实际样品加标回收率为87.3%~115.0%,相对标准偏差(RSD)为1.8%~4.6%。本方法操作简便,灵敏度高,可用于动物源食品中维生素A、E的快速测定。%An automated analytical method for simultaneous determination of vitamin A and E in livers, fortified infant formulae and eggs has been developed based on on-line solid phase extraction (SPE) coupled with a dual gradient high performance liquid chromatography system with column-switching. Firstly, food samples were centrifuged after saponified in mixture solution of anhydrous alcohol, potassium hydroxide and ascorbic acid at 80 ℃ for 30 min. Secondly, the saponified sample was loaded and washed on the first dimension extraction column using methanol-water (60∶40, V/V). Afterwards, the targeted analytes were trapped and enriched on the SPE column. Finally, the trapped analytes were transferred to the second dimension analysis column by valve-switching technique for the following separation and determination. Several key factors such as the type of SPE columns, elution buffer as well as pH of washing solution were optimized. The results showed that the calibration curves of vitamin A and E were linear in the range of 0 . 02-20 mg/L with correlation coefficient (R2) more than 0. 9998. In addition, the limits of detection

  15. Analysis of drugs of abuse in human plasma using microextraction by packed sorbents and ultra-high-performance liquid chromatography.

    Science.gov (United States)

    Fernández, P; González, M; Regenjo, M; Ares, A M; Fernández, A M; Lorenzo, R A; Carro, A M

    2017-02-17

    A miniaturized and simple method based on digitally programmed microextraction by packed sorbent (eVol(®)-MEPS) coupled to ultra-performance liquid chromatography (UPLC) has been developed for quantitative determination of three synthetic cathinones and seven conventional drugs of abuse and metabolites. The influence of several extraction parameters, such as washing and elution solvents were tested. In addition important variables affecting MEPS performance, namely sample volume, sorbent drying time, washing solvent volume, elution volume, number of extraction cycles, sorbent phase and pH, were evaluated using an asymmetrical screening design. The optimal experimental conditions involved 300μL of plasma, loading 10×100μL of sample through a C8/SCX sorbent in a MEPS syringe placed in the semi-automatic eVol(®) system, washing using 150μL H2O:MeOH (90:10, v/v), drying for 0.5min and elution using 200μL dichloromethane:2-propanol:ammonium hydroxide (78:20:2, v/v/v). The drugs separation was achieved using an ACQUITY BEH Shield RP18 column (2.1mm×100mm×1.7μm) in 3min. Under optimized conditions the proposed method was validated in terms of selectivity, linearity, limits of detection (LOD) and quantitation (LOQ), precision and matrix effect, using standard addition calibration. The combination of MEPS and UPLC provides a method for the primary screening of the analytes in 18min with excellent recoveries at three concentration levels, ranging between 80 and 104% (relative standard deviation <11%). The developed methodology has been successfully applied to plasma samples from polydrug abusers.

  16. On-line and Mobil Learning Activities

    Science.gov (United States)

    Ackerman, S. A.; Whittaker, T. M.; Jasmin, T.; Mooney, M. E.

    2012-12-01

    Introductory college-level science courses for non-majors are critical gateways to imparting not only discipline-specific information, but also the basics of the scientific method and how science influences society. They are also indispensable for student success to degree. On-line, web-based homework (whether on computers or mobile devices) is a rapidly growing use of the Internet and is becoming a major component of instruction in science, replacing delayed feedback from a few major exams. Web delivery and grading of traditional textbook-type questions is equally effective as having students write them out for hand grading, as measured by student performance on conceptual and problem solving exams. During this presentation we will demonstrate some of the interactive on-line activities used to teach concepts and how scientists approach problem solving, and how these activities have impacted student learning. Evaluation of the activities, including formative and summative, will be discussed and provide evidence that these interactive activities significantly enhance understanding of introductory meteorological concepts in a college-level science course. More advanced interactive activities are also used in our courses for department majors, some of these will be discussed and demonstrated. Bring your mobile devices to play along! Here is an example on teaching contouring: http://profhorn.aos.wisc.edu/wxwise/contour/index.html

  17. Dual layer hollow fiber sorbents: Concept, fabrication and characterization

    KAUST Repository

    Bhandari, Dhaval

    2013-02-01

    Hollow fiber sorbents are pseudo-monolithic separations materials created with fiber spinning technology using a polymer \\'binder\\', impregnated with high loadings of sorbent \\'fillers\\' [1]. To increase purified gas recovery during the sorption step and to ensure consistent sorption capacity over repeated cycles, a dense, thin polymer barrier layer on the fiber sorbents is needed to allow only thermal interactions between the sorbate loaded layer and the thermal regeneration fluid. This paper considers materials and methods to create delamination-free dual layer fiber sorbents, with a porous core and a barrier sheath layer formed using a simultaneous co-extrusion process. Low permeability polymers were screened for sheath layer creation, with the core layer comprising cellulose acetate polymer as binder and zeolite NaY as sorbent fillers. Appropriate core and sheath layer dope compositions were determined by the cloud-point method and rheology measurements. The morphology of the as-spun fibers was characterized in detail by SEM, EDX and gas permeation analysis. A simplified qualitative model is described to explain the observed fiber morphology. The effects of core, sheath spin dope and bore fluid compositions, spinning process parameters such as air-gap height, spin dope and coagulation bath temperatures, and elongation draw ratio are examined in detail. © 2012 Elsevier B.V. All rights reserved.

  18. Cheap carbon sorbents produced from lignite by catalytic pyrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Kuznetsov, B.N.; Schchipko, M.L. [Inst. of Chemistry of Natural Organic Materials, Akademgorodok, Krasnoyarsk (Russian Federation)

    1995-12-01

    Some data are presented describing the new technology of carbon sorbent production from powdered lignite in the installation with fluidized bed of catalyst. It was shown the different types of char products with extended pore structure and high sorption ability can be produced from cheap and accessible lignite of Kansk-Achinsk coal pit in pilot installation with fluidized bed of Al-Cu-Cr oxide catalyst or catalytically active slag materials. In comparison with the conventional technologies of pyrolysis the catalytic pyrolysis allows to increase by 3-5 times the process productivity and to decrease significantly the formation of harmful compounds. The latter is accomplished by complete oxidation of gaseous pyrolysis products in the presence of catalysts and by avoiding the formation of pyrolysis tars - the source of cancerogenic compounds. The technology of cheap powdered sorbent production from lignites makes possible to obtain from lignite during the time of pyrolysis only a few seconds char products with porosity up to 0.6 cm{sup 3} /g, and specific surface area more than 400 m{sup 3} /g. Some methods of powdered chars molding into carbon materials with the different shape were proved for producing of firmness sorbents. Cheap carbon sorbents obtained by thermocatalytic pyrolysis can be successfully used in purification of different industrial pollutants as one-time sorbent or as adsorbents of long-term application with periodic regeneration.

  19. Advanced Sorbents for Oil-Spill Cleanup: Recent Advances and Future Perspectives.

    Science.gov (United States)

    Ge, Jin; Zhao, Hao-Yu; Zhu, Hong-Wu; Huang, Jin; Shi, Lu-An; Yu, Shu-Hong

    2016-12-01

    Oil sorbents play a very important part in the remediation processes of oil spills. To enhance the oil-sorption properties and simplify the oil-recovery process, various advanced oil sorbents and oil-collecting devices based on them have been proposed recently. Here, we firstly discuss the design considerations for the fabrication of oil sorbents and describe recently developed oil sorbents based on modification strategy. Then, recent advances regarding oil sorbents mainly based on carbon materials and swellable oleophilic polymers are also presented. Subsequently, some additional properties are emphasized, which are required by oil sorbents to cope with oil spills under extreme conditions or to facilitate the oil-collection processes. Furthermore, some oil-collection devices based on oil sorbents that have been developed recently are shown. Finally, an outlook and challenges for the next generation of oil-spill-remediation technology based on oil-sorbents materials are given.

  20. Application of multiwall carbon nanotubes impregnated with 5-dodecylsalicylaldoxime for on-line copper preconcentration and determination in water samples by flame atomic absorption spectrometry.

    Science.gov (United States)

    Tobiasz, Anna; Walas, Stanisław; Soto Hernández, Arlene; Mrowiec, Halina

    2012-07-15

    The paper presents application of multiwall carbon nanotubes (MWCNTs) modified with 5-dodecylsalicylaldoxime to copper(II) flow-injection on-line preconcentration and flame atomic absorption spectrometric (FAAS) determination. Two new sorbents were obtained by impregnation of MWCNTs with Cu(II)-LIX 622(®) complex, however in the first case modification was preceded by carbon wall activation via oxidization (Cu-LIX-CNT-A sorbent), and in the second one no surface activation was performed (Cu-LIX-CNT sorbent). It was found that effective leaching of initially introduced copper and Cu(II) retained in preconcentration process could be realized with the use 7% and 5% (v/v) nitric acid, for particular sorbents. Testing the influence of loading solution pH and rate of loading on sorption it was found out that optimal range of loading solution pH was about 4.5-6.3 for activated and 6.15-6.25 for non-activated CNT. Investigation of sorption kinetics showed that the process can be described by pseudo-second order reaction model. Sorption equilibrium conditions (90% sorption) for LIX-CNT-A and LIX-CNT were obtained after 8-15min, respectively and maximum sorption capacity for the new sorbents amounted to 18.1mgg(-1) and 31.6mgg(-1), respectively. For the examined sorbents enrichment factors increased with extension of loading time up to 180s: linearly for activated and non-linearly for non-activated MWCNTs. Influence of potential interferents such as Cd(II), Zn(II), Fe(III), Mg(II) and Ca(II) ions on copper(II) sorption on the new CNT materials was examined individually and with the use of 2(5-2) factorial design. The study revealed significant interference from iron, magnesium and calcium ions at relatively high concentrations. Applicability of the proposed sorbents was tested for Cu(II) determination in various kinds of water samples and the results were compared with those obtained with the use of ICP MS as a reference technique. Copper(II) determination in two certified

  1. Low-temperature desulfurizing reaction with Cu-containing sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Yi, Kwang Bok; Choi, Eun Mi; Song, Yi Keun; Rhee, Young Woo [Department of Chemical Engineering, Chungnam National University, Taejeon (Korea)

    1999-10-01

    The sorbents containing Cu O as an active material were prepared and their effectiveness in desulfurization was investigated at low temperatures(350-550 degree C). M.I.5 and MnO{sub 2} were chosen as additives and SiO{sub 2} was chosen as support material. In the low temperature regeneration reaction, sulfate was formed, which could not be decomposed until regeneration temperature reached 650 degree C. Sulfidation reaction rate decreased as calcination temperature increased. Promoting effect of MoO{sub 3} was not observed throughout the sulfidation/regeneration reaction. When SiO{sub 2} content was below 25% of sorbents composition, sulfur loading of above 10% could be obtained. Mass transfer inhibition by sulfiding gas was observed for the sorbents containing no SiO{sub 2}. 9 refs., 9 figs., 4 tabs.

  2. Glutathione analogue sorbents selectively bind glutathione S-transferase isoenzymes.

    Science.gov (United States)

    Castro, V M; Kelley, M K; Engqvist-Goldstein, A; Kauvar, L M

    1993-06-01

    Novel affinity sorbents for glutathione S-transferases (GSTs) were created by binding glutathione (GSH) analogues to Sepharose 6B. The GSH molecule was modified at the glycine moiety and at the group attached to the sulphur of cysteine. When tested by affinity chromatography in a flow-through microplate format, several of these sorbents selectively bound GST isoenzymes. gamma E-C(Hx)-phi G (glutathione with a hexyl moiety bound to cysteine and phenylglycine substituted for glycine) specifically bound rat GST 7-7, the Pi-class isoenzyme, from liver, kidney and small intestine. gamma E-C(Bz)-beta A (benzyl bound to cysteine and beta-alanine substituted for glycine) was highly selective for rat subunits 3 and 4, which are Mu-class isoenzymes. By allowing purification of the isoenzymes under mild conditions that preserve activity, the novel sorbents should be useful in characterizing the biological roles of GSTs in both normal animal and cancer tissues.

  3. In-vitro myoglobin clearance by a novel sorbent system.

    Science.gov (United States)

    Kuntsevich, Viktoriya I; Feinfeld, Donald A; Audia, Pat F; Young, Wendell; Capponi, Vincent; Markella, Marianna; Winchester, James F

    2009-01-01

    Rhabdomyolysis may lead to acute kidney injury following deposition of myoglobin in renal tubules. Although high-flux dialysis membranes may remove a substantial amount of myoglobin from plasma, this may still not be sufficient to prevent renal damage. We tested a new polymer sorbent, X-Sorb, in vitro to determine its potential to clear myoglobin from solutions. Normal saline or human serum in which myoglobin was dissolved was perfused by a peristaltic pump through a column packed with the sorbent. After a 4-hour perfusion, the myoglobin level in normal saline fell from 200,000 ng/ml to virtually undetectable ( 90% over 4 hours. X-Sorb appears to be an effective sorbent for myoglobin and warrants a trial in vivo to determine whether it is equally effective and safe.

  4. Aprender a innovar: una experiencia on line

    Directory of Open Access Journals (Sweden)

    Joaquín MORENO MARCHAL

    2014-11-01

    Full Text Available La creatividad y la innovación se han convertido en recursos clave en la denominada sociedad del conocimiento, que bien podría ser también llamada sociedad de la innovación. Pero innovar es una actividad compleja, que integra la aplicación de múltiples capacidades, el pensamiento divergente y convergente, la gestión de equipos humanos, la comunicación. Ahora bien, a innovar se puede, y se debe, aprender. Aprender a innovar es un reto y también una obligación para el conjunto del sistema educativo en todos sus niveles. Partiendo de estas consideraciones este trabajo expone una experiencia de aprendizaje de la creatividad y de la innovación a través de un curso totalmente on line basado en la plataforma MOODLE, en el marco del Programa de Formación Permanente de la Universidad de Cádiz. Se presenta un modelo del proceso de innovación, denominado CREALAB, de elaboración propia. Este modelo se ha utilizado como base del proceso de aprendizaje de la creatividad y de la innovación y en el diseño del curso, está organizado en torno a actividades y tiene un carácter iterativo y realimentado. Se presentan además el conjunto del diseño metodológico y los resultados obtenidos en las dos ediciones celebradas hasta el momento. El diseño del curso totalmente on line y los resultados alcanzados permiten estimar un alto potencial de aplicación, tanto a nivel personal como a nivel organizacional.

  5. On-line chemical composition analyzer development

    Energy Technology Data Exchange (ETDEWEB)

    Roberts, M.J.; Garrison, A.A.; Muly, E.C.; Moore, C.F.

    1992-02-01

    The energy consumed in distillation processes in the United States represents nearly three percent of the total national energy consumption. If effective control of distillation columns can be accomplished, it has been estimated that it would result in a reduction in the national energy consumption of 0.3%. Real-time control based on mixture composition could achieve these savings. However, the major distillation processes represent diverse applications and at present there does not exist a proven on-line chemical composition sensor technology which can be used to control these diverse processes in real-time. This report presents a summary of the findings of the second phase of a three phase effort undertaken to develop an on-line real-time measurement and control system utilizing Raman spectroscopy. A prototype instrument system has been constructed utilizing a Perkin Elmer 1700 Spectrometer, a diode pumped YAG laser, two three axis positioning systems, a process sample cell land a personal computer. This system has been successfully tested using industrially supplied process samples to establish its performance. Also, continued application development was undertaken during this Phase of the program using both the spontaneous Raman and Surface-enhanced Raman modes of operation. The study was performed for the US Department of Energy, Office of Industrial Technologies, whose mission is to conduct cost-shared R D for new high-risk, high-payoff industrial energy conservation technologies. Although this document contains references to individual manufacturers and their products, the opinions expressed on the products reported do not necessarily reflect the position of the Department of Energy.

  6. Characterization of calcium carbonate sorbent particle in furnace environment

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Kang Soo [Aerosol and Particle Technology Laboratory, Department of Mechanical Engineering, KAIST 291 Daehak-ro, Yuseong-gu, Daejeon, 305-701 (Korea, Republic of); Jung, Jae Hee [Environment Sensor System Research Center, KIST 39-1 Hawolgok-dong, Seongbuk-gu, Seoul, 136-791 (Korea, Republic of); Keel, Sang In; Yun, Jin Han; Min, Tai Jin [Environmental Systems Research Division, KIMM 104 Sinseongno, Yuseong-gu, Daejeon, 305-343 (Korea, Republic of); Kim, Sang Soo, E-mail: sskim@kaist.ac.kr [Aerosol and Particle Technology Laboratory, Department of Mechanical Engineering, KAIST 291 Daehak-ro, Yuseong-gu, Daejeon, 305-701 (Korea, Republic of)

    2012-07-01

    The oxy-fuel combustion system is a promising technology to control CO{sub 2} and NO{sub X} emissions. Furthermore, sulfation reaction mechanism under CO{sub 2}-rich atmospheric condition in a furnace may lead to in-furnace desulfurization. In the present study, we evaluated characteristics of calcium carbonate (CaCO{sub 3}) sorbent particles under different atmospheric conditions. To examine the physical/chemical characteristics of CaCO{sub 3}, which is used as a sorbent particle for in-furnace desulfurization in the oxy-fuel combustion system, they were injected into high temperature drop tube furnace (DTF). Experiments were conducted at varying temperatures, residence times, and atmospheric conditions in a reactor. To evaluate the aerosolizing characteristics of the CaCO{sub 3} sorbent particle, changes in the size distribution and total particle concentration between the DTF inlet and outlet were measured. Structural changes (e.g., porosity, grain size, and morphology) of the calcined sorbent particles were estimated by BET/BJH, XRD, and SEM analyses. It was shown that sorbent particles rapidly calcined and sintered in the air atmosphere, whereas calcination was delayed in the CO{sub 2} atmosphere due to the higher CO{sub 2} partial pressure. Instead, the sintering effect was dominant in the CO{sub 2} atmosphere early in the reaction. Based on the SEM images, it was shown that the reactions of sorbent particles could be explained as a grain-subgrain structure model in both the air and CO{sub 2} atmospheres.

  7. A Reusable Calcium-Based Sorbent for Desulfurizing Hot Coal Gas

    Energy Technology Data Exchange (ETDEWEB)

    Wheelock, T.D.; Hasler, D.J.L.

    2002-09-19

    The overall objective of this project has been to develop a superior, regenerable, calcium-based sorbent for desulfurizing hot coal gas. The sorbent should be strong, durable, inexpensive to manufacture, and capable of being reused many times. To achieve these objectives the project has focused on the development of the very promising core-in-shell sorbent.

  8. 40 CFR 75.39 - Missing data procedures for sorbent trap monitoring systems.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 16 2010-07-01 2010-07-01 false Missing data procedures for sorbent... (CONTINUED) AIR PROGRAMS (CONTINUED) CONTINUOUS EMISSION MONITORING Missing Data Substitution Procedures § 75.39 Missing data procedures for sorbent trap monitoring systems. (a) If a primary sorbent...

  9. High Temperature Flue Gas Desulfurization In Moving Beds With Regenerable Copper Based Sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Cengiz, P.A.; Ho, K.K.; Abbasian, J.; Lau, F.S.

    2002-09-20

    The objective of this study was to develop new and improved regenerable copper based sorbent for high temperature flue gas desulfurization in a moving bed application. The targeted areas of sorbent improvement included higher effective capacity, strength and long-term durability for improved process control and economic utilization of the sorbent.

  10. Investigation and Demonstration of Dry Carbon-Based Sorbent Injection for Mercury Control

    Energy Technology Data Exchange (ETDEWEB)

    Jim Butz; Terry Hunt

    2005-11-01

    Public Service Company of Colorado and ADA Technologies, Inc. have performed a study of the injection of activated carbon for the removal of vapor-phase mercury from coal-fired flue gas streams. The project was completed under contract to the US Department of Energy's National Energy Technology Laboratory, with contributions from EPRI and Public Service Company. The prime contractor for the project was Public Service Company, with ADA Technologies as the major subcontractor providing technical support to all aspects of the project. The research and development effort was conducted in two phases. In Phase I a pilot facility was fabricated and tests were performed using dry carbon-based sorbent injection for mercury control on a coal-fired flue gas slipstream extracted from an operating power plant. Phase II was designed to move carbon injection technology towards commercial application on coal-fired power plants by addressing key reliability and operability concerns. Phase II field work included further development work with the Phase I pilot and mercury measurements on several of PSCo's coal-fired generating units. In addition, tests were run on collected sorbent plus fly ash to evaluate the impact of the activated carbon sorbent on the disposal of fly ash. An economic analysis was performed where pilot plant test data was used to develop a model to predict estimated costs of mercury removal from plants burning western coals. Testing in the pilot plant was undertaken to quantify the effects of plant configuration, flue gas temperature, and activated carbon injection rate on mercury removal. All three variables were found to significantly impact the mercury removal efficiency in the pilot. The trends were clear: mercury removal rates increased with decreasing flue gas temperature and with increasing carbon injection rates. Mercury removal was much more efficient with reverse-gas and pulse-jet baghouse configurations than with an ESP as the particulate

  11. Sorbents based on xerogels of zirconium, aluminum and manganese oxyhydroxides

    Directory of Open Access Journals (Sweden)

    R.V. Smotraiev

    2016-05-01

    Full Text Available The actual problem of water supply in the world and in Ukraine, in particular, is a high level of pollution in water resources and an insufficient level of drinking water purification. With industrial wastewater, a significant amount of pollutants falls into water bodies, including suspended particles, sulfates, iron compounds, heavy metals, etc. Aim: The aim of this work is to determine the impact of aluminum and manganese ions additives on surface and sorption properties of zirconium oxyhydroxide based sorbents during their production process. Materials and Methods: The sorbents based on xerogels of zirconium, aluminum and manganese oxyhydroxides were prepared by sol-gel method during the hydrolysis of metal chlorides (zirconium oxychloride ZrOCl2, aluminum chloride AlCl3 and manganese chloride MnCl2 with carbamide. Results: The surface and sorption properties of sorbents based on xerogels of zirconium, aluminum and manganese oxyhydroxides were investigated. X-ray amorphous structure and evolved hydroxyl-hydrate cover mainly characterize the obtained xerogels. The composite sorbents based on xerogels of zirconium oxyhydroxide doped with aluminum oxyhydroxide (aS = 537 m2/g and manganese oxyhydroxide (aS = 356 m2/g have more developed specific surface area than single-component xerogels of zirconium oxyhydroxide (aS = 236 m2/g and aluminum oxyhydroxide (aS = 327 m2/g. The sorbent based on the xerogel of zirconium and manganese oxyhydroxides have the maximum SO42--ions sorption capacity. It absorbs 1.5 times more SO42–-ions than the industrial anion exchanger AN-221. The sorbents based on xerogels of zirconium oxyhydroxide has the sorption capacity of Fe3+-ions that is 1.5…2 times greater than the capacity of the industrial cation exchanger KU-2-8. The Na+-ions absorption capacity is 1.47…1.56 mmol/g for each sorbent. Conclusions: Based on these data it can be concluded that the proposed method is effective for sorbents production based on

  12. Multi-phase extraction of glycoraphanin from broccoli using aminium ionic liquid-based silica.

    Science.gov (United States)

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

    2013-01-01

    Glucosinolates, a class of phytochemicals found in broccoli, have attracted recent interest due to the potential health benefits associated with their dietary intake. Glucoraphanin, the most common glucosinolate in broccoli can be converted to a known cancer chemopreventive agent. Multi-phase extraction in solid-phase extraction cartridges was developed to simultaneously extract and separate this compound. Multi-phase extraction with functionalised ionic liquid-based silica as a sorbent was used to simultaneously extract and separate glucoraphanin from broccoli. The sorbent and broccoli sample were packed into a single cartridge, and a fixed volume of water was then used to extract and remove the target compound from the sample to the sorbent over 15 repetitions. The sorbent was then washed with n-hexane to remove any interference and the target compound was eluted with water-1% acetic acid (vol.). Under the optimised condition, 0.038 mg/g of glucoraphanin was obtained by multi-phase extraction with 0.2 g of sorbent. The adsorption isotherm allowed investigation of the interactions between the sorbent and target compound and provided evidence for the accuracy of this method. The low deviation error, small amount of solvents required, highly selective separation and stability of the method justify further research. Copyright © 2012 John Wiley & Sons, Ltd.

  13. Chalcogenide aerogels as sorbents for radioactive iodine

    Energy Technology Data Exchange (ETDEWEB)

    Subrahmanyam, Kota S.; Sarma, Debajit; Malliakas, Christos; Polychronopoulou, Kyriaki; Riley, Brian J.; Pierce, David A.; Chun, Jaehun; Kanatzidis, Mercouri G.

    2015-04-14

    Iodine (129I) is one of the radionuclides released in nuclear fuel reprocessing and poses risk to public safety due to its involvement in human metabolic processes. In order to prevent the leaching of hazardous radioactive iodine into the environment, its effective capture and sequestration is pivotal. In the context of finding a suitable matrix for capturing radioactive iodine the chalcogels, NiMoS4, CoMoS4, Sb4Sn4S12, Zn2Sn2S6, and CoSx (x = 4-5) were explored as iodine sorbents. All the chalcogels showed high uptake, reaching up to 225 mass% (2.25 g/g) of the final mass owing to strong chemical and physical iodine-chalcogen interactions. Analysis of the iodine-loaded specimens revealed that the iodine chemically reacted with Sb4Sn4S12, Zn2Sn2S6, and CoSx to form metal complexes SbI3, SnI4, and, KI respectively. The NiMoS4 and CoMoS4 chalcogels did not appear to undergo a chemical reaction with iodine since iodide complexes were not observed with these samples. Once heated, the iodine-loaded chalcogels released iodine in the temperature range of 75 °C to 220 °C, depending on the nature of iodine speciation. In the case of Sb4Sn4S12 and Zn2Sn2S6 iodine release was observed around 150 °C in the form of SnI4 and SbI3, respectively. The NiMoS4, CoMoS4, and CoSx released iodine at ~75 °C, which is consistent with physisorbed iodine. Preliminary investigations on consolidation of iodine-loaded Zn2Sn2S6 with Sb2S3 as a glass forming additive showed the content of iodine in consolidated glass ingots at around 25 mass%.

  14. High capacity MnOx:ZrO2 sorbent for elementary mercury capture: preparation, characterization and comparison to other sorbents

    Science.gov (United States)

    Lakatos, J.; Snape, C. E.

    2017-02-01

    Manganese oxide-zirconia type (MnOx:ZrO2) sorbents were prepared using the sol-gel technique by co precipitation ZrO(NO3)2.xH2O and Mn(NO3)2 xH2O. The heat treatment below 500°C resulted a high surface area solid structure which consists of amorphous Mn2O3 (Bixbyite) and amorphous ZrO2 phases. This material was found a high capacity oxidative sorbent for mercury removal from gas streams.

  15. Influence of visualization on consumption during on-line shopping

    OpenAIRE

    Hictaler, Urška

    2013-01-01

    This diploma work studies the influence of visualization on consumption during on-line shopping. The first part of the thesis starts with key areas of visualization, consumption and on-line shopping. Visualization, areas of use, human perception and ways of product presentation in on-line shops are defined discussed first. Next, consumption, consumers and factors that influence their decisions and satisfaction are defined. The last topic in the first part of the thesis discusses on-line shopp...

  16. 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.

  17. On-Line Learning: One Way to Bring People Together

    Science.gov (United States)

    Goff-Kfouri, Carol Ann

    2006-01-01

    The purpose of this study was to demonstrate the benefits of on-line learning for adult learners and to further demystify three common misconceptions concerning on-line learning: students certainly do receive support from their on-line professors, the professor is pro-active rather than passive, and students may be more motivated to learn than in…

  18. A Distributed System for Learning Programming On-Line

    Science.gov (United States)

    Verdu, Elena; Regueras, Luisa M.; Verdu, Maria J.; Leal, Jose P.; de Castro, Juan P.; Queiros, Ricardo

    2012-01-01

    Several Web-based on-line judges or on-line programming trainers have been developed in order to allow students to train their programming skills. However, their pedagogical functionalities in the learning of programming have not been clearly defined. EduJudge is a project which aims to integrate the "UVA On-line Judge", an existing…

  19. Development of novel copper-based sorbents for hot-gas cleanup

    Energy Technology Data Exchange (ETDEWEB)

    Abbasian, J.

    1991-01-01

    The objective of this investigation is to evaluate several novel copper-based binary oxides for their suitability as regenerable sorbents for hot gas cleanup application in the temperature range of 650{degree} to 850{degree}C (1200{degree}--1550{degree}F). To achieve this objective, several novel copper-based binary oxide sorbents will be prepared. Experimental tests will be conducted at ambient pressure to determine the stability, sulfidation capacity, regenerability, and sulfidation kinetics of the novel sorbents. Tests will also be conducted at high pressure for the determination of the sulfidation reactivity, regenerability, and durability of the sorbents. The attrition characteristics of the sorbents will also be determined.

  20. On-Line Impact Load Identification

    Directory of Open Access Journals (Sweden)

    Krzysztof Sekuła

    2013-01-01

    Full Text Available The so-called Adaptive Impact Absorption (AIA is a research area of safety engineering devoted to problems of shock absorption in various unpredictable scenarios of collisions. It makes use of smart technologies (systems equipped with sensors, controllable dissipaters and specialised tools for signal processing. Examples of engineering applications for AIA systems are protective road barriers, automotive bumpers or adaptive landing gears. One of the most challenging problems for AIA systems is on-line identification of impact loads, which is crucial for introducing the optimum real-time strategy of adaptive impact absorption. This paper presents the concept of an impactometer and develops the methodology able to perform real-time impact load identification. Considered dynamic excitation is generated by a mass M1 impacting with initial velocity V0. An analytical formulation of the problem, supported with numerical simulations and experimental verifications is presented. Two identification algorithms based on measured response of the impacted structure are proposed and discussed. Finally, a concept of the AIA device utilizing the idea of impactometer is briefly presented.

  1. SOL: INNOVACIÓN ON-LINE

    Directory of Open Access Journals (Sweden)

    Rubén Faúndez

    2007-11-01

    Full Text Available Las aplicaciones de simulación tienden a ser cada vez más cercanas a usuarios e industrias. Sin embargo, muchas de ellas no poseen ni la capacidad ni el conocimiento como para desarrollar internamente sus modelos de simulación. Por este motivo, y como una forma de apoyar la toma de decisiones basándose en modelos de simulación, se presenta la plataforma SOL (Simulación On Line. La metodología completa de trabajo, así como la interacción entre SOL, Empresa y Asesor, son presentadas. Su base de datos, los niveles de usuarios, sus funcionalidades, y la creación automatizada de información grafica y visual, también son explicadas. En el caso de aplicación, el uso de SOL para apoyar la toma de decisiones en una operación de movimiento de material, permite a los tomadores de decisión acceder a análisis robustos basados en información extraída de los modelos de simulación. SOL, al almacenar información, funcionar vía web, generar análisis automatizados y crear visualizaciones, permite cumplir con las expectativas de los usuarios respecto a una solución integral en simulación.

  2. Recent developments in novel sorbents for flue gas clean up

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Yan; Bisson, Teresa M.; Yang, Hongqun; Xu, Zhenghe [Department of Chemical and Materials Engineering, University of Alberta, Edmonton, Alberta (Canada)

    2010-10-15

    Coal combustion is one of the most important energy sources for electricity generation, but also produces airborne pollutants. The amount of SO{sub 2} and NO{sub x} for example, is in the order of hundreds to thousands of ppm, and tens to hundreds of ppm, respectively, while Hg in flue gases could be up to tens to hundreds of ppb. Flue gas desulphurization technology is already in place for SO{sub 2} removal, and new sorbents such as zeolites are being investigated for such an application. NO{sub x} can be removed by selective catalytic reduction with various catalysts. Mercury is the hardest to remove due to its persistent nature and relatively low concentration in flue gases. New sorbents have also been developed for mercury removal applications. A current trend in flue gas emission control is to remove Hg, NO{sub x} and SO{sub 2} simultaneously. Various catalytic sorbents have been investigated to remove two or more of these pollutants concurrently. This article reviews recent developments made for emission control of coal-fired power plant flue gases using novel sorbents to target individual or multiple pollutants. (author)

  3. MERCURY CONTROL WITH CALCIUM-BASED SORBENTS AND OXIDIZING AGENTS

    Energy Technology Data Exchange (ETDEWEB)

    Thomas K. Gale

    2002-06-01

    The initial tasks of this DOE funded project to investigate mercury removal by calcium-based sorbents have been completed, and initial testing results have been obtained. Mercury monitoring capabilities have been obtained and validated. An approximately 1MW (3.4 Mbtu/hr) Combustion Research Facility at Southern Research Institute was used to perform pilot-scale investigations of mercury sorbents, under conditions representative of full-scale boilers. The initial results of ARCADIS G&M proprietary sorbents, showed ineffective removal of either elemental or oxidized mercury. Benchscale tests are currently underway to ascertain the importance of differences between benchscale and pilot-scale experiments. An investigation of mercury-capture temperature dependence using common sorbents has also begun. Ordinary hydrated lime removed 80 to 90% of the mercury from the flue gas, regardless of the temperature of injection. High temperature injection of hydrated lime simultaneously captured SO{sub 2} at high temperatures and Hg at low temperatures, without any deleterious effects on mercury speciation. Future work will explore alternative methods of oxidizing elemental mercury.

  4. Modifying sorbents in controlled release formulations to prevent herbicides pollution

    Energy Technology Data Exchange (ETDEWEB)

    Cespedes, F.F.; Sanchez, M.V.; Garcia, S.P.; Perez, M.F. [University of Almeria, Almeria (Spain). Dept. of Inorganic Chemistry

    2007-10-15

    The herbicides chloridazon and metribuzin, identified as groundwater pollutants, were incorporated in alginate-based granules to obtain controlled release properties. In this research the effect of incorporation of sorbents such as bentonite, anthracite and activated carbon in alginate basic formulation were not only studied on encapsulation efficiency but also on the release rate of herbicides which was studied using water release kinetic tests. In addition, sorption studies of herbicides with bentonite, anthracite and activated carbon were made. The kinetic experiments of chloridazon and metribuzin release in water have shown that the release rate is higher in metribuzin systems than in those prepared with chloridazon, which has lower water solubility. Besides, it can be deduced that the use of sorbents reduces the release rate of the chloridazon and metribuzin in comparison to the technical product and to the alginate formulation without sorbents. The highest decrease in release rate corresponds to the formulations prepared with activated carbon as a sorbent. The water uptake, permeability, and time taken for 50% of the active ingredient to be released into water, were calculated to compare the formulations. On the basis of a parameter of an empirical equation used to fit the herbicide release data, the release of chloridazon and metribuzin from the various formulations into water is controlled by a diffusion mechanism.

  5. Evaluation of inorganic sorbent treatment for LWR coolant process streams

    Energy Technology Data Exchange (ETDEWEB)

    Roddy, J.W.

    1984-03-01

    This report presents results of a survey of the literature and of experience at selected nuclear installations to provide information on the feasibility of replacing organic ion exchangers with inorganic sorbents at light-water-cooled nuclear power plants. Radioactive contents of the various streams in boiling water reactors and pressurized water reactors were examined. In addition, the methods and performances of current methods used for controlling water quality at these plants were evaluated. The study also includes a brief review of the physical and chemical properties of selected inorganic sorbents. Some attributes of inorganic sorbents would be useful in processing light water reactor (LWR) streams. The inorganic resins are highly resistant to damage from ionizing radiation, and their exchange capacities are generally equivalent to those of organic ion exchangers. However, they are more limited in application, and there are problems with physical integrity, especially in acidic solutions. Research is also needed in the areas of selectivity and anion removal before inorganic sorbents can be considered as replacements for the synthetic organic resins presently used in LWRs. 11 figures, 14 tables.

  6. Monolithic natural gas storage delivery system based on sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Hornbostel, Marc; Krishnan, Gopala N.; Sanjurjo, Angel

    2016-09-27

    The invention provides methods for producing a strong, light, sorbent-based storage/dispenser system for gases and fuels. The system comprises a porous monolithic material with an adherent strong impervious skin that is capable of storing a gas under pressure in a safe and usable manner.

  7. Monolithic natural gas storage delivery system based on sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Hornbostel, Marc; Krishnan, Gopala N.; Sanjurjo, Angel

    2016-09-27

    The invention provides methods for producing a strong, light, sorbent-based storage/dispenser system for gases and fuels. The system comprises a porous monolithic material with an adherent strong impervious skin that is capable of storing a gas under pressure in a safe and usable manner.

  8. Modeling of calcium-based sorbent reactions with sulfur dioxide

    Directory of Open Access Journals (Sweden)

    Tomanović Ivan

    2015-01-01

    Full Text Available A mathematical model of calcium sorbent reactions for simulation of sulfur dioxide reduction from pulverized coal combustion fl e gasses is developed, implemented within numerical code and validated against available measurements under controlled conditions. The model attempts to closely resemble reactions of calcination, sintering and sulfation, occurring during the sorbent particles motion in the furnace. The sulfation is based on PSSM (Partially Sintered Spheres Model, coupled with simulated particle calcination and sintering. Complex geometry of the particle is taken into account, with the assumption that it consists of spherical grains in contact with each other. Numerical simulations of drop down tube reactors were performed for both CaCO3 and Ca(OH2 sorbent particles and results were compared with available experimental data from literature. The sorbent reactions model will be further used for simulations of desulfurization reactions in turbulent gas-particle flow under coalcombustion conditions. [Projekat Ministarstva nauke Republike Srbije, br. TR-33018: Increase in energy and ecology efficiency of processes in pulverized coal-fired furnace and optimization of utility steam boiler air preheater by using in-house developed software tools

  9. A selective sorbent for removing bacterial endotoxins from blood

    Science.gov (United States)

    Morozov, A. S.; Kopitsyna, M. N.; Bessonov, I. V.; Karelina, N. V.; Nuzhdina, A. V.; Sarkisov, I. Yu.; Pavlova, L. A.; Tsyurupa, M. P.; Blinnikova, Z. K.; Davankov, V. A.

    2016-12-01

    Synthetic ligands carrying a positive charge and capable of selective binding of bacterial endotoxins are covalently immobilized on surfaces of domestic hemosorbent Styrosorb-514 based on hypercrosslinked polystyrene. It is shown that the resulting sorbent aimed at treating sepsis exceeds imported specific hemosorbent in Toraymyxin™ columns in removing lipopolysaccharides, and can be used in domestically-produced Desepta columns.

  10. Solid-phase extraction based on ground methacrylate monolith modified with gold nanoparticles for isolation of proteins.

    Science.gov (United States)

    Vergara-Barberán, María; Lerma-García, María Jesús; Simó-Alfonso, Ernesto Francisco; Herrero-Martínez, José Manuel

    2016-04-21

    In this study, a novel polymeric material functionalized with gold nanoparticles (AuNPs) was prepared as solid-phase extraction (SPE) sorbent for isolation of proteins. The sorbent was synthesized from a powdered poly(glycidyl-co-ethylene dimethacrylate) monolith, and modified with ammonia, followed by immobilization of AuNPs on the pore surface of the material. To evaluate the performance of this SPE support, proteins were selected as test solutes, being the extraction conditions and other parameters (loading capacity and regenerative ability of sorbent) established. The results indicated that this sorbent could be employed to selectively capture proteins according to their pI, on the basis of the strong affinity of these biomacromolecules towards to AuNPs surface. The applicability of this sorbent was demonstrated by isolating protein species of interest (bovine serum albumin, cytochrome c and lectins in European mistletoe leaves), followed by SDS-PAGE analysis.

  11. Solid sorbents for removal of carbon dioxide from gas streams at low temperatures

    Science.gov (United States)

    Sirwardane, Ranjani V.

    2005-06-21

    New low-cost CO.sub.2 sorbents are provided that can be used in large-scale gas-solid processes. A new method is provided for making these sorbents that involves treating substrates with an amine and/or an ether so that the amine and/or ether comprise at least 50 wt. percent of the sorbent. The sorbent acts by capturing compounds contained in gaseous fluids via chemisorption and/or physisorption between the unit layers of the substrate's lattice where the polar amine liquids and solids and/or polar ether liquids and solids are located. The method eliminates the need for high surface area supports and polymeric materials for the preparation of CO.sub.2 capture systems, and provides sorbents with absorption capabilities that are independent of the sorbents' surface areas. The sorbents can be regenerated by heating at temperatures in excess of 35.degree. C.

  12. Evaluation of electrospun polyvinyl chloride/polystyrene fibers as sorbent materials for oil spill cleanup.

    Science.gov (United States)

    Zhu, Haitao; Qiu, Shanshan; Jiang, Wei; Wu, Daxiong; Zhang, Canying

    2011-05-15

    A novel, high-capacity oil sorbent consisting of polyvinyl chloride (PVC)/polystyrene (PS) fiber was prepared by an electrospinning process. The sorption capacity, oil/water selectivity, and sorption mechanism of the PVC/PS sorbent were studied. The results showed that the sorption capacities of the PVC/PS sorbent for motor oil, peanut oil, diesel, and ethylene glycol were 146, 119, 38, and 81 g/g, respectively. It was about 5-9 times that of a commercial polypropylene (PP) sorbent. The PVC/PS sorbent also had excellent oil/water selectivity (about 1000 times) and high buoyancy in the cleanup of oil over water. The SEM analysis indicated that voids among fibers were the key for the high capacity. The electrospun PVC/PS sorbent is a better alternative to the widely used PP sorbent for oil spill cleanup.

  13. Solid Sorbents for Removal of Carbon Dioxide from Gas Streams at Low Temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Sirwardane, Ranjani V.

    2005-06-21

    New low-cost CO2 sorbents are provided that can be used in large-scale gas-solid processes. A new method is provided for making these sorbents that involves treating substrates with an amine and/or an ether so that the amine and/or ether comprise at least 50 wt. percent of the sorbent. The sorbent acts by capturing compounds contained in gaseous fluids via chemisorption and/or physisorption between the unit layers of the substrate's lattice where the polar amine liquids and solids and/or polar ether liquids and solids are located. The method eliminates the need for high surface area supports and polymeric materials for the preparation of CO2 capture systems, and provides sorbents with absorption capabilities that are independent of the sorbents' surface areas. The sorbents can be regenerated by heating at temperatures in excess of 35 degrees C.

  14. Fuel gas desulfurization at elevated temperatures with copper-based sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Abbasian, J.; Hill, A.H.; Lau, F.S. [Inst. of Gas Technology, Des Plaines, IL (United States); Flytzani-Stephanopoulos, M. [Tufts Univ., Medford, MA (United States); Honea, F.I. [Illinois Clean Coal Inst., Carbondale, IL (United States)

    1995-12-31

    Zinc-based sorbents, the leading candidates for hot gas cleanup, have been shown to suffer from zinc volatilization at elevated temperatures, leading to sorbent deterioration, increasing sorbent replacement costs. Copper-based sorbents, because of the high melting point of the metal, do not suffer from this problem. However, bulk copper oxide is generally reduced to metallic copper in reducing fuel gas environments leading to thermodynamic limitations, resulting in insufficient level of desulfurization. The reduction stability and therefore the desulfurization performance of copper oxide sorbents can be significantly improved by combining copper oxide with other oxides in a supported form or as bulk mixed metal oxides. This paper addresses the results of a systematic study of several novel copper-based sorbents for hot gas cleanup application. The evaluation criteria included reduction stability, sulfidation reactivity and regenerability at elevated temperatures. The performance of the most promising sorbent in long duration cycle sulfidation-regeneration tests is also presented.

  15. Flow injection on-line preconcentration of low levels of Cr(VI) with detection by ETAAS

    DEFF Research Database (Denmark)

    Som-aum, Waraporn; Liawruangrath, Saisunee; Hansen, Elo Harald

    2002-01-01

    A flow injection (FI) on-line sorption preconcentration procedure utilizing a packed column reactor and combined with electrothermal atomic absorption spectrometry (ETAAS) is proposed for the determination of low levels of Cr(VI) in water samples. Polytetrafluoroethylene (PTFE) beads packed...... in a mini-column is used as sorbent material. The complex formed between Cr(VI) and ammonium pyrrolidine dithiocarbamate (APDC) is sorbed on the PTFE beads, and is subsequently eluted by an air-monosegmented discrete zone of absolute ethanol (35mul), the analyte being quantified by ETAAS....... The preconcentration procedure using the proposed column significantly enhances the preconcentration efficiency as compared with the preconcentration approach incorporating an open tubular PTFE knotted reactor (KR). Comparing the two procedure for equal surface sorption area, the advantages of using a packed column...

  16. Modifying sorbents in controlled release formulations to prevent herbicides pollution.

    Science.gov (United States)

    Flores Céspedes, F; Villafranca Sánchez, M; Pérez García, S; Fernández Pérez, M

    2007-10-01

    The herbicides chloridazon and metribuzin, identified as groundwater pollutants, were incorporated in alginate-based granules to obtain controlled release properties. In this research the effect of incorporation of sorbents such as bentonite, anthracite and activated carbon in alginate basic formulation were not only studied on encapsulation efficiency but also on the release rate of herbicides which was studied using water release kinetic tests. In addition, sorption studies of herbicides with bentonite, anthracite and activated carbon were made. The kinetic experiments of chloridazon and metribuzin release in water have shown that the release rate is higher in metribuzin systems than in those prepared with chloridazon, which has lower water solubility. Besides, it can be deduced that the use of sorbents reduces the release rate of the chloridazon and metribuzin in comparison to the technical product and to the alginate formulation without sorbents. The highest decrease in release rate corresponds to the formulations prepared with activated carbon as a sorbent. The water uptake, permeability, and time taken for 50% of the active ingredient to be released into water, T(50), were calculated to compare the formulations. On the basis of a parameter of an empirical equation used to fit the herbicide release data, the release of chloridazon and metribuzin from the various formulations into water is controlled by a diffusion mechanism. Sorption capacity of the sorbents for chloridazon and metribuzin, ranging from 0.53mgkg(-1) for the metribuzin sorption on bentonite to 2.03x10(5)mgkg(-1) for the sorption of chloridazon on the activated carbon, was the most important factor modulating the herbicide release.

  17. Silica- and germania-based dual-ligand sol-gel organic-inorganic hybrid sorbents combining superhydrophobicity and π-π interaction. The role of inorganic substrate in sol-gel capillary microextraction.

    Science.gov (United States)

    Seyyal, Emre; Malik, Abdul

    2017-04-29

    Principles of sol-gel chemistry were utilized to create silica- and germania-based dual-ligand surface-bonded sol-gel coatings providing enhanced performance in capillary microextraction (CME) through a combination of ligand superhydrophobicity and π-π interaction. These organic-inorganic hybrid coatings were prepared using sol-gel precursors with bonded perfluorododecyl (PF-C12) and phenethyl (PhE) ligands. Here, the ability of the PF-C12 ligand to provide enhanced hydrophobic interaction was advantageously combined with π-π interaction capability of the PhE moiety to attain the desired sorbent performance in CME. The effect of the inorganic sorbent component on microextraction performance of was explored by comparing microextraction characteristics of silica- and germania-based sol-gel sorbents. The germania-based dual-ligand sol-gel sorbent demonstrated superior CME performance compared to its silica-based counterpart. Thermogravimetric analysis (TGA) of the created silica- and germania-based dual-ligand sol-gel sorbents suggested higher carbon loading on the germania-based sorbent. This might be indicative of more effective condensation of the organic ligand-bearing sol-gel-active chemical species to the germania-based sol-gel network (than to its silica-based counterpart) evolving in the sol solution. The type and concentration of the organic ligands were varied in the sol-gel sorbents to fine-tune extraction selectivity toward different classes of analytes. Specific extraction (SE) values were used for an objective comparison of the prepared sol-gel CME sorbents. The sorbents with higher content of PF-C12 showed remarkable affinity for aliphatic hydrocarbons. Compared to their single-ligand sol-gel counterparts, the dual-ligand sol-gel coatings demonstrated significantly superior CME performance in the extraction of alkylbenzenes, providing up to ∼65.0% higher SE values. The prepared sol-gel CME coatings provided low ng L(-1) limit of detections (LOD

  18. Preparation of molecularly imprinted polymers using theanine as dummy template and its application as SPE sorbent for the determination of eighteen amino acids in tobacco.

    Science.gov (United States)

    Zhu, Fengling; Wang, Jing; Zhu, Lijun; Tan, Lanlan; Feng, Guanglin; Liu, Shaomin; Dai, Ya; Wang, Hua

    2016-04-01

    In this paper, a novel dummy template molecularly imprinted polymer (DMIP) based on a vinyl-SiO2 microspheres surface for the simultaneous selective recognition and enrichment of 18 amino acids was prepared via a surface molecular imprinting technique using theanine as a dummy template. Compared to the imprinted polymers prepared using traditional polymerization techniques, the obtained DMIPs exhibited a regular spherical shape and were relatively monodisperse. The maximal sorption capacity (Qmax) of the resulting DMIPs for the 18 amino acids was up to 1444.3 mg g(-1). A kinetic binding study showed that the sorption capacity reached 85.40% of Qmax in 25 min and sorption equilibrium at 30 min. The imprint factors of the sorbents ranged from 2.86 to 6.9 for the 18 amino acids, which indicated that the DMIP sorbents have high selectivity. An HPLC-UV method for the simultaneous determination of 18 amino acids in tobacco and tobacco smoke was developed using the DMIPs as sorbents for solid phase extraction (SPE) in the sample pretreatment procedure. Under the optimum experimental conditions, the materials had enrichment factors of up to 200 for the amino acids, and the recoveries of the 18 amino acids in tobacco smoke were in the range from 79% to 104% with relative standard deviations of less than 7.4%. It indicated that the obtained DMIP sorbents could specifically recognize the amino acids from complicated samples.

  19. Lime-based sorbents for high-temperature CO2 capture--a review of sorbent modification methods.

    Science.gov (United States)

    Manovic, Vasilije; Anthony, Edward J

    2010-08-01

    This paper presents a review of the research on CO(2) capture by lime-based looping cycles undertaken at CanmetENERGY's (Ottawa, Canada) research laboratories. This is a new and very promising technology that may help in mitigation of global warming and climate change caused primarily by the use of fossil fuels. The intensity of the anticipated changes urgently requires solutions such as more cost-effective technologies for CO(2) capture. This new technology is based on the use of lime-based sorbents in a dual fluidized bed combustion (FBC) reactor which contains a carbonator-a unit for CO(2) capture, and a calciner-a unit for CaO regeneration. However, even though natural materials are cheap and abundant and very good candidates as solid CO(2) carriers, their performance in a practical system still shows significant limitations. These limitations include rapid loss of activity during the capture cycles, which is a result of sintering, attrition, and consequent elutriation from FBC reactors. Therefore, research on sorbent performance is critical and this paper reviews some of the promising ways to overcome these shortcomings. It is shown that reactivation by steam/water, thermal pre-treatment, and doping simultaneously with sorbent reforming and pelletization are promising potential solutions to reduce the loss of activity of these sorbents over multiple cycles of use.

  20. Lime-Based Sorbents for High-Temperature CO2 Capture—A Review of Sorbent Modification Methods

    Directory of Open Access Journals (Sweden)

    Edward J. Anthony

    2010-08-01

    Full Text Available This paper presents a review of the research on CO2 capture by lime-based looping cycles undertaken at CanmetENERGY’s (Ottawa, Canada research laboratories. This is a new and very promising technology that may help in mitigation of global warming and climate change caused primarily by the use of fossil fuels. The intensity of the anticipated changes urgently requires solutions such as more cost-effective technologies for CO2 capture. This new technology is based on the use of lime-based sorbents in a dual fluidized bed combustion (FBC reactor which contains a carbonator—a unit for CO2 capture, and a calciner—a unit for CaO regeneration. However, even though natural materials are cheap and abundant and very good candidates as solid CO2 carriers, their performance in a practical system still shows significant limitations. These limitations include rapid loss of activity during the capture cycles, which is a result of sintering, attrition, and consequent elutriation from FBC reactors. Therefore, research on sorbent performance is critical and this paper reviews some of the promising ways to overcome these shortcomings. It is shown that reactivation by steam/water, thermal pre-treatment, and doping simultaneously with sorbent reforming and pelletization are promising potential solutions to reduce the loss of activity of these sorbents over multiple cycles of use.

  1. Lime-Based Sorbents for High-Temperature CO2 Capture—A Review of Sorbent Modification Methods

    Science.gov (United States)

    Manovic, Vasilije; Anthony, Edward J.

    2010-01-01

    This paper presents a review of the research on CO2 capture by lime-based looping cycles undertaken at CanmetENERGY’s (Ottawa, Canada) research laboratories. This is a new and very promising technology that may help in mitigation of global warming and climate change caused primarily by the use of fossil fuels. The intensity of the anticipated changes urgently requires solutions such as more cost-effective technologies for CO2 capture. This new technology is based on the use of lime-based sorbents in a dual fluidized bed combustion (FBC) reactor which contains a carbonator—a unit for CO2 capture, and a calciner—a unit for CaO regeneration. However, even though natural materials are cheap and abundant and very good candidates as solid CO2 carriers, their performance in a practical system still shows significant limitations. These limitations include rapid loss of activity during the capture cycles, which is a result of sintering, attrition, and consequent elutriation from FBC reactors. Therefore, research on sorbent performance is critical and this paper reviews some of the promising ways to overcome these shortcomings. It is shown that reactivation by steam/water, thermal pre-treatment, and doping simultaneously with sorbent reforming and pelletization are promising potential solutions to reduce the loss of activity of these sorbents over multiple cycles of use. PMID:20948952

  2. Water Treatment Residuals and Scrap Tire Rubber as Green Sorbents for Removal of Stormwater Metals.

    Science.gov (United States)

    Deng, Yang; Morris, Ciapha; Rakshit, Sudipta; Landa, Edward; Punamiya, Pravin; Sarkar, Dibyendu

    2016-06-01

    Bench scale tests were performed to evaluate two recycled wastes, water treatment residuals (WTR) and scrap tire rubber (STR), for adsorption of selected metals from urban stormwater, and assess their release from used sorbents. Aluminum-WTR alone could rapidly and effectively remove Cu, Pb, and Zn, while STR alone continuously released Zn accompanied with Cu and Pb adsorption. Zn leaching from STR was significantly reduced in the presence of WTR. Very little metals released from used combined adsorbents in NaNO3 solution, and only part of them were extracted with EDTA (a strong chelating agent), suggesting that metal release is not a concern in a typical stormwater condition. A combination of WTR and STR is a new, effective method for mitigation of urban stormwater metals-WTR can inhibit the STR leaching, and STR improves the hydraulic permeability of WTR powders, a limiting factor for stormwater flow when WTR is used alone.

  3. CHARACTERIZATION OF MODIFIED MONOSODIUM TITANATE - AN IMPROVED SORBENT FOR STRONTIUM AND ACTINIDE SEPARATIONS

    Energy Technology Data Exchange (ETDEWEB)

    Hobbs, D.; Taylor-Pashow, K.; Missimer, D.

    2010-12-21

    High-level nuclear waste produced from fuel reprocessing operations at the Savannah River Site (SRS) requires pretreatment to remove {sup 134,137}Cs, {sup 90}Sr, and alpha-emitting radionuclides (i.e., actinides) prior to disposal onsite as low level waste. An inorganic sorbent, monosodium titanate (MST), is currently used to remove {sup 90}Sr and alpha-emitting radionuclides, while a caustic-side solvent extraction process is used for removing {sup 134,137}Cs. A new peroxotitanate material, modified MST, or mMST, has recently been developed and has shown increased removal kinetics and capacity for {sup 90}Sr and alpha-emitting radionuclides compared to the current baseline material, MST. This paper describes recent results focused on further characterization of this material.

  4. Low temperature SO{sub 2} removal with solid sorbents in a circulating fluidized bed absorber. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Lee, S.K.; Keener, T.C.

    1994-10-10

    A novel flue gas desulfurization technology has been developed at the University of Cincinnati incorporating a circulating fluidized bed absorber (CFBA) reactor with dry sorbent. The main features of CFBA are high sorbent/gas mixing ratios, excellent heat and mass transfer characteristics, and the ability to recycle partially utilized sorbent. Subsequently, higher SO{sub 2} removal efficiencies with higher overall sorbent utilization can be realized compared with other dry sorbent injection scrubber systems.

  5. Process Analytical Technology and On-Line Spectroscopic Measurements of Chemical Meat Quality

    DEFF Research Database (Denmark)

    Sørensen, Klavs Martin

    This thesis deals with process analytical technology and how it can be implemented in the meat industry through on-line grading of chemical meat quality. The focus will be on two applications, namely the rapid quality control of fat quality and the development of a method for on-line detection...... of boar taint. The chemical makeup of fat has a large effect on meat cut quality. Fat quality has traditionally been determined by methylation of a tissue sample followed by chromatography on a GC-MS system, elucidating the composition of the individual fatty acids. As this procedure typically takes far...... on surgical castration will be in effect starting 2018. With the ban, the risk of meat products with the malodorous taint reaching the consumer is highly increased, and thus, detection of boar taint is a necessity. No current on-line detection system is available; the only alternative is chemical extraction...

  6. Determination of 18 Organic Phosphorus and Pyrthroid Pesticides in Dried Vegetables using Solid-phase Extraction and On-line Gel Permeation Chromatography-GC/MS%固相萃取-在线凝胶渗透色谱-气相色谱质谱联用测定蔬菜干制品中的18种有机磷和拟除虫菊酯残留

    Institute of Scientific and Technical Information of China (English)

    薛丽; 钟艳梅

    2012-01-01

    建立了蔬菜干制品中18种有机磷农药和拟除虫菊酯农药残留的在线凝胶渗透色谱-气相色谱/质谱(GPC-GC/MS)分析方法.样品以乙腈为提取剂超声波高速匀浆提取,提取液经ENVI-Carb固相萃取柱净化,除去样品中大部分的色素等干扰基质,再经在线GPC进一步净化除去大分子干扰物质,有效降低了样品基质带来的背景干扰.采用外标法定量,在质量浓度为0.02 mg/kg~0.5mg/kg有良好的线性关系,加标水平为0.4 mg/kg时,18种农药的回收率基本都在80%~130%,相对标准偏差小于10%,检出限为0.001mg/kg~0.026 mg/kg.经实验证明,该方法是一种快速,准确,灵敏度高的同时检测梅菜干中多种农药残留的检测方法.%An on-line gel permeation chromatography-GC/MS analytical method was developed for the determination of 18 organic phosphorus pesticide and pyrethroid pesticides in dried vegetables.The samples were extracted with acetonitrile by means of ultrasonic high-speed homogenization, cleaned up by an ENVI-Carb solid phase extraction column to remove pigment in the sample and analyzed by on-line gel permeation chromatography-GC/MS. All the compounds demonstrated good linear relationship in the range of 0.02-0.5 mg/kg. The recoveries for the most of pestive standards of 0.4 mg/kg were 80%-130% and the relative standard deviations were less than 10%. The limits of detection were from 0.001 mg/kg to 0.026 mg/kg. The method was rapid, accurate and highly sensitive, which can be used for the simultaneous determination of pesticide residues in dried vegetables.

  7. Carbon Dioxide Capture from Flue Gas Using Dry Regenerable Sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Thomas Nelson; David Green; Paul Box; Raghubir Gupta; Gennar Henningsen

    2007-06-30

    Regenerable sorbents based on sodium carbonate (Na{sub 2}CO{sub 3}) can be used to separate carbon dioxide (CO{sub 2}) from coal-fired power plant flue gas. Upon thermal regeneration and condensation of water vapor, CO{sub 2} is released in a concentrated form that is suitable for reuse or sequestration. During the research project described in this report, the technical feasibility and economic viability of a thermal-swing CO{sub 2} separation process based on dry, regenerable, carbonate sorbents was confirmed. This process was designated as RTI's Dry Carbonate Process. RTI tested the Dry Carbonate Process through various research phases including thermogravimetric analysis (TGA); bench-scale fixed-bed, bench-scale fluidized-bed, bench-scale co-current downflow reactor testing; pilot-scale entrained-bed testing; and bench-scale demonstration testing with actual coal-fired flue gas. All phases of testing showed the feasibility of the process to capture greater than 90% of the CO{sub 2} present in coal-fired flue gas. Attrition-resistant sorbents were developed, and these sorbents were found to retain their CO{sub 2} removal activity through multiple cycles of adsorption and regeneration. The sodium carbonate-based sorbents developed by RTI react with CO{sub 2} and water vapor at temperatures below 80 C to form sodium bicarbonate (NaHCO3) and/or Wegscheider's salt. This reaction is reversed at temperatures greater than 120 C to release an equimolar mixture of CO{sub 2} and water vapor. After condensation of the water, a pure CO{sub 2} stream can be obtained. TGA testing showed that the Na{sub 2}CO3 sorbents react irreversibly with sulfur dioxide (SO{sub 2}) and hydrogen chloride (HCl) (at the operating conditions for this process). Trace levels of these contaminants are expected to be present in desulfurized flue gas. The sorbents did not collect detectable quantities of mercury (Hg). A process was designed for the Na{sub 2}CO{sub 3}-based sorbent that

  8. Developments in coupled solid-phase extraction-capillary electrophoresis 2013-2015.

    Science.gov (United States)

    Ramautar, Rawi; Somsen, Govert W; de Jong, Gerhardus J

    2016-01-01

    An overview of the design and application of coupled solid-phase extraction-capillary electrophoresis (SPE-CE) systems reported in the literature between July 2013 and June 2015 is provided in this paper. The present article is a continuation of our previous review papers on this topic which covered the time period 2000-2013 (Electrophoresis 2008, 29, 108-128; Electrophoresis 2010, 31, 44-54; Electrophoresis 2012, 33, 243-250; Electrophoresis 2014, 35, 128-137). The use of in-line and on-line SPE-CE approaches is treated and outlined in this review. Recent advancements, such as, for example, the use of aptamers as affinity material for in-line SPE-CE, the use of a bead string design for in-line fritless SPE-CE, and new interfacing techniques for the on-line coupling of SPE to CE, are outlined. Selected examples demonstrate the applicability of the coupled SPE-CE systems for biomedical, pharmaceutical, environmental, and food studies. A complete overview of the recent SPE-CE studies is given in table format, providing information on sample type, SPE sorbent, coupling mode, detection mode, and LOD. Finally, some general conclusions and perspectives are provided.

  9. On-line sample-pre-treatment schemes for trace-level determinations of metals by coupling flow injection or sequential injection with ICP-MS

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2003-01-01

    for on-line matrix separation and pre-concentration of trace levels of metals with detection by ICP-MS. It highlights some of the frequently applied on-line, sample-pre-treatment schemes, including solid phase extraction (SPE), on-wall molecular sorption and precipitate/(co)-precipitate retention using...... a polytetrafluoroethylene (PTFE) knotted reactor (KR), solvent extraction-back extraction and hydride/vapor generation. It also addresses a novel, robust approach, whereby the protocol of SI-LOV-bead injection (BI) on-line separation and pre-concentration of ultra-trace levels of metals by a renewable microcolumn...

  10. Robust on-line monitoring of biogas processes; Robusta maettekniker on-line foer optimerad biogasproduktion

    Energy Technology Data Exchange (ETDEWEB)

    Nordberg, Aake; Hansson, Mikael; Kanerot, Mija; Krozer, Anatol; Loefving, Bjoern; Sahlin, Eskil

    2010-03-15

    Although demand for biomethane in Sweden is higher than ever, many Swedish codigestion plants are presently operated below their designed capacity. Efforts must be taken to increase the loading rate and guarantee stable operation and high availability of the plants. There are currently no commercial systems for on-line monitoring, and due to the characteristics of the material, including corrosion and tearing, robust applications have to be developed. The objective of this project was to identify and study different monitoring technologies with potential for on-line monitoring of both substrate mixtures and anaerobic digester content. Based on the prerequisites and demands at Boraas Energi och Miljoe AB's (BEMAB, the municipal energy and waste utility in the city of Boraas, Sweden) biogas plant, the extent of the problems, measurement variables and possible ways of managing these issues have been identified and prioritized. The substrate mixtures in question have a high viscosity and are inhomogeneous with variation in composition, which calls for further homogenization, dilution and filtration to achieve high precision in the necessary analyses. Studies of using different mixers and mills showed that the particle size (800 mum) needed for on-line COD measurement could not be achieved. The problem of homogenization can be avoided if indirect measurement methods are used. Laboratory tests with NIR (near-infra red spectroscopy) showed that VS can be predicted (R2=0,78) in the interval of 2-9% VS. Furthermore, impedance can give a measurement of soluble components. However, impedance is not sensitive enough to give a good measurement of total TS. Microwave technology was installed at the production plant and showed a faster response to changes in TS than the existing TS-sensor. However, due to technical problems, the evaluation only could be done during a limited period of ten days. BEMAB will continue the measurements and evaluation of the instrument. The

  11. The role of humic acids and biochar as specific sorbents of pesticides in soil

    Science.gov (United States)

    Ćwieląg-Piasecka, Irmina; Dębicka, Magdalena; Medyńska-Jureszek, Agnieszka; Weber, Jerzy; Jamroz, Elżbieta

    2017-04-01

    Pesticides are widely used in agriculture to prevent or control different pests and increase yield as well as products quality. Despite of the strict regulations concerning sustainable use of plant protection products, their residues are very often present in soil. Depending on their chemical and physical properties, they undergo various transformations in the soil. This results in their retention on different sorbents, degradation by microorganisms or leaching to the groundwater. Biochar is a carbon-rich byproduct of thermal biomass conversion, and due to its high sorption properties can be an efficient sorbent for pesticides in soil. The aim of the research was to compare the effect of two types of organic sorbents - humic acids (HA) and biochar (BC) - in sorption-desorption processes of different pesticides, which residues are commonly present in arable soils and thus are potentially harmful for the environment. The humic acids were extracted from topsoil horizon of arable cambisoil derived from loam (Lower Silesia, Poland) by Shnitzer's method, then purified using XAD resin and freeze-dried. Biochar was produced from wheat straw in gasification process at 550˚C, remaining 30 minutes in the reactor. Investigated pesticides belong to three different chemical classes: carbamates (carbaryl and carbofuran), phenoxyacetic acids (2,4-D and MCPA) and aniline derivatives (metolachlor), and are active substances of commonly used plant protection products in agriculture. To obtain the experimental goal the sorption experiment was conducted. To the investigated organic matter samples (HA or BC) aliquots of pesticides solutions in 10M CaCl2 were added and the mixtures were shaken for 24h. Afterwards the samples were centrifuged and supernatants analyzed by LC-MS/MS for the pesticides content. After that the same samples were refilled with CaCl2 and analyzed in the same way for desorption studies. Humic acids exhibited strong affinity for the ionic substances (2,4-D, MCPA

  12. Comparing the Hierarchy of Keywords in On-Line News Portals

    Science.gov (United States)

    Tibély, Gergely; Sousa-Rodrigues, David; Pollner, Péter; Palla, Gergely

    2016-01-01

    Hierarchical organization is prevalent in networks representing a wide range of systems in nature and society. An important example is given by the tag hierarchies extracted from large on-line data repositories such as scientific publication archives, file sharing portals, blogs, on-line news portals, etc. The tagging of the stored objects with informative keywords in such repositories has become very common, and in most cases the tags on a given item are free words chosen by the authors independently. Therefore, the relations among keywords appearing in an on-line data repository are unknown in general. However, in most cases the topics and concepts described by these keywords are forming a latent hierarchy, with the more general topics and categories at the top, and more specialized ones at the bottom. There are several algorithms available for deducing this hierarchy from the statistical features of the keywords. In the present work we apply a recent, co-occurrence-based tag hierarchy extraction method to sets of keywords obtained from four different on-line news portals. The resulting hierarchies show substantial differences not just in the topics rendered as important (being at the top of the hierarchy) or of less interest (categorized low in the hierarchy), but also in the underlying network structure. This reveals discrepancies between the plausible keyword association frameworks in the studied news portals. PMID:27802319

  13. Comparing the Hierarchy of Keywords in On-Line News Portals.

    Science.gov (United States)

    Tibély, Gergely; Sousa-Rodrigues, David; Pollner, Péter; Palla, Gergely

    2016-01-01

    Hierarchical organization is prevalent in networks representing a wide range of systems in nature and society. An important example is given by the tag hierarchies extracted from large on-line data repositories such as scientific publication archives, file sharing portals, blogs, on-line news portals, etc. The tagging of the stored objects with informative keywords in such repositories has become very common, and in most cases the tags on a given item are free words chosen by the authors independently. Therefore, the relations among keywords appearing in an on-line data repository are unknown in general. However, in most cases the topics and concepts described by these keywords are forming a latent hierarchy, with the more general topics and categories at the top, and more specialized ones at the bottom. There are several algorithms available for deducing this hierarchy from the statistical features of the keywords. In the present work we apply a recent, co-occurrence-based tag hierarchy extraction method to sets of keywords obtained from four different on-line news portals. The resulting hierarchies show substantial differences not just in the topics rendered as important (being at the top of the hierarchy) or of less interest (categorized low in the hierarchy), but also in the underlying network structure. This reveals discrepancies between the plausible keyword association frameworks in the studied news portals.

  14. CAN SORBENT-BASED GAS PHASE AIR CLEANING FOR VOCS SUBSTITUTE FOR VENTILATION IN COMMERCIAL BUILDINGS?

    Energy Technology Data Exchange (ETDEWEB)

    Fisk, William; Fisk, William J.

    2007-08-01

    This paper reviews current knowledge about the suitability of sorbent-based air cleaning for removing volatile organic compounds (VOCs) from the air in commercial buildings, as needed to enable reductions in ventilation rates and associated energy savings. The principles of sorbent air cleaning are introduced, criteria are suggested for sorbent systems that can counteract indoor VOC concentration increases from reduced ventilation, major findings from research on sorbent performance for this application are summarized, and related priority research needs are identified. Major conclusions include: sorbent systems can remove a broad range of VOCs with moderate to high efficiency, sorbent technologies perform effectively when challenged with VOCs at the low concentrations present indoors, and there is a large uncertainty about the lifetime and associated costs of sorbent air cleaning systems when used in commercial buildings for indoor VOC control. Suggested priority research includes: experiments to determine sorbent system VOC removal efficiencies and lifetimes considering the broad range and low concentration of VOCs indoors; evaluations of in-situ regeneration of sorbents; and an updated analysis of the cost of sorbent air cleaning relative to the cost of ventilation.

  15. Characteristics and reactivity of rapidly hydrated sorbent for semidry flue gas desulfurization.

    Science.gov (United States)

    Zhang, Jie; You, Changfu; Zhao, Suwei; Chen, Changhe; Qi, Haiying

    2008-03-01

    Semidry flue gas desulfurization with a rapidly hydrated sorbent was studied in a pilot-scale circulating fluidized bed (CFB) experimental facility. The desulfurization efficiency was measured for various operating parameters, including the sorbent recirculation rate and the water spray method. The experimental results show that the desulfurization efficiencies of the rapidly hydrated sorbent were 1.5-3.0 times higher than a commonly used industrial sorbent for calcium to sulfur molar ratios from 1.2 to 3.0, mainly due to the higher specific surface area and pore volume. The Ca(OH)2 content in the cyclone separator ash was about 2.9% for the rapidly hydrated sorbent and was about 0.1% for the commonly used industrial sorbent, due to the different adhesion between the fine Ca(OH)2 particles and the fly ash particles, and the low cyclone separation efficiency for the fine Ca(OH)2 particles that fell off the sorbent particles. Therefore the actual recirculation rates of the active sorbent with Ca(OH)2 particles were higher for the rapidly hydrated sorbent, which also contributed to the higher desulfurization efficiency. The high fly ash content in the rapidly hydrated sorbent resulted in good operating stability. The desulfurization efficiency with upstream water spray was 10-15% higher than that with downstream water spray.

  16. Development of low-cost amine-enriched solid sorbent for CO2 capture.

    Science.gov (United States)

    Bachelor, Thuy Thi Nguyen; Toochinda, Pisanu

    2012-12-01

    CO2 capture amine-enriched solid sorbent using agricultural wastes, such as bagasse, or industrial wastes, such as mullite, as support materials could provide efficient alternative CO2 reduction due to their low cost and ability to shape into many forms. These amine-enriched solid sorbents were prepared by treatment with monoethanolamine (MEA), diethanolamine, piperazine (PZ), 2-(2-aminoethyl-amino) ethanol (AEEA) and mixtures of these amines. The performance of amine-enriched solid sorbents with various amine compositions was studied in a tubular column at 1 atm and an adsorption temperature of 303 K. The CO2 capture capacities of the amine-enriched solid sorbents were determined by gas chromatography at a desorption temperature of 393 K. Amine-enriched solid sorbents in this study exhibited high performance CO2 capture. The MEA-PZ-enriched solid sorbent does have the highest CO2 capture performance of the amine-enriched bagasse support-based sorbents, and the results indicate that PZ is the most effective promoter in this study. The CO2 capture performances of solid sorbents in this study were compared with commercial solid sorbents. This study could lead to the development of low-cost solid sorbents for CO2 capture that can be used in many industrial applications.

  17. Regenerable MgO-based sorbents for high-temperature CO{sub 2} removal from syngas: 1. Sorbent development, evaluation, and reaction modeling

    Energy Technology Data Exchange (ETDEWEB)

    Armin Hassanzadeh; Javad Abbasian [Pyrophase Inc., Chicago, IL (United States)

    2010-06-15

    Highly reactive and mechanically strong low-cost regenerable MgO-based sorbents were prepared by modification of dolomite which involved partial calcinations followed by impregnation with a potassium-based salt. The sorbents are capable of removing CO{sub 2} from gasification-based processes such as Integrated Gasification Combined Cycle (IGCC). The sorbents have high reactivity and good capacity toward CO{sub 2} absorption in the temperature range of 300-450{sup o}C at 20 atm. and can be easily regenerated at 500{sup o}C. The reaction appears to be first order with respect to CO{sub 2} concentration with an activation energy of 44 kJ/mol. The reactivity and the absorption capacity of the sorbents increase with increasing temperature, as long as the partial pressure of CO{sub 2} is above the equilibrium value for sorbent carbonation. The reactivity of the sorbents appears to improve in the presence of steam, which is likely due to the increase in the BET surface area and the porosity of the sorbent. A two-zone expanding grain model, consisting of a high-reactivity outer shell and a low-reactivity inner core is shown to provide an excellent fit to the TGA experimental data on sorbent carbonation at various operating conditions. 31 refs., 16 figs.,3 tabs.

  18. On-line monitoring of pharmaceutical production processes using Hidden Markov Model.

    Science.gov (United States)

    Zhang, Hui; Jiang, Zhuangde; Pi, J Y; Xu, H K; Du, R

    2009-04-01

    This article presents a new method for on-line monitoring of pharmaceutical production process, especially the powder blending process. The new method consists of two parts: extracting features from the Near Infrared (NIR) spectroscopy signals and recognizing patterns from the features. Features are extracted from spectra by using Partial Least Squares method (PLS). The pattern recognition is done by using Hidden Markov Model (HMM). A series of experiments are conducted to evaluate the effectiveness of this new method. In the experiments, wheat powder and corn powder are blended together at a set concentration. The proposed method can effectively detect the blending uniformity (the success rate is 99.6%). In comparison to the conventional Moving Block of Standard Deviation (MBSD), the proposed method has a number of advantages, including higher reliability, higher robustness and more transparent decision making. It can be used for effective on-line monitoring of pharmaceutical production processes.

  19. Good control practices underlined by an on-line fuzzy control database

    Directory of Open Access Journals (Sweden)

    Alonso, M. V.

    1994-04-01

    Full Text Available In the olive oil trade, control systems that automate extraction processes, cutting production costs and increasing processing capacity without losing quality, are always desirable. The database structure of an on-line fuzzy control of centrifugation systems and the algorithms used to attain the best control conditions are analysed. Good control practices are suggested to obtain virgin olive oil of prime quality.

    In the olive oil trade, control systems that automate extraction processes, cutting production costs and increasing processing capacity without losing quality, are always desirable. The database structure of an on-line fuzzy control of centrifugation systems and the algorithms used to attain the best control conditions are analysed. Good control practices are suggested to obtain virgin olive oil of prime quality.

  20. On-line sample treatment and FT-IR determination of doxylamine succinate in pharmaceuticals.

    Science.gov (United States)

    Ventura-Gayete, Josep F; de la Guardia, Miguel; Garrigues, Salvador

    2006-12-15

    A low solvent consumption method for Fourier transform infrared spectroscopy (FT-IR) determination of doxylamine succinate in pharmaceuticals has been developed. The analyte was continuous and selectively extracted with a 13% (v/v) ethanol:chloroform solvent mixture, recirculating the solvent through the sample and monitoring the process by FT-IR. Doxylamine succinate was determined by on-line standard addition measuring the peak area in the regions 1730-1710 and 1485-1462cm(-1) corrected with a two-point baseline established between 2000 and 1800cm(-1). This new method implies low volumes of chloroformic solvent mixture, only 2.6mL per sample, in front of classical batch FT-IR methods, improving analytical efficiency and reducing waste generation. The on-line extraction and standard addition determination of doxylamine succinate allowed a throughput of 10h(-1).

  1. DOE-EPRI On-Line Monitoring Implementation Guidelines

    Energy Technology Data Exchange (ETDEWEB)

    E. Davis, R. Bickford

    2003-01-02

    Industry and EPRI experience at several plants has shown on-line monitoring to be very effective in identifying out-of-calibration instrument channels or indications of equipment-degradation problems. The EPRI implementation project for on-line monitoring has demonstrated the feasability of on-line monitoring at several participating nuclear plants. The results have been very enouraging, and substantial progress is anticipated in the coming years.

  2. Poss On-line (Personalisation of Self-Service Solutions across On-line platforms)

    DEFF Research Database (Denmark)

    Nielsen, Janni; Nielsen, Lene; Jespersen, Mikkel

    2005-01-01

    The project on Personalisation of Self-service Solutions across On-line Platforms (POSS ON-LINE) focuses on users, clients, and self-service solutions. It is based on the understanding that clients and users are different and have different goals, and that self-service takes place in different co...... at the process of development. However, we lack methods to predict user behaviour without having to deal with huge amounts of data and data from both quantitative data as well as life world observations are required....... the client and the user. The system gathers data about the user, which enables the client to push information to the user. Personalisation enables graphic user interface design that is personalised and relevant to the individual user and invites the user to get access to information with less strain....... Personalisation of self-service solutions is promising and IT companies are experiencing an increase in the clients' demands. At the same time the development of solutions moves within a shorter and shorter time span. Hence the process of innovations is paced and there is an increasing need of new ways of looking...

  3. Determination of glyphosate, glufosinate and aminomethylphonic acid residues in tea by liquid chromatography-tandem mass spectrometry using multi-walled carbon nanotubes as dispersive solid-phase extraction sorbent%多壁碳纳米管分散固相萃取-液质联用技术测定茶叶中草甘膦、草铵膦、氨甲基膦酸残留量

    Institute of Scientific and Technical Information of China (English)

    冯月超; 马立利; 贾丽; 张春梅; 刘艳; 范筱京; 潘灿平

    2014-01-01

    Objective An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) analysis method was established for simultaneous determination of glyphosate, glufosinate and aminomethyl-phonic acid (AMPA) in tea. Methods The sample was extracted with water, and cleaned up by multi-walled carbon nanotubes(MWCNTS)and primary-secondary amine(PSA)as dispersive solid-phase extraction sorbent, then derived using fluorenyl methyl chloroformate(FMOC-Cl). The derivatives were separated by ACQUITY UPLC BEH C18 column, using acetonitrile and 4 mmol/L ammonium acetate as the mobile phase. The identifi-cation and quantification of glyphosate, glufosinate and AMPA were carried out by MS/MS in positive electro-spray ionization(ESI+) and multiple reaction monitoring(MRM) mode, and the quantification analysis was per-formed by external standard method. Results The calibration curve showed a good linearity in the range of 0.1∼1 μg/mL with the correlation coefficient r2> 0.999. The quantification (LOQ) limits were 10 μg/kg. The average recoveries of glyphosate, glufosinate and AMPA spiked at 0.25, 0.50 mg/kg and 1.00 mg/kg levels in green tea were 95%~116%, 98%~118% and 74%~84%, and the relative standard deviations (RSD, n=6) were lower than 6.79%. Conclusion This method is simple, effective and sensitive, and it is suitable for the deter-mination and confirmation of glyphosate, glufosinate and AMPA in tea.%目的:建立茶叶中草甘膦、草铵膦和氨甲基膦酸残留量的超高效液相色谱串联质谱分析方法。方法样品经水提取后采用分散固相萃取技术,以多壁碳纳米管(MWCNTS)和N-丙基乙二胺键合固相吸附剂(PSA)吸附提取液中的杂质,上清液用9-芴基氯甲酸酯(FMOC-Cl)衍生。衍生物用 BEH C18进行分离,以乙腈-4 mmol乙酸铵水溶液为流动相,电喷雾正离子模式电离(ESI+),多反应监测模式检测(MRM),外标法定量。结果方法的线性范围是0.1∼1μg/mL,相关系数大于0.999,

  4. CARBON DIOXIDE CAPTURE FROM FLUE GAS USING DRY REGENERABLE SORBENTS

    Energy Technology Data Exchange (ETDEWEB)

    David A. Green; Brian S. Turk; Raghubir Gupta; Alejandro Lopez-Ortiz

    2001-01-01

    Four grades of sodium bicarbonate and two grades of trona were characterized in terms of particle size distribution, surface area, pore size distribution, and attrition. Surface area and pore size distribution determinations were conducted after calcination of the materials. The sorbent materials were subjected to thermogravimetric testing to determine comparative rates and extent of calcination (in inert gas) and sorption (in a simulated coal combustion flue gas mixture). Selected materials were exposed to five calcination/sorption cycles and showed no decrease in either sorption capacity or sorption rate. Process simulations were conducted involving different heat recovery schemes. The process is thermodynamically feasible. The sodium-based materials appear to have suitable physical properties for use as regenerable sorbents and, based on thermogravimetric testing, are likely to have sorption and calcination rates that are rapid enough to be of interest in full-scale carbon sequestration processes.

  5. On-Line Bunch Tomography and Beam Modelling for MTE Commissioning

    CERN Document Server

    Rothe, Johannes

    2015-01-01

    For my stay as a CERN Summer Student from June 29 to September 25, 2015, I worked with Guido Sterbini of the Accelerator and Beam Physics group. I was based in the CERN Control Center (CCC) at the Prevessin Site, and supported the ongoing beam commissioning work on Multi-Turn Extraction through the development of on-line monitoring and control tools for the Proton Synchrotron (PS) machine.

  6. Simple and rapid determination of phthalates using microextraction by packed sorbent and gas chromatography with mass spectrometry quantification in cold drink and cosmetic samples.

    Science.gov (United States)

    Kaur, Ramandeep; Heena; Kaur, Ripneel; Rani, Susheela; Malik, Ashok Kumar

    2016-03-01

    A simple and rapid method using microextraction by packed sorbent coupled with gas chromatography and mass spectrometry has been developed for the analysis of five phthalates, namely, diethyl phthalate, benzyl-n-butyl phthalate, dicyclohexyl phthalate, di-n-butyl phthalate, and di-n-propyl phthalate, in cold drink and cosmetic samples. The various parameters that influence the microextraction by packed sorbent performance such as extraction cycle (extract-discard), type and amount of solvent, washing solvent, and pH have been studied. The optimal conditions of microextraction using C18 as the packed sorbent were 15 extraction cycles with water as washing solvent and 3 × 10 μL of ethyl acetate as the eluting solvent. Chromatographic separation was also optimized for injection temperature, flow rate, ion source, interface temperature, column temperature gradient and mass spectrometry was evaluated using the scan and selected ion monitoring data acquisition mode. Satisfactory results were obtained in terms of linearity with R(2) >0.9992 within the established concentration range. The limit of detection was 0.003-0.015 ng/mL, and the limit of quantification was 0.009-0.049 ng/mL. The recoveries were in the range of 92.35-98.90% for cold drink, 88.23-169.20% for perfume, and 88.90-184.40% for cream. Analysis by microextraction by packed sorbent promises to be a rapid method for the determination of these phthalates in cold drink and cosmetic samples, reducing the amount of sample, solvent, time and cost.

  7. Durable zinc ferrite sorbent pellets for hot coal gas desulfurization

    Science.gov (United States)

    Jha, Mahesh C.; Blandon, Antonio E.; Hepworth, Malcolm T.

    1988-01-01

    Durable, porous sulfur sorbents useful in removing hydrogen sulfide from hot coal gas are prepared by water pelletizing a mixture of fine zinc oxide and fine iron oxide with inorganic and organic binders and small amounts of activators such as sodium carbonate and molybdenite; the pellets are dried and then indurated at a high temperature, e.g., 1800.degree. C., for a time sufficient to produce crush-resistant pellets.

  8. Polymer sorbent with the properties of an artificial cholesterol receptor

    Science.gov (United States)

    Polyakova, I. V.; Ezhova, N. M.; Osipenko, A. A.; Pisarev, O. A.

    2015-02-01

    A cholesterol-imprinted polymer sorbent and the corresponding reticular control copolymer were synthesized from hydroxyethyl methacrylate and ethyleneglycol dimethacrylate. The sorption isotherms of cholesterol were analyzed using the generalized Langmuir and Freundlich equations. In the case of the imprinted reticular polymer, cholesterol sorption occurred on the energetically homogeneous binding centers, forming one monolayer, while the nonspecific sorption of cholesterol on the control copolymer occurred with energetically nonhomogeneous binding of the sorbate and depended on the physicochemical conditions of sorption.

  9. Pilot plant tests of Z-Sorb{trademark} sorbent

    Energy Technology Data Exchange (ETDEWEB)

    Greenwood, G.J.; Khare, G.P.; Kubicek, D.H.; Delzer, G.A.; Kinsinger, D.L.

    1995-06-01

    The objective of this work is to determine the long-term chemical reactivity and mechanical durability of Phillips Petroleum Company`s (PPCo`s) proprietary Z-Sorb{trademark} sorbent. Materials developed for fixed-, moving- and fluid bed desulfurization of coal derived gases at high pressure (5-20 atm) and moderate operating temperatures (600-1000{degrees}F) will be discussed.

  10. The effect of preparation of biogenic sorbent on zinc sorption

    Directory of Open Access Journals (Sweden)

    Jana Jenčárová

    2011-12-01

    Full Text Available The aim of this study is to prepare biogenic sulphides by using bacteria for the removal of zinc cations from their solutions. Theproduction was realized in a bioreactor under anaerobic conditions at 30 °C. Sorbents were prepared by sulphate-reducing bacteria indifferent nutrient medium modifications, under two modes of bacteria cultivation. Created precipitates of iron sulphides were removedfrom the liquid phase of the cultivation medium by filtration, dried and used for the sorption experiments.

  11. Sorbents for CO2 capture from high carbon fly ashes.

    Science.gov (United States)

    Maroto-Valer, M Mercedes; Lu, Zhe; Zhang, Yinzhi; Tang, Zhong

    2008-11-01

    Fly ashes with high-unburned-carbon content, referred to as fly ash carbons, are an increasing problem for the utility industry, since they cannot be marketed as a cement extender and, therefore, have to be disposed. Previous work has explored the potential development of amine-enriched fly ash carbons for CO2 capture. However, their performance was lower than that of commercially available sorbents, probably because the samples investigated were not activated prior to impregnation and, therefore, had a very low surface area. Accordingly, the work described here focuses on the development of activated fly ash derived sorbents for CO2 capture. The samples were steam activated at 850 degrees C, resulting in a significant increase of the surface area (1075 m2/g). The activated samples were impregnated with different amine compounds, and the resultant samples were tested for CO2 capture at different temperatures. The CO2 adsorption of the parent and activated samples is typical of a physical adsorption process. The impregnation process results in a decrease of the surface areas, indicating a blocking of the porosity. The highest adsorption capacity at 30 and 70 degrees C for the amine impregnated activated carbons was probably due to a combination of physical adsorption inherent from the parent sample and chemical adsorption of the loaded amine groups. The CO2 adsorption capacities for the activated amine impregnated samples are higher than those previously published for fly ash carbons without activation (68.6 vs. 45 mg CO2/g sorbent).

  12. Enhanced capture of elemental mercury by bamboo-based sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Tan, Zengqiang [State Key Laboratory of Coal Combustion, Huazhong University of Science and Technology, Wuhan, Hubei 430074 (China); Xiang, Jun, E-mail: xiangjun@mail.hust.edu.cn [State Key Laboratory of Coal Combustion, Huazhong University of Science and Technology, Wuhan, Hubei 430074 (China); Su, Sheng, E-mail: susheng_sklcc@hotmail.com [State Key Laboratory of Coal Combustion, Huazhong University of Science and Technology, Wuhan, Hubei 430074 (China); Zeng, Hancai; Zhou, Changsong; Sun, Lushi; Hu, Song; Qiu, Jianrong [State Key Laboratory of Coal Combustion, Huazhong University of Science and Technology, Wuhan, Hubei 430074 (China)

    2012-11-15

    Highlights: Black-Right-Pointing-Pointer The KI-modified BC has excellent capacity for elemental mercury removal. Black-Right-Pointing-Pointer The chemisorption plays a dominant role for the modified BC materials. Black-Right-Pointing-Pointer The BC-I has strong anti-poisoning ability with the presence of NO or SO{sub 2}. - Abstract: To develop cost-effective sorbent for gas-phase elemental mercury removal, the bamboo charcoal (BC) produced from renewable bamboo and KI modified BC (BC-I) were used for elemental mercury removal. The effect of NO, SO{sub 2} on gas-phase Hg{sup 0} adsorption by KI modified BC was evaluated on a fixed bed reactor using an online mercury analyzer. BET surface area analysis, temperature programmed desorption (TPD) and X-ray photoelectron spectroscopy (XPS) were used to determine the pore structure and surface chemistry of the sorbents. The results show that KI impregnation reduced the sorbents' BET surface area and total pore volume compared with that of the original BC. But the BC-I has excellent adsorption capacity for elemental mercury at a relatively higher temperature of 140 Degree-Sign C and 180 Degree-Sign C. The presence of NO or SO{sub 2} could inhibit Hg{sup 0} capture, but BC-I has strong anti-poisoning ability. The specific reaction mechanism has been further analyzed.

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

    KAUST Repository

    Bhandari, Dhaval A.

    2013-05-01

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

  14. Simultaneous extraction and separation of flavonols and flavones from Chamaecyparis obtusa by multi-phase extraction using an ionic liquid-modified microsphere polymer.

    Science.gov (United States)

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

    2012-01-01

    Flavonols and flavones, especially quercitrin, myricetin and amentoflavone, are the main anti-bacterial and anti-cancer compounds in Chamaecyparis obtuse. Multi-phase extraction is a new method that can extract and separate target compounds simultaneously. An amino ionic liquid immobilised microsphere polymer was used as a multi-phase extraction sorbent to extract and separate quercitrin, myricetin and amentoflavone from Chamaecyparis obtusa. The sorbent and Chamaecyparis obtusa powder were packed into a single cartridge. Using a fixed volume of methanol with five repetitions, the target compounds were extracted from the powder to the sorbent. The sorbent was then washed with n-hexane to remove any interfering species and the target compounds were eluted sequentially using water, methanol and methanol containing 1% acetic acid (vol.). Under the optimised conditions, 0.45 mg/g of quercitrin, 0.18 mg/g of myricetin and 0.12 mg/g of amentoflavone from 2.0 g of powder were obtained by multi-phase extraction using 0.3 g of sorbent. The method described has a low deviation error, requires a small amount of solvent and is highly selective and reproducible. Copyright © 2012 John Wiley & Sons, Ltd.

  15. New ZnO-Based Regenerable Sulfur Sorbents for Fluid-Bed/Transport Reactor Applications

    Energy Technology Data Exchange (ETDEWEB)

    Slimane, R.B.; Lau, F.S.; Abbasian, J.; Ho, K.H.

    2002-09-19

    The overall objective of the ongoing sorbent development work at GTI is the advancement to the demonstration stage of a promising ZnO-TiO2 sulfur sorbent that has been developed under DCCA/ICCI and DOE/NETL sponsorship. This regenerable sorbent has been shown to possess an exceptional combination of excellent chemical reactivity, high effective capacity for sulfur absorption, high resistance to attrition, and regenerability at temperatures lower than required by typical zinc titanates.

  16. Peat hybrid sorbents for treatment of wastewaters and remediation of polluted environment

    Science.gov (United States)

    Klavins, Maris; Burlakovs, Juris; Robalds, Artis; Ansone-Bertina, Linda

    2015-04-01

    For remediation of soils and purification of polluted waters, wastewaters, sorbents might be considered as an prospective group of materials and amongst them peat have a special role due to low cost, biodegradability, high number of functional groups, well developed surface area and combination of hydrophilic/hydrophobic structural elements. Peat as sorbent have good application potential for removal of trace metals, and we have demonstrated peat sorption capacities, sorption kinetics, thermodynamics in respect to metals with different valencies - Tl(I), Cu(II), Cr(III). However peat sorption capacity in respect to nonmetallic (anionic species) elements is low. Also peat mechanical properties do not support application in large scale column processes. To expand peat application possibilities the approach of biomass based hybrid sorbents has been elaborated. The concept "hybrid sorbent" in our understanding means natural, biomass based sorbent modified, covered with another sorbent material, thus combining two types of sorbent properties, sorbent functionalities, surface properties etc. As the "covering layer" both inorganic substances, mineral phases (iron oxohydroxides, oxyapatite) both organic polymers (using graft polymerization) were used. The obtained sorbents were characterised by their spectral properties, surface area, elemental composition. The obtained hybrid sorbents were tested for sorption of compounds in anionic speciation forms, for example of arsenic, antimony, tellurium and phosphorous compounds in comparison with weakly basic anionites. The highest sorption capacity was observed when peat sorbents modified with iron compounds were used. Sorption of different arsenic speciation forms onto iron-modified peat sorbents was investigated as a function of pH and temperature. It was established that sorption capacity increases with a rise in temperature, and the calculation of sorption process thermodynamic parameters indicates the spontaneity of sorption

  17. Reactivity of Metal Oxide Sorbents for Removal of H{sub 2}S

    Energy Technology Data Exchange (ETDEWEB)

    Kwon, K.C.; Crowe, E.R. [Chemical Engineering Dept., School of Engineering and Architecture, Tuskegee Univ., AL (United States)

    1996-12-31

    Removal of hydrogen sulfide contained in hot coal gases produced from integrated gasification combined cycle power generation systems is required to protect downstream combustion turbines from being corroded with sulfur compounds. Removal of sulfur compounds from hot coal gas products is investigated by using various metal oxide sorbents and membrane separation methods. The main requirements of these metal oxide sorbents are durability and high sulfur loading capacity during absorption-regeneration cycles. In this research, durable metal oxide sorbents were formulated. Reactivity of the formulated metal oxide sorbents with simulated coal gas mixtures was examined to search for an ideal sorbent formulation with a high-sulfur loading capacity suitable for removal of hydrogen sulfide from coal gases. The main objectives of this research are to formulate durable metal oxide sorbents with high-sulfur loading capacity by a physical mixing method, to investigate reaction kinetics on the removal of sulfur compounds from coal gases at high temperature and pressure, to study reaction kinetics on the regeneration of sulfided sorbents, to identify effects of hydrogen partial pressures and moisture on equilibrium/dynamic absorption of hydrogen sulfide into formulated metal oxide sorbents as well as initial reaction rates of H{sub 2}S with formulated metal oxide sorbents, and to evaluate intraparticular diffusivity of H{sub 2}S into formulated sorbents at various reaction conditions. The metal oxide sorbents such as TU-1, TU-19, TU-24, TU-25 and TU-28 were formulated with zinc oxide powder as an active sorbent ingredient, bentonite as a binding material and titanium oxide as a supporting metal oxide.

  18. Adsorption refinement of waste transformer oil using industrial montmorillonite-containing sorbents

    OpenAIRE

    Koval, Е. О.; Bogomolov, М. S.; Mayer, E. А.; Bondaletov, V. G.

    2007-01-01

    The possibilities of adsorption contact refining of waste transformer oil with active montmorillonite-containing sorbents of «Filtrol» series of BASF Catalysts LLC corporation and Zikeevsk М-80 deposit sorbent have been investigated. Usage of F-160 sorbents of «Filtrol» series in the refinement process allows achieving high quality degree of lean transformer oil, permitting its further use in the equipment with operating voltage to 750 kV.

  19. Quantitative Analysis of Cepharanthine in Plasma Based on Semiautomatic Microextraction by Packed Sorbent Combined with Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Camille Desgrouas

    2014-01-01

    Full Text Available The spread of Plasmodium falciparum resistance toward most of the used drugs requires new antimalarial compounds. Taking advantage of the biodiversity, the ethnopharmacological approach opens the way for the discovery and the characterization of potent original molecules. Previous works led to the selection of a bisbenzylisoquinoline, cepharanthine, extracted from Stephania rotunda, which is mainly present in Cambodia. A sensitive and selective liquid chromatography method has been developed for the determination of cepharanthine in mouse plasma. The method involved a semiautomated microextraction by packed sorbent (MEPS using 4 mg of solid phase silica-C8 sorbent. LC separation was performed on a Kinetex XB-C18 column (2.6 µm with a mobile phase of acetonitrile containing formic acid and 10 mM ammonium formate buffer pH 3.5. Data were acquired at 282 nm with a diode array detector. The drug/internal standard peak area ratios were linked via linear relationships to plasma concentrations (75–2,000 ng/mL. Precision was below 5% and accuracy was 99.0–102%. Extraction recovery of cepharanthine was 56–58%. The method was successfully used to determine the pharmacokinetic profile of cepharanthine in healthy and Plasmodium berghei infected mice. The infection did not impact pharmacokinetic parameters of cepharanthine.

  20. Modified biopolymers as sorbents for the removal of naphthenic acids from oil sands process affected water (OSPW).

    Science.gov (United States)

    Arshad, Muhammad; Khosa, M A; Siddique, Tariq; Ullah, Aman

    2016-11-01

    Oil sands operations consume large volumes of water in bitumen extraction process and produce tailings that express pore water to the surface of tailings ponds known as oil sands process-affected water (OSPW). The OSPW is toxic and cannot be released into the environment without treatment. In addition to metals, dissolved solids, dissolved gases, hydrocarbons and polyaromatic compounds etc., OSPW also contains a complex mixture of dissolved organic acids, referred to as naphthenic acids (NAs). The NAs are highly toxic and react with metals to develop highly corrosive functionalities which cause corrosion in the oil sands processing and refining processes. We have chemically modified keratin biopolymer using polyhedral oligomeric silsesquioxanes (POSS) nanocages and goethite dopant to unfold keratinous structure for improving functionality. The untreated neat keratin and two modified sorbents were characterized to investigate structural, morphological, dimensional and thermal properties. These sorbents were then tested for the removal of NAs from OSPW. The NAs were selectively extracted and quantified before and after sorption process. The biosorption capacity (Q), rejection percentage (R%) and isotherm models were studied to investigate NAs removal efficiency of POSS modified keratin biopolymer (PMKB) and goethite modified keratin biopolymer (GMKB) from aliquots of OSPW.

  1. Magnetic sorbents added to soil slurries lower Cr aqueous concentration

    Science.gov (United States)

    Aravantinos, Konstantinos; Isari, Ekavi; Karapanagioti, Hrissi K.; Manariotis, Ioannis D.; Werner, David

    2016-04-01

    Activated carbon (AC) acts as a strong binding agent that lowers the pollutant concentration and, thus its toxicity. Another promising sorbent material in environmental applications is biochar (BC) which is obtained from the incomplete combustion of carbon-rich biomass under oxygen-limited conditions. Both of these materials could be used as soil or sediment amendments that would lower the toxicity in the aqueous phase. A draw back of this technique is that although the pollutant will remain non- bioavailable for many years being sorbed into these sorbents, it actually stays into the system. The objective of this study was (a) to synthesize a magnetic powdered activated carbon (AC/Fe) and magnetic powdered biochar (BC/Fe) produced from a commercial AC sample and BC, respectively and (b) to evaluate the potential use of AC/Fe and BC/Fe to lower Cr concentration that desorb from two soils in their soil slurries. The two soil samples originate from the vicinity of a local metal shop. The BC was produced from olive pomace. The surface area, the pore volume, and the average pore size of each sorbent were determined using gas (N2) adsorption-desorption cycles and the Brunauer, Emmett, and Teller (BET) equation. Isotherms with 30 adsorption and 20 desorption points were conducted at liquid nitrogen temperature (77K). Open surface area and micropore volume were determined using t-plot method and Harkins & Jura equation. For both AC/Fe, surface area measurements resulted in 66% those of corresponding AC. For BC/Fe, the surface area was 82% that of BC. Our previous studies have shown that both AC/Fe and BC/Fe are effective sorbents for mercury in aqueous solutions but with lower sorption capacity compared to the initial materials (50-75% lower). Batch experiments with all sorbent samples and each soil were conducted at room temperature (25oC) in order to compare the sorption properties of the materials. The soil slurries demonstrated low Cr concentrations (10.9 and 14.6

  2. Advanced Utility Mercury-Sorbent Field-Testing Program

    Energy Technology Data Exchange (ETDEWEB)

    Ronald Landreth

    2007-12-31

    This report summarizes the work conducted from September 1, 2003 through December 31, 2007 on the project entitled Advanced Utility Mercury-Sorbent Field-Testing Program. The project covers the testing at the Detroit Edison St. Clair Plant and the Duke Power Cliffside and Buck Stations. The St. Clair Plant used a blend of subbituminous and bituminous coal and controlled the particulate emissions by means of a cold-side ESP. The Duke Power Stations used bituminous coals and controlled their particulate emissions by means of hot-side ESPs. The testing at the Detroit Edison St. Clair Plant demonstrated that mercury sorbents could be used to achieve high mercury removal rates with low injection rates at facilities that burn subbituminous coal. A mercury removal rate of 94% was achieved at an injection rate of 3 lb/MMacf over the thirty day long-term test. Prior to this test, it was believed that the mercury in flue gas of this type would be the most difficult to capture. This is not the case. The testing at the two Duke Power Stations proved that carbon- based mercury sorbents can be used to control the mercury emissions from boilers with hot-side ESPs. It was known that plain PACs did not have any mercury capacity at elevated temperatures but that brominated B-PAC did. The mercury removal rate varies with the operation but it appears that mercury removal rates equal to or greater than 50% are achievable in facilities equipped with hot-side ESPs. As part of the program, both sorbent injection equipment and sorbent production equipment was acquired and operated. This equipment performed very well during this program. In addition, mercury instruments were acquired for this program. These instruments worked well in the flue gas at the St. Clair Plant but not as well in the flue gas at the Duke Power Stations. It is believed that the difference in the amount of oxidized mercury, more at Duke Power, was the difference in instrument performance. Much of the equipment was

  3. ON-LINE PREEMPTIVE SCHEDULING ON UNIFORM MACHINES

    Institute of Scientific and Technical Information of China (English)

    ZHANG Yuzhong; WANG Shouyang; Bo Chen; ZHANG Shuxia

    2001-01-01

    We address the problem of preemptively schedule on-line jobs on arbitrary muniformly related machines with the objective of minimizing the schedule length. We provide the first on-line algorithm for this general problem, and show that the algorithm being the speeds of the m machines.

  4. From Off-line to On-line Handwriting Recognition

    NARCIS (Netherlands)

    Lallican, P.; Viard-Gaudin, C.; Knerr, S.

    2004-01-01

    On-line handwriting includes more information on time order of the writing signal and on the dynamics of the writing process than off-line handwriting. Therefore, on-line recognition systems achieve higher recognition rates. This can be concluded from results reported in the literature, and has been

  5. On-Line and Off-Line Assessment of Metacognition

    Science.gov (United States)

    Saraç, Seda; Karakelle, Sema

    2012-01-01

    The study investigates the interrelationships between different on-line and off-line measures for assessing metacognition. The participants were 47 fifth grade elementary students. Metacognition was assessed through two off-line and two on-line measures. The off-line measures consisted of a teacher rating scale and a self-report questionnaire. The…

  6. On-line characterization of a hybridoma cell culture process.

    Science.gov (United States)

    Zhou, W; Hu, W S

    1994-06-20

    The on-line determination of the physiological state of a cell culture process requires reliable on-line measurements of various parameters and calculations of specific rates from these measurements. The cell concentration of a hybridoma culture was estimated on-line by measuring optical density (OD) with a laser turbidity probe. The oxygen uptake rate (OUR) was determined by monitoring dynamically dissolved oxygen concentration profiles and closing oxygen balances in the culture. The base addition for neutralizing lactate produced by cells was also monitored on-line via a balance. Using OD and OUR measurements, the specific growth and specific oxygen consumption rates were determined on-line. By combining predetermined stoichiometric relationships among oxygen and glucose consumption and lactate production, the specific glucose consumption and lactate production rates were also calculated on-line. Using these on-line measurements and calculations, the hybridoma culture process was characterized on-line by identifying the physiological states. They will also facilitate the implementation of nutrient feeding strategies for fed-batch and perfusion cultures. (c) 1994 John Wiley & Sons, Inc.

  7. On-line optimal control of greenhouse crop cultivation.

    NARCIS (Netherlands)

    Straten, van G.

    1996-01-01

    Thus far, optimal control has primarily been investigated for seasonal crop growth optimization. On-line aspects have received much less attention. The decomposition between long term strategies and on-line control, however, is not trivial. Appreciable losses occur when set-points generated by seaso

  8. On-line optimal control of greenhouse crop cultivation.

    NARCIS (Netherlands)

    Straten, van G.

    1996-01-01

    Thus far, optimal control has primarily been investigated for seasonal crop growth optimization. On-line aspects have received much less attention. The decomposition between long term strategies and on-line control, however, is not trivial. Appreciable losses occur when set-points generated by seaso

  9. Research on using Mineral Sorbents for A Sorption Process in the Environment Contaminated with Petroleum Substances

    Directory of Open Access Journals (Sweden)

    Pijarowski Piotr Marek

    2014-06-01

    Full Text Available A research on diatomite sorbents was carried out to investigate their ability to remove hazardous substances from oil spillages. We used two types of sorbents available on the market with differences in material density and particles size of composition. As sorbents we used Ekoterm oil and unleaded petrol 95 coming from refinery PKN Orlen S.A. Two types of sorbents with similar chemical composition but different granulometric composition were used. They are marked as D1 and C1 samples. The fastest absorbent was C1, but D1 sample was the most absorptive.

  10. Iron blast furnace slag/hydrated lime sorbents for flue gas desulfurization.

    Science.gov (United States)

    Liu, Chiung-Fang; Shih, Shin-Min

    2004-08-15

    Sorbents prepared from iron blast furnace slag (BFS) and hydrated lime (HL) through the hydration process have been studied with the aim to evaluate their reactivities toward SO2 under the conditions prevailing in dry or semidry flue gas desulfurization processes. The BFS/HL sorbents, having large surface areas and pore volumes due to the formation of products of hydration, were highly reactive toward SO2, as compared with hydrated lime alone (0.24 in Ca utilization). The sorbent reactivity increased as the slurrying temperature and time increased and as the particle size of BFS decreased; the effects of the liquid/solid ratio and the sorbent drying conditions were negligible. The structural properties and the reactivity of sorbent were markedly affected by the BFS/HL ratio; the sorbent with 30/70 ratio had the highest 1 h utilization of Ca, 0.70, and SO2 capture, 0.45 g SO2/g sorbent. The reactivity of a sorbent was related to its initial specific surface area (Sg0) and molar content of Ca (M(-1)); the 1 h utilization of Ca increased almost linearly with increasing Sg0/M. The results of this study are useful to the preparation of BFS/HL sorbents with high reactivity for use in the dry and semidry processes to remove SO2 from the flue gas.

  11. Use of biomass sorbents for oil removal from gas station runoff.

    Science.gov (United States)

    Khan, Eakalak; Virojnagud, Wanpen; Ratpukdi, Thunyalux

    2004-11-01

    The use of biomass sorbents, which are less expensive and more biodegradable than synthetic sorbents, for oil removal from gas station runoff was investigated. A bench-scale flume experiment was conducted to evaluate the oil removal and retention capabilities of the biomass sorbents which included kapok fiber, cattail fiber, Salvinia sp., wood chip, rice husk, coconut husk, and bagasse. Polyester fiber, a commercial synthetic sorbent, was also experimented for comparison purpose. Oil sorption and desorption tests were performed at a water flow rate of 20 lmin-1. In the oil sorption tests, a 50 mgl(-1) of used engine oil-water mixture was synthesized to simulate the gas station runoff. The mass of oil sorbed for all sorbents, except coconut husk and bagasse, was greater than 70%. Cattail fiber and polyester fiber were the sorbents that provided the least average effluent oil concentrations. Oil selectivity (hydrophobic properties) and physical characteristics of the sorbents are the two main factors that influence the oil sorption capability. The used sorbents from the sorption tests were employed in the desorption tests. Results indicated that oil leached out of all the sorbents tested. Polyester fiber released the highest amount of oil, approximately 4% (mass basis) of the oil sorbed.

  12. Ultratrace determination of arsenic in water samples by electrothermal atomic absorption spectrometry after pre-concentration with Mg-Al-Fe ternary layered double hydroxide nano-sorbent.

    Science.gov (United States)

    Abdolmohammad-Zadeh, Hossein; Jouyban, Abolghasem; Amini, Roghayeh

    2013-11-15

    A selective solid phase extraction method, based on nano-structured Mg-Al-Fe(NO3(-)) ternary layered double hydroxide as a sorbent, is developed for the pre-concentration of ultra-trace levels of arsenic (As) prior to determination by electrothermal atomic absorption spectrometry. It is found that both As(III) and As(V) could be quantitatively retained on the sorbent within a wide pH range of 4-12. Accordingly, the presented method is applied to determination of total inorganic As in aqueous solutions. Maximum analytical signal of As is achieved when the pyrolysis and atomization temperatures are close to 900 °C and 2300 °C, respectively. Several variables affecting the extraction efficiency including pH, sample flow rate, amount of nano-sorbent, elution conditions and sample volume are optimized. Under the optimized conditions, the limit of detection (3Sb/m) and the relative standard deviation are 4.6 pg mL(-1) and 3.9%, respectively. The calibration graph is linear in the range of 15.0-650 pg mL(-1) with a correlation coefficient of 0.9979, sorption capacity and pre-concentration factor are 8.68 mg g(-1) and 300, respectively. The developed method is validated by the analysis of a standard reference material (SRM 1643e) and is successfully applied to the determination of ultra-trace amounts of As in different water samples.

  13. Algorithms for semi on-line multiprocessor scheduling problems

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    In the classical multiprocessor scheduling problems, it is assumed that the problems are considered in off-line or on-line environment. But in practice, problems are often not really off-line or on-line but somehow in between. This means that, with respect to the on-line problem, some further information about the tasks is available, which allows the improvement of the performance of the best possible algorithms. Problems of this class are called semi on-line ones. The authors studied two semi on-line multiprocessor scheduling problems, in which, the total processing time of all tasks is known in advance, or all processing times lie in a given interval. They proposed approximation algorithms for minimizing the makespan and analyzed their performance guarantee. The algorithms improve the known results for 3 or more processor cases in the literature.

  14. Remote Automatic Material On-Line Sensor

    Energy Technology Data Exchange (ETDEWEB)

    Magnuson, Erik

    2005-12-20

    Low cost NMR sensor for measuring moisture content of forest products. The Department of Energy (DOE) Industries of the Future (IOF) program seeks development and implementation of technologies that make industry more efficient--in particular, more energy-efficient. Quantum Magnetics, Inc. (QM), a wholly-owned subsidiary of GE Security, received an award under the program to investigate roles for low-cost Nuclear Magnetic Resonance (NMR) technology in furtherance of these goals. Most NMR systems are designed for high-resolution spectroscopy applications. These systems use intense magnetic fields produced by superconducting magnets that drive price and operating cost to levels beyond industry tolerance. At low magnetic fields, achievable at low cost, one loses the ability to obtain spectroscopic information. However, measuring the time constants associated with the NMR signal, called NMR relaxometry, gives indications of chemical and physical states of interest to process control and optimization. It was the purpose of this effort to investigate the technical and economic feasibility of using such low-field, low-cost NMR to monitor parameters enabling greater process efficiencies. The primary target industry identified in the Cooperative Development Agreement was the wood industry, where the moisture content of wood is a key process parameter from the time the cut tree enters a mill until the time it is delivered as pieces of lumber. Extracting the moisture is energy consuming, and improvements in drying efficiency stand to reduce costs and emissions substantially. QM designed and developed a new, low-cost NMR instrument suitable for inspecting lumber up to 3 inches by 12 inches in cross section, and other materials of similar size. Low cost is achieved via an inexpensive, permanent magnet and low-cost NMR spectrometer electronics. Laboratory testing demonstrated that the NMR system is capable of accurate ({+-} 0.5%) measurements of the moisture content of wood for

  15. Comparative DNA isolation behaviours of silica and polymer based sorbents in batch fashion: monodisperse silica microspheres with bimodal pore size distribution as a new sorbent for DNA isolation.

    Science.gov (United States)

    Günal, Gülçin; Kip, Çiğdem; Eda Öğüt, S; İlhan, Hasan; Kibar, Güneş; Tuncel, Ali

    2017-03-22

    Monodisperse silica microspheres with bimodal pore-size distribution were proposed as a high performance sorbent for DNA isolation in batch fashion under equilibrium conditions. The proposed sorbent including both macroporous and mesoporous compartments was synthesized 5.1 μm in-size, by a "staged shape templated hydrolysis and condensation method". Hydrophilic polymer based sorbents were also obtained in the form of monodisperse-macroporous microspheres ca 5.5 μm in size, with different functionalities, by a developed "multi-stage microsuspension copolymerization" technique. The batch DNA isolation performance of proposed material was comparatively investigated using polymer based sorbents with similar morphologies. Among all sorbents tried, the best DNA isolation performance was achieved with the monodisperse silica microspheres with bimodal pore size distribution. The collocation of interconnected mesoporous and macroporous compartments within the monodisperse silica microspheres provided a high surface area and reduced the intraparticular mass transfer resistance and made easier both the adsorption and desorption of DNA. Among the polymer based sorbents, higher DNA isolation yields were achieved with the monodisperse-macroporous polymer microspheres carrying trimethoxysilyl and quaternary ammonium functionalities. However, batch DNA isolation performances of polymer based sorbents were significantly lower with respect to the silica microspheres.

  16. Experimental study on the reuse of spent rapidly hydrated sorbent for circulating fluidized bed flue gas desulfurization.

    Science.gov (United States)

    Li, Yuan; Zheng, Kai; You, Changfu

    2011-11-01

    Rapidly hydrated sorbent, prepared by rapidly hydrating adhesive carrier particles and lime, is a highly effective sorbent for moderate temperature circulating fluidized bed flue gas desulfurization (CFB-FGD) process. The residence time of fine calcium-containing particles in CFB reactors increases by adhering on the surface of larger adhesive carrier particles, which contributes to higher sorbent calcium conversion ratio. The circulation ash of CFB boilers (α-adhesive carrier particles) and the spent sorbent (β and γ-adhesive carrier particles) were used as adhesive carrier particles for producing the rapidly hydrated sorbent. Particle physical characteristic analysis, abrasion characteristics in fluidized bed and desulfurization characteristics in TGA and CFB-FGD systems were investigated for various types of rapidly hydrated sorbent (α, β, and γ-sorbent). The adhesion ability of γ-sorbent was 50.1% higher than that of α-sorbent. The abrasion ratio of β and γ-sorbent was 16.7% lower than that of α-sorbent. The desulfurization abilities of the three sorbent in TGA were almost same. The desulfurization efficiency in the CFB-FGD system was up to 95% at the bed temperature of 750 °C for the β-sorbent.

  17. Different methods to select the best extraction system for solid-phase extraction.

    Science.gov (United States)

    Bielicka-Daszkiewicz, Katarzyna

    2015-02-01

    The optimization methods for planning a solid-phase extraction experiment are presented. These methods are based on a study of interactions between different parts of an extraction system. Determination of the type and strength of interaction depends on the physicochemical properties of the individual components of the system. The main parameters that determine the extraction properties are described in this work. The influence of sorbents' and solvents' polarity on extraction efficiency, Hansen solubility parameters and breakthrough volume determination on sorption and desorption extraction step are discussed.

  18. Highly effective sorbents obtained by treating agrowaste products in cold plasma

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    Sorbents are widely used in purification of various liquids and gases, offering a universal means for wastewater and air cleaning. The most promising sorbents are those obtained from agrowaste products such as rice or buckwheat husk. Processing of husk in cold plasma modifies the composition, structure and surface properties of the raw material and raises its porosity, thus substantially improving the sorption properties of the final product.Husk as a raw material for producing sorbents has the following advantageous properties: (1) appropriate chemical composition; (2) low cost; (3) high dispersity, due to which there is no need in any special treatment of the material prior to its exposing to plasma; (4) scaly structure and developed porous surface ensuring a high surface-to-volume ratio. The best properties are displayed by the sorbents obtained in cold plasma under reduced pressures of 53.2 Pa. The raw naterial traverses the region occupied by the plasma and, as it does so, it gets heated up to a temperature of 250 - 350 ℃. The whole process involves two stages: combustion of the raw material and modification of its properties under the action of the plasma. The combustion proceeds due to the oxygen contained in the starting material. During the combustion, the hydrogen contained in the starting material and some part of the carbon also burn out.The resultant scaly sorbent is accumulated in a cooler. The scales are black; they range in sizes from 1mm to 5 mm.The sorbents obtained are remarkable for their useful properties and outperform most of the traditional sorbents used in modern industry. The starting materials are inexpensive, and their resources are almost unlimited. The sorbents have rather a low production cost (1.8-2.5($)/kg). The sorbents can be used for cleaning hydrosphere from water pollutants on a large scale. The degree of cleaning water surface from oil products with sorbents was a subject of investigation. The highest degree of purification

  19. KINETICS OF Mn-BASED SORBENTS FOR HOT COAL GAS DESULFURIZATION

    Energy Technology Data Exchange (ETDEWEB)

    J.J. BERNS; K.A. SADECKI; M.T. HEPWORTH

    1997-09-15

    Mixed manganese oxide sorbents have been investigated for high-temperature removal of hydrogen sulfide (the primary sulfur bearing compound) from hot coal gases. The sorbents were screened by thermodynamic equilibrium considerations for sulfidation. Preliminary experimental work using thermogravimetric analysis (TGA) indicated titania to be a superior substrate than alumina. Four formulations showing superior reactivity in a TGA were then tested in an ambient pressure fixed-bed reactor to determine steady state H 2 S concentrations, breakthrough times and effectiveness of the sorbent when subjected to cyclic sulfidation and regeneration testing. Eight tests were conducted with each test consisting of five cycles of sulfidation and regeneration. Sulfidation occurred at 600 o C using a simulated coal gas at an empty-bed space velocity of approximately 12,000 per hour. Manganese-based sorbents with molar ratios > 1:1 Mn:Substrate were effective in reducing the H 2 S concentration in simulated coal gases to less than 100 ppmv over five cycles. Actual breakthrough time for formulation C6-2-1100 was as high as 73% of breakthrough time based on wt% Mn in sorbent at 600 o C. Regeneration tests determined that loaded pellets can be essentially completely regenerated in an air/steam mixture at 750 o C with minimal sulfate formation. The leading formulation (designated C6-2) from the fixed-bed tests was then further tested under varying sorbent induration temperature, sulfidation temperature and superficial gas velocity. Four tests were conducted with each test consisting of four cycles of sulfidation and regeneration. Results showed that the induration temperature of the sorbent and the reaction temperature greatly affected the H 2 S removal capacity of the sorbent while the superficial gas velocity between 1090 and 1635 cm/min had minimal affect on the sorbent's breakthrough capacity. Testing showed that the sorbent's strength was a strong function of the sorbent

  20. ASSESSMENT OF LOW COST NOVEL SORBENTS FOR COAL-FIRED POWER PLANT MERCURY CONTROL

    Energy Technology Data Exchange (ETDEWEB)

    Sharon Sjostrom

    2004-03-01

    The injection of sorbents upstream of a particulate control device is one of the most promising methods for controlling mercury emissions from coal-fired utility boilers with electrostatic precipitators and fabric filters. Studies carried out at the bench-, pilot-, and full-scale have shown that a wide variety of factors may influe