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Sample records for on-line sorbent extraction

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

    Science.gov (United States)

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

    2016-10-01

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

  2. Approaches for on-line coupling of extraction and chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Hyoetylaeinen, Tuulia; Riekkola, Marja-Liisa [Laboratory of Analytical Chemistry, Department of Chemistry, University of Helsinki, P.O. Box 55, 00014, Helsinki (Finland)

    2004-04-01

    This review provides an overview of the approaches available in order to perform on-line coupling of various extraction techniques with liquid and gas chromatography, for the analysis of semivolatile and nonvolatile analytes in liquid and solid samples. The main focus is on the instrumental set-up of these techniques. Selected real applications are described by way of illustration. The extraction methods suitable for on-line coupling covered in this review are: liquid-liquid extraction, solid-phase extraction, membrane-based techniques, pressurised liquid extraction, supercritical fluid extraction, and microwave- and sonication-assisted extractions. The following systems are not covered in this review: on-line coupled solid-phase extraction-liquid chromatography, purge-and-trap-GC, and membrane extraction with a sorbent interface-GC. (orig.)

  3. Application of cotton as a solid phase extraction sorbent for on-line preconcentration of copper in water samples prior to inductively coupled plasma optical emission spectrometry determination.

    Science.gov (United States)

    Faraji, Mohammad; Yamini, Yadollah; Shariati, Shahab

    2009-07-30

    Copper, as a heavy metal, is toxic for many biological systems. Thus, the determination of trace amounts of copper in environmental samples is of great importance. In the present work, a new method was developed for the determination of trace amounts of copper in water samples. The method is based on the formation of ternary Cu(II)-CAS-CTAB ion-pair and adsorption of it into a mini-column packed with cotton prior applying inductively coupled plasma optical emission spectrometry (ICP-OES). The experimental parameters that affected the extraction efficiency of the method such as pH, flow rate and volume of the sample solution, concentration of chromazurol S (CAS) and cethyltrimethylammonium bromide (CTAB) as well as type and concentration of eluent were investigated and optimized. The ion-pair (Cu(II)-CAS-CTAB) was quantitatively retained on the cotton under the optimum conditions, then eluted completely using a solution of 25% (v/v) 1-propanol in 0.5 mol L(-1) HNO(3) and directly introduced into the nebulizer of the ICP-OES. The detection limit (DL) of the method for copper was 40 ng L(-1) (V(sample)=100mL) and the relative standard deviation (R.S.D.) for the determination of copper at 10 microg L(-1) level was found to be 1.3%. The method was successfully applied to determine the trace amounts of copper in tap water, deep well water, seawater and two different mineral waters, and suitable recoveries were obtained (92-106%).

  4. Graphene oxide-based composite monolith as new sorbent for the on-line solid phase extraction and high performance liquid chromatography determination of ß-sitosterol in food samples.

    Science.gov (United States)

    Cui, Beijiao; Guo, Bin; Wang, Huimin; Zhang, Doudou; Liu, Haiyan; Bai, Ligai; Yan, Hongyuan; Han, Dandan

    2018-08-15

    A composite monolithic column was prepared by redox initiation method for the on-line purification and enrichment of β-sitosterol, in which graphene oxide (GO) was embedded. The obtained monolithic column was characterized by scanning electron microscopy (SEM) and nitrogen adsorption-desorption isotherm measurement, which indicated that the monolith possessed characteristics of porous structure and high permeability. Under the optimum conditions for extraction and determination, the calibration equation was y = 47.92 × -0.1391; the linear range was 0.008-1.0 mg mL -1 ; the linear regression coefficient was 0.998; the limit of detection (LOD) is 2.4 μg mL -1 ; the limit of quantitation (LOQ) was 8 μg mL -1 ; precisions for intra-day and inter-day assays presented as relative standard deviations were less than 4.3% and 6.8%, respectively. Under the selective conditions, the enrichment factor of the method was 119. The recovery was in the range of 80.40-98.00%. Moreover, the adsorption amount of the monolith was compared with silica gel-C18 adsorbent and the monolith without graphene oxide being embedded. The polymerization monolithic column showed high selectivity and good permeability, and it was successfully used as on-line solid-phase extraction (SPE) column for determination of β-sitosterol in edible oil. Copyright © 2018 Elsevier B.V. All rights reserved.

  5. The current role of on-line extraction approaches in clinical and forensic toxicology.

    Science.gov (United States)

    Mueller, Daniel M

    2014-08-01

    In today's clinical and forensic toxicological laboratories, automation is of interest because of its ability to optimize processes, to reduce manual workload and handling errors and to minimize exposition to potentially infectious samples. Extraction is usually the most time-consuming step; therefore, automation of this step is reasonable. Currently, from the field of clinical and forensic toxicology, methods using the following on-line extraction techniques have been published: on-line solid-phase extraction, turbulent flow chromatography, solid-phase microextraction, microextraction by packed sorbent, single-drop microextraction and on-line desorption of dried blood spots. Most of these published methods are either single-analyte or multicomponent procedures; methods intended for systematic toxicological analysis are relatively scarce. However, the use of on-line extraction will certainly increase in the near future.

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

    KAUST Repository

    Naidu, Gayathri; Loganathan, Paripurnanda; Jeong, Sanghyun; Johir, Md.Abu Hasan; To, Vu Hien Phuong; Kandasamy, Jaya; Vigneswaran, Saravanamuthu

    2016-01-01

    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

  7. Development of Novel Sorbents for Uranium Extraction from Seawater

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Wenbin [Univ. of Chicago, IL (United States); Taylor-Pashow, Kathryn [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    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

  8. Development of Novel Sorbents for Uranium Extraction from Seawater

    International Nuclear Information System (INIS)

    Lin, Wenbin; Taylor-Pashow, Kathryn

    2014-01-01

    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

  9. 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

    are focused on the applications of SI-BI-LOV protocols for on-line microcolumn based solid phase extraction of ultra-trace levels of heavy metals, employing the so-called renewable surface separation and preconcentration manipulatory scheme. Two types of sorbents have been employed as packing material...

  10. Immobilized humic substances and immobilized aggregates of humic substances as sorbent for solid phase extraction.

    Science.gov (United States)

    Erny, Guillaume L; Gonçalves, Bruna M; Esteves, Valdemar I

    2013-09-06

    In this work, humic substances (HS) immobilized, as a thin layer or as aggregates, on silica gel were tested as material for solid phase extraction. Some triazines (simazine, atrazine, therbutylazine, atrazine-desethyl-desisopropyl-2-hydroxy, ametryn and terbutryn), have been selected as test analytes due to their environmental importance and to span a large range of solubility and octanol/water partition coefficient (logP). The sorbent was obtained immobilizing a thin layer of HS via physisorption on a pre-coated silica gel with a cationic polymer (polybrene). While the sorbent could be used as it is, it was demonstrated that additional HS could be immobilized, via weak interactions, to form stable humic aggregates. However, while a higher quantity of HS could be immobilized, no significant differences were observed in the sorption parameters. This sorbent have been tested for solid phase extraction to concentrate triazines from aqueous matrixes. The sorbent demonstrated performances equivalent to commercial alternatives as a concentration factor between 50 and 200, depending on the type of triazines, was obtained. Moreover the low cost and the high flow rate of sample through the column allowed using high quantity of sorbent. The analytical procedure was tested with different matrixes including tap water, river water and estuarine water. Copyright © 2013 Elsevier B.V. All rights reserved.

  11. 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.

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

    International Nuclear Information System (INIS)

    Zhang, Yong; Mei, Meng; Huang, Xiaojia; Yuan, Dongxing

    2015-01-01

    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

  13. Improving the On-Line Extraction of Polar Compounds by IT-SPME with Silica Nanoparticles Modified Phases

    Directory of Open Access Journals (Sweden)

    Pascual Serra-Mora

    2018-02-01

    Full Text Available In the present work the extraction efficiency of in-tube solid-phase microextraction (IT-SPME for polar herbicides has been evaluated using extractive capillaries coated with different polymeric sorbents. For this purpose, aqueous solutions of herbicides with a wide range of polarities, including some highly polar compounds (log Kow < 1, have been directly processed by IT-SPME coupled on-line to capillary liquid chromatography with UV-diode array detection. For extraction, commercially available capillary columns coated with polydimethylsiloxane (PDMS and polyetilenglicol (PEG-based phases have been used, and the results have been compared with those obtained with a synthesized tetraethyl orthosilicate (TEOS-trimethoxyethylsilane (MTEOS polymer, as well as the same polymer reinforced with silica nanoparticles (SiO2 NPs. The SiO2 NPs functionalized TEOS-MTEOS coating provided the best results for most herbicides, especially for the most polar compounds. On the basis of the results obtained, conditions for the quantification of the herbicides tested are described using a SiO2 NPs reinforced TEOS-MTEOS coated capillary. The proposed method provided satisfactory linearity up to concentrations of 200 μg/L. The precision was also suitable, with relative standard deviations (RSDs values ≤9% (n = 3, and the limits of detection (LODs were within the 0.5–7.5 µg/L range. The method has been applied to different water samples and the extract obtained from an agricultural soil.

  14. Preliminary studies of using preheated carrier gas for on-line membrane extraction of semivolatile organic compounds.

    Science.gov (United States)

    Liu, Xinyu; Pawliszyn, Janusz

    2007-04-01

    In this paper, we present results for the on-line determination of semivolatile organic compounds (SVOCs) in air using membrane extraction with a sorbent interface-ion mobility spectrometry (MESI-IMS) system with a preheated carrier (stripping) gas. The mechanism of the mass transfer of SVOCs across a membrane was initially studied. In comparison with the extraction of volatile analytes, the mass transfer resistance that originated from the slow desorption from the internal membrane surface during the SVOC extraction processes should be taken into account. A preheated carrier gas system was therefore built to facilitate desorption of analytes from the internal membrane surface. With the benefit of a temperature gradient existing between the internal and external membrane surfaces, an increase in the desorption rate of a specific analyte at the internal surface and the diffusion coefficient within the membrane could be achieved while avoiding a decrease of the distribution constant on the external membrane interface. This technique improved both the extraction rate and response times of the MESI-IMS system for the analysis of SVOCs. Finally, the MESI-IMS system was shown to be capable of on-site measurement by monitoring selected polynuclear aromatic hydrocarbons emitted from cigarette smoke.

  15. Critical comparison of the on-line and off-line molecularly imprinted solid-phase extraction of patulin coupled with liquid chromatography.

    Science.gov (United States)

    Lhotská, Ivona; Holznerová, Anežka; Solich, Petr; Šatínský, Dalibor

    2017-12-01

    Reaching trace amounts of mycotoxin contamination requires sensitive and selective analytical tools for their determination. Improving the selectivity of sample pretreatment steps covering new and modern extraction techniques is one way to achieve it. Molecularly imprinted polymers as selective sorbent for extraction undoubtedly meet these criteria. The presented work is focused on the hyphenation of on-line molecularly imprinted solid-phase extraction with a chromatography system using a column-switching approach. Making a critical comparison with a simultaneously developed off-line extraction procedure, evaluation of pros and cons of each method, and determining the reliability of both methods on a real sample analysis were carried out. Both high-performance liquid chromatography methods, using off-line extraction on molecularly imprinted polymer and an on-line column-switching approach, were validated, and the validation results were compared against each other. Although automation leads to significant time savings, fewer human errors, and required no handling of toxic solvents, it reached worse detection limits (15 versus 6 μg/L), worse recovery values (68.3-123.5 versus 81.2-109.9%), and worse efficiency throughout the entire clean-up process in comparison with the off-line extraction method. The difficulties encountered, the compromises made during the optimization of on-line coupling and their critical evaluation are presented in detail. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Automated magnetic sorbent extraction based on octadecylsilane functionalized maghemite magnetic particles in a sequential injection system coupled with electrothermal atomic absorption spectrometry for metal determination.

    Science.gov (United States)

    Giakisikli, Georgia; Anthemidis, Aristidis N

    2013-06-15

    A new automatic sequential injection (SI) system for on-line magnetic sorbent extraction coupled with electrothermal atomic absorption spectrometry (ETAAS) has been successfully developed for metal determination. In this work, we reported effective on-line immobilization of magnetic silica particles into a microcolumn by the external force of two strong neodymium iron boron (NdFeB) magnets across it, avoiding the use of frits. Octadecylsilane functionalized maghemite magnetic particles were used as sorbent material. The potentials of the system were demonstrated for trace cadmium determination in water samples. The method was based on the on-line complex formation with diethyldithiocarbamate (DDTC), retention of Cd-DDTC on the surface of the MPs and elution with isobutyl methyl ketone (IBMK). The formation mechanism of the magnetic solid phase packed column and all critical parameters (chemical, flow, graphite furnace) influencing the performance of the system were optimized and offered good analytical characteristics. For 5 mL sample volume, a detection limit of 3 ng L(-1), a relative standard deviation of 3.9% at 50 ng L(-1) level (n=11) and a linear range of 9-350 ng L(-1) were obtained. The column remained stable for more than 600 cycles keeping the cost down in routine analysis. The proposed method was evaluated by analyzing certified reference materials and natural waters. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. Synthesis and application of chloromethylated polystyrene modified with 1-phenyl-1,2-propanedione-2-oxime thiosemicarbazone (PPDOT) as a new sorbent for the on-line preconcentration and determination of copper in water, soil, and food samples by FAAS

    Energy Technology Data Exchange (ETDEWEB)

    Chamjangali, Mansour Arab, E-mail: marab@shahroodut.ac.ir [College of Chemistry, Shahrood University of Technology, P.O. Box 36155-316, Shahrood (Iran, Islamic Republic of); Bagherian, Ghadamali; Mokhlesian, Ali; Bahramian, Bahram [College of Chemistry, Shahrood University of Technology, P.O. Box 36155-316, Shahrood (Iran, Islamic Republic of)

    2011-09-15

    Highlights: {yields} This paper is the first report on the use of PS-PPDOT resin in the SPE studies. {yields} The proposed adsorbent is highly selective for trace determination of copper. {yields} The method is applicable for copper determination in water, soil, and food samples. - Abstract: In this paper, we report a simple and sensitive on-line solid phase extraction system for the preconcentration and determination of Cu(II) by flame atomic absorption spectrometry (FAAS). This method is based upon the on-line retention of copper at pH 5.0 on a minicolumn packed with chloromethylated polystyrene modified by 1-phenyl-1,2-propanedione-2-oxime thiosemicarbazone (PPDOT) as a new solid-phase extraction (SPE) sorbent. The retained Cu(II) ions were eluted with 1.0 M HNO{sub 3}, and transported directly to FAAS for determination. Several chemical and flow variables were studied and optimized for a quantitative preconcentration and determination of copper(II). At the optimized conditions, for preconcentration of 10.0 mL of a sample solution, a linear calibration graph was obtained over the concentration range of 3.00-120.0 {mu}g L{sup -1} for Cu(II). The limit of detection (3{sigma}), limit of quantification (10{sigma}), and enrichment factor are 0.56 {mu}g L{sup -1}, 2.0 {mu}g L{sup -1} and 41, respectively. The relative standard deviation (n = 6) at 20 {mu}g L{sup -1} of Cu(II) is 2.0%. This method could be applied for determination of trace amounts of Cu(II) in water, soil, and food samples with satisfactory results.

  18. Synthesis and application of chloromethylated polystyrene modified with 1-phenyl-1,2-propanedione-2-oxime thiosemicarbazone (PPDOT) as a new sorbent for the on-line preconcentration and determination of copper in water, soil, and food samples by FAAS

    International Nuclear Information System (INIS)

    Chamjangali, Mansour Arab; Bagherian, Ghadamali; Mokhlesian, Ali; Bahramian, Bahram

    2011-01-01

    Highlights: → This paper is the first report on the use of PS-PPDOT resin in the SPE studies. → The proposed adsorbent is highly selective for trace determination of copper. → The method is applicable for copper determination in water, soil, and food samples. - Abstract: In this paper, we report a simple and sensitive on-line solid phase extraction system for the preconcentration and determination of Cu(II) by flame atomic absorption spectrometry (FAAS). This method is based upon the on-line retention of copper at pH 5.0 on a minicolumn packed with chloromethylated polystyrene modified by 1-phenyl-1,2-propanedione-2-oxime thiosemicarbazone (PPDOT) as a new solid-phase extraction (SPE) sorbent. The retained Cu(II) ions were eluted with 1.0 M HNO 3 , and transported directly to FAAS for determination. Several chemical and flow variables were studied and optimized for a quantitative preconcentration and determination of copper(II). At the optimized conditions, for preconcentration of 10.0 mL of a sample solution, a linear calibration graph was obtained over the concentration range of 3.00-120.0 μg L -1 for Cu(II). The limit of detection (3σ), limit of quantification (10σ), and enrichment factor are 0.56 μg L -1 , 2.0 μg L -1 and 41, respectively. The relative standard deviation (n = 6) at 20 μg L -1 of Cu(II) is 2.0%. This method could be applied for determination of trace amounts of Cu(II) in water, soil, and food samples with satisfactory results.

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

    International Nuclear Information System (INIS)

    Mendoza R, L. G.; Rodriguez de San Miguel, E.; Pardo G, D. Y.; De Gyves, J.; Sanchez G, J. P.

    2011-01-01

    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, 29 Si and 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 -1 HCl + 0.1% KCl medium, while the maximum desorption was observed at 60 min in a 1.5 mol L -1 H 2 SO 4 + 20% v/v H 2 O 2 medium when titanium concentration was 70 mg L -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)

  20. 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)

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

    Science.gov (United States)

    Xu, Li; Lee, Hian Kee

    2008-05-30

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

  2. Supercritical fluid extraction-capillary gas chromatography: on-line coupling with a programmed temperature vaporizer

    NARCIS (Netherlands)

    Houben, R.J.; Janssen, J.G.M.; Leclercq, P.A.; Rijks, J.A.; Cramers, C.A.M.G.

    1990-01-01

    A simple and versatile system is described for the on-line coupling of SFE to capillary GC. The interfacing consists of a programmed temperature vaporizer (PTV) injector. With this injector it is possible to combine solute trapping, elimination of a high flow of extraction fluid, and quantitative

  3. Magnetic hydrophilic-lipophilic balance sorbent for efficient extraction of chemical warfare agents from water samples.

    Science.gov (United States)

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

    2016-02-19

    Magnetic hydrophilic-lipophilic balance (MHLB) hybrid resin was prepared by precipitation polymerization using N-vinylpyrrolidone (PVP) and divinylbenzene (DVB) as monomers and Fe2O3 nanoparticles as magnetic material. These resins were successfully applied for the extraction of chemical warfare agents (CWAs) and their markers from water samples through magnetic dispersive solid-phase extraction (MDSPE). By varying the ratios of monomers, resin with desired hydrophilic-lipophilic balance was prepared for the extraction of CWAs and related esters of varying polarities. Amongst different composites Fe2O3 nanoparticles coated with 10% PVP+90% DVB exhibited the best recoveries varying between 70.32 and 97.67%. Parameters affecting the extraction efficiencies, such as extraction time, desorption time, nature and volume of desorption solvent, amount of extraction sorbent and the effect of salts on extraction were investigated. Under the optimized conditions, linearity was obtained in the range of 0.5-500 ng mL(-1) with correlation ranging from 0.9911-0.9980. Limits of detection and limits of quantification were 0.5-1.0 and 3.0-5.0 ng mL(-1) respectively with RSDs varying from 4.88-11.32% for markers of CWAs. Finally, the developed MDSPE method was employed for extraction of analytes from water samples of various sources and the OPCW proficiency test samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. New sorbent materials for selective extraction of cocaine and benzoylecgonine from human urine samples.

    Science.gov (United States)

    Bujak, Renata; Gadzała-Kopciuch, Renata; Nowaczyk, Alicja; Raczak-Gutknecht, Joanna; Kordalewska, Marta; Struck-Lewicka, Wiktoria; Waszczuk-Jankowska, Małgorzata; Tomczak, Ewa; Kaliszan, Michał; Buszewski, Bogusław; Markuszewski, Michał J

    2016-02-20

    An increase in cocaine consumption has been observed in Europe during the last decade. Benzoylecgonine, as a main urinary metabolite of cocaine in human, is so far the most reliable marker of cocaine consumption. Determination of cocaine and its metabolite in complex biological samples as urine or blood, requires efficient and selective sample pretreatment. In this preliminary study, the newly synthesized sorbent materials were proposed for selective extraction of cocaine and benzoylecgonine from urine samples. Application of these sorbent media allowed to determine cocaine and benzoylecgonine in urine samples at the concentration level of 100ng/ml with good recovery values as 81.7%±6.6 and 73.8%±4.2, respectively. The newly synthesized materials provided efficient, inexpensive and selective extraction of both cocaine and benzoylecgonine from urine samples, which can consequently lead to an increase of the sensitivity of the current available screening diagnostic tests. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. 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.

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

    Science.gov (United States)

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

    2013-04-12

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

  7. Characteristic of New Solid-Phase Extraction Sorbent: Activated Carbon Prepared from Rice Husks under Base Treated Condition

    OpenAIRE

    Afrida Kurnia Putri; Wang-Hsien Ding; Han-Wen Kuo

    2012-01-01

    A characterization of activated carbon (ACs) prepared from rice husks (RHs) under base treated condition as a new sorbent for solid-phase extraction (SPE) to extract 4-nonylphenol isomers (4-NPs) in water samples has been done. The ACs prepared from RHs usually exhibits low specific surface area due to its high ash content, but in case of its application for SPE, there are other factors need to be considered, such as the existence of functional groups inside the sorbent, that can enhance inte...

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

    Science.gov (United States)

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

    2017-08-15

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

  9. Solid-Phase Extraction of Sulfur Mustard Metabolites Using an Activated Carbon Fiber Sorbent.

    Science.gov (United States)

    Lee, Jin Young; Lee, Yong Han

    2016-01-01

    A novel solid-phase extraction method using activated carbon fiber (ACF) was developed and validated. ACF has a vast network of pores of varying sizes and microporous structures that result in rapid adsorption and selective extraction of sulfur mustard metabolites according to the pH of eluting solvents. ACF could not only selectively extract thiodiglycol and 1-methylsulfinyl-2-[2-(methylthio)-ethylsulfonyl]ethane eluting a 9:1 ratio of dichloromethane to acetone, and 1,1'-sulfonylbis[2-(methylsulfinyl)ethane] and 1,1'-sulfonylbis- [2-S-(N-acetylcysteinyl)ethane] eluting 3% hydrogen chloride in methanol, but could also eliminate most interference without loss of analytes during the loading and washing steps. A sample preparation method has been optimized for the extraction of sulfur mustard metabolites from human urine using an ACF sorbent. The newly developed extraction method was applied to the trace analysis of metabolites of sulfur mustard in human urine matrices in a confidence-building exercise for the analysis of biomedical samples provided by the Organisation for the Prohibition of Chemical Weapons. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

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

    International Nuclear Information System (INIS)

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

    1977-02-01

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

  11. Flow injection microfluidic device with on-line fluorescent derivatization for the determination of Cr(III) and Cr(VI) in water samples after solid phase extraction

    Energy Technology Data Exchange (ETDEWEB)

    Peng, Guilong [Key Laboratory of Eco-Environment of Three Gorges Region of Ministry of Education, Chongqing University, Chongqing, 400045 (China); Department of Chemistry, Beijing Key Laboratory of Microanalytical Methods and Instrumentation, Tsinghua University, Beijing, 100084 (China); He, Qiang, E-mail: heqiang0980@163.com [Key Laboratory of Eco-Environment of Three Gorges Region of Ministry of Education, Chongqing University, Chongqing, 400045 (China); Lu, Ying [Department of Mathematics and Physics, Armed Police College, Chengdu, 610213 (China); Huang, Jing [Research Center for Advanced Computation, College of Science, Xihua University, Chengdu, 610039 (China); Lin, Jin-Ming, E-mail: jmlin@mail.tsinghua.edu.cn [Department of Chemistry, Beijing Key Laboratory of Microanalytical Methods and Instrumentation, Tsinghua University, Beijing, 100084 (China)

    2017-02-22

    In this paper, a rapid and simple method using magnetic multi-walled carbon nanotubes (MWCNTS), as a solid-phase extraction (SPE) sorbent, was successfully developed for extraction and preconcentration trace amounts of Cr(III) in water samples. The synthesized magnetic-MWCNTs nanocomposite was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). A rhodamine derivative (R1) was synthesized and characterized as a highly selective and sensitive fluorescent derivatizing agent for Cr(III). After SPE procedure, Cr(III) analysis was performed by flow injection microfluidic chip with on-line fluorescent derivatization and laser-induced fluorescence (LIF) spectroscopy detection. The parameters, which affected the efficiency of the developed method were investigated and optimized. Under the optimized conditions, the method exhibited a linear dynamic range of 0–10.0 nM, with a detection limit of 0.094 nM and an enrichment factor of 38. Furthermore, real water samples were analyzed and good recoveries were obtained from 91.0 to 101.6%. - Graphical abstract: Flow injection microfluidic device with on-line fluorescent derivatization and detection coupled to LIF. - Highlights: • A highly selective and sensitive derivatizing reagent for Cr(III) was synthesized and characterized. • The magnetic-MWCNTs nanocomposite as a SPE sorbent was successfully synthesized and characterized. • A new portable detection system was developed for microfluidic chip FIA platform.

  12. 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%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Characteristic of New Solid-Phase Extraction Sorbent: Activated Carbon Prepared from Rice Husks under Base Treated Condition

    Directory of Open Access Journals (Sweden)

    Afrida Kurnia Putri

    2012-10-01

    Full Text Available A characterization of activated carbon (ACs prepared from rice husks (RHs under base treated condition as a new sorbent for solid-phase extraction (SPE to extract 4-nonylphenol isomers (4-NPs in water samples has been done. The ACs prepared from RHs usually exhibits low specific surface area due to its high ash content, but in case of its application for SPE, there are other factors need to be considered, such as the existence of functional groups inside the sorbent, that can enhance interaction of non-polar sorbent with analyte in the water matrices. In this case, silanol groups from ash content may affect the extraction efficiency for 4-NPs. The ACs made from RHs were chemically impregnated with ZnCl2 and carbonized at 800oC. To investigate the role of silica, three types of ACs were prepared, i.e., untreated ACs (AC–Si, contain silica, base treated ACs (AC–B–Si, remain some silica inside, and ACs made by base treated RHs (AC–B, no silica, the surface area obtained from these treatments were 1352 m2/g, 1666 m2/g, and 1712m2/g respectively.  ACs made by base treatment has the highest surface area (related to BET, which indicat that silica removal process promotes the formation of open pore system on ACs and enhances the surface area of ACs. However, extraction efficiency measured by GC-MS in SPE process showed the reversal trends (i.e., AC–Si= 32.08%, AC–B–Si= 82.63%, AC–B=51.78%, among them the AC–B–Si sorbent reveal the best performance in SPE process. It is indicated that although silica usually exhibits low specific surface area, but control presence of silica as a polar functional group has a positive influence in the interaction between non-polar sorbent and 4-NPs.

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

    International Nuclear Information System (INIS)

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

    2006-01-01

    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

  15. 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.

  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

    presents an on-line SI-solvent extraction/back extraction procedure used in connection with detection by either ETAAS or ICPMS. Incorporating two newly designed dual-conical gravitational phase separators, its performance is demonstrated for the determination of various metals in reference materials.......Electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICPMS) are highly sensitive techniques for trace metal analyses. Nevertheless, separation/preconcentration procedures are often called for in order to overcome their inherent low matrix...... 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...

  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

    presents an on-line SI-solvent extraction/back extraction procedure used in connection with detection by either ETAAS or ICPMS. Incorporating two newly designed dual-conical gravitational phase separators, its performance is demonstrated for the determination of various metals in reference materials.......Electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICPMS) are highly sensitive techniques for trace metal analyses. Nevertheless, separation/preconcentration procedures are often called for in order to overcome their inherent low matrix tolerance....... 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...

  18. On-line solid-phase extraction coupled to hydrophilic interaction chromatography-mass spectrometry for the determination of polar drugs.

    Science.gov (United States)

    Fontanals, Núria; Marcé, Rosa M; Borrull, Francesc

    2011-09-02

    The present study describes the first fully automated method based on on-line solid-phase extraction (SPE) coupled to hydrophilic interaction chromatography-electrospray-mass spectrometry (HILIC-(ESI)MS) to determine a group of polar drugs that includes illicit drugs (such as cocaine, morphine, codeine and metabolites) and pharmaceuticals in environmental water samples. The SPE was performed using a highly retentive polymeric sorbent. The HILIC separation was optimised and the initial high organic content of the chromatographic mobile phase, was also suitable for the proper on-line elution of the analytes retained in the SPE column and for enhancing the ESI ionisation efficiency. This method allows the loading of samples of up to 250ml of ultrapure water or 10ml of environmental water samples spiked at low ngl(-1) levels of the analytes. The method yields near 100% recoveries for all the analytes. The method was also validated with environmental water samples with linear ranges from 5 to 1000ngl(-1) and limits of detection ≤2ngl(-1) for most of the compounds. Copyright © 2010 Elsevier B.V. All rights reserved.

  19. On-line solid phase selective separation and preconcentration of Cd(II) by solid-phase extraction using carbon active modified with methyl thymol blue

    Energy Technology Data Exchange (ETDEWEB)

    Ensafi, Ali A. [College of Chemistry, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of)], E-mail: Ensafi@cc.iut.ac.ir; Ghaderi, Ali R. [College of Chemistry, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of)

    2007-09-05

    An on-line flow system was used to develop a selective and efficient on-line sorbent extraction preconcentration system for cadmium. The method is based on adsorption of cadmium ions onto the activated carbon modified with methyl thymol blue. Then the adsorbed ions were washed using 0.5 M HNO{sub 3} and the eluent was used to determine the Cd(II) ions using flame atomic absorption spectrometry. The results obtained show that the modified activated carbon has the greatest adsorption capacity of 80 {mu}g of Cd(II) per 1.0 g of the solid phase. The optimal pH value for the quantitative preconcentration was 9.0 and full desorption is achieved by using 0.5 M HNO{sub 3} solution. It is established that the solid phase can be used repeatedly without a considerable adsorption capacity loss. The detection limit was less than 1 ng mL{sup -1} Cd(II), with an enrichment factor of 1000. The calibration graph was linear in the range of 1-2000 ng mL{sup -1} Cd(II). The developed method has been applied to the determination of trace cadmium (II) in water samples and in the following reference materials: sewage sludge (CRM144R), and sea water (CASS.4) with satisfactory results. The accuracy was assessed through recovery experiments.

  20. On-line solid phase selective separation and preconcentration of Cd(II) by solid-phase extraction using carbon active modified with methyl thymol blue

    International Nuclear Information System (INIS)

    Ensafi, Ali A.; Ghaderi, Ali R.

    2007-01-01

    An on-line flow system was used to develop a selective and efficient on-line sorbent extraction preconcentration system for cadmium. The method is based on adsorption of cadmium ions onto the activated carbon modified with methyl thymol blue. Then the adsorbed ions were washed using 0.5 M HNO 3 and the eluent was used to determine the Cd(II) ions using flame atomic absorption spectrometry. The results obtained show that the modified activated carbon has the greatest adsorption capacity of 80 μg of Cd(II) per 1.0 g of the solid phase. The optimal pH value for the quantitative preconcentration was 9.0 and full desorption is achieved by using 0.5 M HNO 3 solution. It is established that the solid phase can be used repeatedly without a considerable adsorption capacity loss. The detection limit was less than 1 ng mL -1 Cd(II), with an enrichment factor of 1000. The calibration graph was linear in the range of 1-2000 ng mL -1 Cd(II). The developed method has been applied to the determination of trace cadmium (II) in water samples and in the following reference materials: sewage sludge (CRM144R), and sea water (CASS.4) with satisfactory results. The accuracy was assessed through recovery experiments

  1. On-line solid phase selective separation and preconcentration of Cd(II) by solid-phase extraction using carbon active modified with methyl thymol blue.

    Science.gov (United States)

    Ensafi, Ali A; Ghaderi, Ali R

    2007-09-05

    An on-line flow system was used to develop a selective and efficient on-line sorbent extraction preconcentration system for cadmium. The method is based on adsorption of cadmium ions onto the activated carbon modified with methyl thymol blue. Then the adsorbed ions were washed using 0.5M HNO(3) and the eluent was used to determine the Cd(II) ions using flame atomic absorption spectrometry. The results obtained show that the modified activated carbon has the greatest adsorption capacity of 80 microg of Cd(II) per 1.0 g of the solid phase. The optimal pH value for the quantitative preconcentration was 9.0 and full desorption is achieved by using 0.5M HNO(3) solution. It is established that the solid phase can be used repeatedly without a considerable adsorption capacity loss. The detection limit was less than 1 ngmL(-1) Cd(II), with an enrichment factor of 1000. The calibration graph was linear in the range of 1-2000 ngmL(-1) Cd(II). The developed method has been applied to the determination of trace cadmium (II) in water samples and in the following reference materials: sewage sludge (CRM144R), and sea water (CASS.4) with satisfactory results. The accuracy was assessed through recovery experiments.

  2. 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.

  3. Synthesis and application of surface-imprinted activated carbon sorbent for solid-phase extraction and determination of copper (II)

    Science.gov (United States)

    Li, Zhenhua; Li, Jingwen; Wang, Yanbin; Wei, Yajun

    2014-01-01

    A new Cu(II)-imprinted amino-functionalized activated carbon sorbent was prepared by a surface imprinting technique for selective solid-phase extraction (SPE) of Cu(II) prior to its determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). Experimental conditions for effective adsorption of Cu(II) were optimized with respect to different experimental parameters using static and dynamic procedures in detail. Compared with non-imprinted sorbent, the ion-imprinted sorbent had higher selectivity and adsorption capacity for Cu(II). The maximum static adsorption capacity of the ion-imprinted and non-imprinted sorbent for Cu(II) was 26.71 and 6.86 mg g-1, respectively. The relatively selectivity factor values (αr) of Cu(II)/Zn(II), Cu(II)/Ni(II), Cu(II)/Co(II) and Cu(II)/Pb(II) were 166.16, 50.77, 72.26 and 175.77, respectively, which were greater than 1. Complete elution of the adsorbed Cu(II) from Cu(II)-imprinted sorbent was carried out using 2 mL of 0.1 mol L-1 EDTA solution. The relative standard deviation of the method was 2.4% for eleven replicate determinations. The method was validated for the analysis by two certified reference materials (GBW 08301, GBW 08303), the results obtained is in good agreement with standard values. The developed method was also successfully applied to the determination of trace copper in natural water samples with satisfactory results.

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

    International Nuclear Information System (INIS)

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

    1998-10-01

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

  5. 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).

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

    Science.gov (United States)

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

    2016-06-01

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

  7. On-line immunoaffinity solid-phase extraction capillary electrophoresis mass spectrometry using Fab´antibody fragments for the analysis of serum transthyretin.

    Science.gov (United States)

    Pont, Laura; Benavente, Fernando; Barbosa, José; Sanz-Nebot, Victoria

    2017-08-01

    This paper describes an on-line immunoaffinity solid-phase extraction capillary electrophoresis mass spectrometry (IA-SPE-CE-MS) method using an immunoaffinity sorbent with Fab' antibody fragments (Fab'-IA) for the analysis of serum transthyretin (TTR), a homotetrameric protein (M r ~56,000) involved in different types of amyloidosis. The IA sorbent was prepared by covalent attachment of Fab' fragments obtained from a polyclonal IgG antibody against TTR to succinimidyl silica particles. The Fab'-IA-SPE-CE-MS methodology was first established analyzing TTR standard solutions. Under optimized conditions, repeatability and reproducibility were acceptable, the method was linear between 1 and 25µgmL -1 , limits of detection (LODs) were around 0.5µgmL -1 (50-fold lower than by CE-MS, ~25µgmL -1 ) and different TTR conformations were observed (folded and unfolded). The applicability of the developed method to screen for familial amyloidotic polyneuropathy type I (FAP-I), which is the most common hereditary systemic amyloidosis, was evaluated analyzing serum samples from healthy controls and FAP-I patients. For the analysis of sera, the most abundant proteins were precipitated with 5% (v/v) of phenol before Fab'-IA-SPE-CE-MS. The current method enhanced our previous results for the analysis of TTR using intact antibodies immobilized on magnetic beads. It allowed a slight improvement on LODs (2-fold), the detection of proteoforms found at lower concentrations and the preparation of microcartridges with extended durability. Copyright © 2017. Published by Elsevier B.V.

  8. A novel molybdenum disulfide nanosheet self-assembled flower-like monolithic sorbent for solid-phase extraction with high efficiency and long service life.

    Science.gov (United States)

    Ran, Fanpeng; Liu, Hongmei; Wang, Xiaoqi; Guo, Yong

    2017-07-21

    A novel material consisting of molybdenum disulfide (MoS 2 ) nanosheet that self-assemble into flower-like microspheres which aggregate to form a monolithic matrix with a micro or nano-scaled mesopore structure was successfully synthesized and used as an efficient sorbent for solid-phase extraction (SPE) due to its large specific adsorption area and good stability. The extraction properties of the as-prepared sorbent were evaluated by high-performance liquid chromatography with variable wavelength detection (HPLC-VWD) by analyzing four flavonoids (apigenin, quercetin, luteolin, and kaempferol). Under optimal conditions, the LODs and LOQs were found to be in the ranges of 0.1-0.25 and 0.4-0.5μgL -1 , respectively, and wide linear ranges were obtained with correlation coefficients (R) ranging from 0.9991 to 0.9996. Compared with commercial C18 and Alumina-N sorbents, the as-prepared sorbent showed high extraction efficiency at different concentrations of flavonoids. After 100 uses, the extraction ability of the self-assembled MoS 2 nanosheet monolithic sorbent had no evident decline, denoting a long service life. Finally, the SPE-HPLC-VWD method using the as-prepared sorbent was applied to flavonoid analysis in beverage samples with satisfactory results. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Effects of dissolved organic matter (DOM) sources and nature of solid extraction sorbent on recoverable DOM composition: Implication into potential lability of different compound groups.

    Science.gov (United States)

    Chen, Meilian; Kim, Sunghwan; Park, Jae-Eun; Kim, Hyun Sik; Hur, Jin

    2016-07-01

    Noting the source-dependent properties of dissolved organic matter (DOM), this study explored the recoverable compounds by solid phase extraction (SPE) of two common sorbents (C18 and PPL) eluted with methanol solvent for contrasting DOM sources via fluorescence excitation-emission matrix coupled with parallel factor analysis (EEM-PARAFAC) and Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS). Fresh algae and leaf litter extracts DOM, one riverine DOM, and one upstream lacustrine DOM were selected for the comparison. C18 sorbent was generally found to extract more diverse molecular formula, relatively higher molecular weight, and more heteroatomic DOM compounds within the studied mass range than PPL sorbent except for the leaf litter extract. Even with the same sorbent, the main molecular features of the two end member DOM were distributed on different sides of the axes of a multivariate ordination, indicating the source-dependent characteristics of the recoverable compounds by the sorbents. In addition, further examination of the molecular formula uniquely present in the two end members and the upstream lake DOM suggested that proteinaceous, tannin-like, and heteroatomic DOM constituents might be potential compound groups which are labile and easily degraded during their mobilization into downstream watershed. This study provides new insights into the sorbent selectivity of DOM from diverse sources and potential lability of various compound groups.

  10. 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

  11. Miniaturized solid-phase extraction of macrolide antibiotics in honey and bovine milk using mesoporous MCM-41 silica as sorbent.

    Science.gov (United States)

    Du, Li-Jing; Yi, Ling; Ye, Li-Hong; Chen, Yu-Bo; Cao, Jun; Peng, Li-Qing; Shi, Yu-Ting; Wang, Qiu-Yan; Hu, Yu-Han

    2018-02-16

    A simple and effective method of miniaturized solid-phase extraction (mini-SPE) was developed for the simultaneous purification and enrichment of macrolide antibiotics (MACs) (i.e. azithromycin, clarithromycin, erythromycin, lincomycin and roxithromycin) from honey and skim milk. Mesoporous MCM-41 silica was synthesized and used as sorbent in mini-SPE. Several key parameters affecting the performance of mini-SPE procedure were thoroughly investigated, including sorbent materials, amount of sorbent and elution solvents. Under the optimized condition, satisfactory linearity (r 2  > 0.99), acceptable precision (RSDs, 0.3-7.1%), high sensitivity (limit of detection in the range of 0.01-0.76 μg/kg), and good recoveries (83.21-105.34%) were obtained. With distinct advantages of simplicity, reliability and minimal sample requirement, the proposed mini-SPE procedure coupled with ultrahigh performance liquid chromatography and quadrupole time-of-flight tandem mass spectrometry could become an alternative tool to analyze the residues of MACs in complex food matrixes. Copyright © 2018 Elsevier B.V. All rights reserved.

  12. An on-line coupling of nanofibrous extraction with column-switching high performance liquid chromatography - A case study on the determination of bisphenol A in environmental water samples.

    Science.gov (United States)

    Háková, Martina; Chocholoušová Havlíková, Lucie; Chvojka, Jiří; Solich, Petr; Šatínský, Dalibor

    2018-02-01

    Polyamide 6 nanofiber polymers were used as modern sorbents for on-line solid phase extraction (SPE) coupled with liquid chromatography. The on-line SPE system was tested for the determination of bisphenol A in river water samples. Polyamide nanofibers were prepared using needleless electrospinning, inserted into a mini-column cartridge (5 × 4.6mm) and coupled with HPLC. The effect of column packing and the amount of polyamide 6 on extraction efficiency was tested and the packing process was optimized. The proposed method was performed using a 50-µL sample injection followed by an on-line nanofibrous extraction procedure. The influence of the washing mobile phase on the retention of bisphenol A during the extraction procedure was evaluated. Ascentis ® Express C18 (10cm × 4.6mm) core-shell column was used as an analytical column. Fluorescence detection wavelengths (λ ex = 225nm and λ em = 320nm) were used for identification and quantification of Bisphenol A in river waters. The linearity was tested in the range from 2 to 500µgL -1 (using nine calibration points). The limits of detection and quantification were 0.6 and 2µgL -1 , respectively. The developed method was successfully used for the determination of bisphenol A in various samples of river waters in the Czech Republic (The Ohře, Labe, Nisa, Úpa, and Opava Rivers). Copyright © 2017 Elsevier B.V. All rights reserved.

  13. On-line supercritical fluid extraction-supercritical fluid chromatography-mass spectrometry of polycyclic aromatic hydrocarbons in soil.

    Science.gov (United States)

    Wicker, A Paige; Carlton, Doug D; Tanaka, Kenichiro; Nishimura, Masayuki; Chen, Vivian; Ogura, Tairo; Hedgepeth, William; Schug, Kevin A

    2018-06-01

    On-line supercritical fluid extraction - supercritical fluid chromatography - mass spectrometry (SFE-SFC-MS) has been applied for the determination of polycyclic aromatic hydrocarbons (PAHs) in soil. The purpose of this study was to develop and validate the first on-line SFE-SFC-MS method for the quantification of PAHs in various types of soil. By coupling the sample extraction on-line with chromatography and detection, sample preparation is minimized, diminishing sample loss and contamination, and significantly decreasing the required extraction time. Parameters for on-line extraction coupled to chromatographic analysis were optimized. The method was validated for concentrations of 10-1500 ng of PAHs per gram of soil in Certified Reference Material (CRM) sediment, clay, and sand with R 2  ≥ 0.99. Limits of detection (LOD) were found in the range of 0.001-5 ng/g, and limits of quantification (LOQ) in the range of 5-15 ng/g. The method developed in this study can be effectively applied to the study of PAHs in the environment, and may lay the foundation for further applications of on-line SFE-SFC-MS. Copyright © 2018 Elsevier B.V. All rights reserved.

  14. 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

  15. 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. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. Solid-phase extraction sorbent consisting of alkyltrimethylammonium surfactants immobilized onto strong cation-exchange polystyrene resin.

    Science.gov (United States)

    Reid, Kendra R; Kennedy, Lonnie J; Crick, Eric W; Conte, Eric D

    2002-10-25

    Presented is a solid-phase extraction sorbent material composed of cationic alkyltrimethylammonium surfactants attached to a strong cation-exchange resin via ion-exchange. The original hydrophilic cation-exchange resin is made hydrophobic by covering the surface with alkyl chains from the hydrophobic portion of the surfactant. The sorbent material now has a better ability to extract hydrophobic molecules from aqueous samples. The entire stationary phase (alkyltrimethylammonium surfactant) is removed along with the analyte during the elution step. The elution step requires a mild elution solvent consisting of 0.25 M Mg2+ in a 50% 2-propanol solution. The main advantage of using a removable stationary phase is that traditionally utilized toxic elution solvents such as methylene chloride, which are necessary to efficiently release strongly hydrophobic species from SPE stationary phases, may now be avoided. Also, the final extract is directly compatible with reversed-phase liquid chromatography. The performance of this procedure is presented using pyrene as a test molecule.

  17. Determination of inorganic arsenic in algae using bromine halogenation and on-line nonpolar solid phase extraction followed by hydride generation atomic fluorescence spectrometry.

    Science.gov (United States)

    Zhang, Weihong; Qi, Yuehan; Qin, Deyuan; Liu, Jixin; Mao, Xuefei; Chen, Guoying; Wei, Chao; Qian, Yongzhong

    2017-08-01

    Accurate, stable and fast analysis of toxic inorganic arsenic (iAs) in complicated and arsenosugar-rich algae matrix is always a challenge. Herein, a novel analytical method for iAs in algae was reported, using bromine halogenation and on-line nonpolar solid phase extraction (SPE) followed by hydride generation atomic fluorescence spectrometry (HG-AFS). The separation of iAs from algae was first performed by nonpolar SPE sorbent using Br - for arsenic halogenation. Algae samples were extracted with 1% perchloric acid. Then, 1.5mL extract was reduced by 1% thiourea, and simultaneously reacted (for 30min) with 50μL of 10% KBr for converting iAs to AsBr 3 after adding 3.5mL of 70% HCl to 5mL. A polystyrene (PS) resin cartridge was employed to retain arsenicals, which were hydrolyzed, eluted from the PS resin with H 2 O, and categorized as iAs. The total iAs was quantified by HG-AFS. Under optimum conditions, the spiked recoveries of iAs in real algae samples were in the 82-96% range, and the method achieved a desirable limit of detection of 3μgkg -1 . The inter-day relative standard deviations were 4.5% and 4.1% for spiked 100 and 500μgkg -1 respectively, which proved acceptable for this method. For real algae samples analysis, the highest presence of iAs was found in sargassum fusiforme, followed by kelp, seaweed and laver. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. 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.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

    Highlights: ► The use of CNTs as sorbent for metal species in solid phase extraction has been described. ► Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. ► 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.

  20. Determination of major aromatic constituents in vanilla using an on-line supercritical fluid extraction coupled with supercritical fluid chromatography.

    Science.gov (United States)

    Liang, Yanshan; Liu, Jiaqi; Zhong, Qisheng; Shen, Lingling; Yao, Jinting; Huang, Taohong; Zhou, Ting

    2018-04-01

    An on-line supercritical fluid extraction coupled with supercritical fluid chromatography method was developed for the determination of four major aromatic constituents in vanilla. The parameters of supercritical fluid extraction were systematically investigated using single factor optimization experiments and response surface methodology by a Box-Behnken design. The modifier ratio, split ratio, and the extraction temperature and pressure were the major parameters which have significant effects on the extraction. While the static extraction time, dynamic extraction time, and recycle time had little influence on the compounds with low polarity. Under the optimized conditions, the relative extraction efficiencies of all the constituents reached 89.0-95.1%. The limits of quantification were in the range of 1.123-4.747 μg. The limits of detection were in the range of 0.3368-1.424 μg. The recoveries of the four analytes were in the range of 76.1-88.9%. The relative standard deviations of intra- and interday precision ranged from 4.2 to 7.6%. Compared with other off-line methods, the present method obtained higher extraction yields for all four aromatic constituents. Finally, this method has been applied to the analysis of vanilla from different sources. On the basis of the results, the on-line supercritical fluid extraction-supercritical fluid chromatography method shows great promise in the analysis of aromatic constituents in natural products. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. A polyaniline-magnetite nanocomposite as an anion exchange sorbent for solid-phase extraction of chromium(VI) ions

    International Nuclear Information System (INIS)

    Rezvani, Mehdi; Asgharinezhad, Ali Akbar; Ebrahimzadeh, Homeira; Shekari, Nafiseh

    2014-01-01

    This work describes a novel polyaniline-magnetite nanocomposite and its application to the preconcentration of Cr(VI) anions. The material was obtained by oxidative polymerization of aniline in the presence of magnetite nanoparticles. The parameters affecting preconcentration were optimized by a Box-Behnken design through response surface methodology. Extraction time, amount of magnetic sorbent and pH value were selected as the main factors affecting sorption. The sorption capacity of the sorbent for Cr(VI) is 54 mg g −1 . The type, volume and concentration of the eluents, and the elution time were selected as main factors in the optimization study of the elution step. Following sorption and elution, the Cr(VI) ions were reacted with diphenylcarbazide, and the resulting dye was quantified by HPLC with optical detection at 546 nm. The limit of detection is 0.1 μg L −1 , and all the relative standard deviations are <6.3 %. The nanocomposite was successfully applied to the rapid extraction and determination of trace quantities of Cr(VI) ions in spiked water samples. (author)

  2. Carbon Nanotubes as a New Solid Phase Extraction Sorbent for Analysis of Environmental Pollutants

    OpenAIRE

    Constantin, Bele

    2010-01-01

    SPE is an increasingly useful technique for sample concentration and clean-up in environmental applications and can be easily incorporated into automated analytical procedures. The future of SPE is closely related to improvement of sorbents that can be more effective in obtaining high enrichment efficiency of analytes. The unusual properties of CNTs, their large sorption capacity, wide surface area and the presence of a wide spectrum of surface functional groups have generated a great interes...

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

    International Nuclear Information System (INIS)

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

    2016-01-01

    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

  4. 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

  5. Combining cationic and anionic mixed-mode sorbents in a single cartridge to extract basic and acidic pharmaceuticals simultaneously from environmental waters.

    Science.gov (United States)

    Salas, Daniela; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa Maria

    2018-01-01

    The aim of the present study is to broaden the applications of mixed-mode ion-exchange solid-phase extraction sorbents to extract both basic and acidic compounds simultaneously by combining the sorbents in a single cartridge and developing a simplified extraction procedure. Four different cartridges containing negative and positive charges in the same configuration were evaluated and compared to extract a group of basic, neutral, and acidic pharmaceuticals selected as model compounds. After a thorough optimization of the extraction conditions, the four different cartridges showed to be capable of retaining basic and acidic pharmaceuticals simultaneously through ionic interactions, allowing the introduction of a washing step with 15 mL methanol to eliminate interferences retained by hydrophobic interactions. Using the best combined cartridge, a method was developed, validated, and further applied to environmental waters to demonstrate that the method is promising for the extraction of basic and acidic compounds from very complex samples.

  6. Aerogel sorbents

    Energy Technology Data Exchange (ETDEWEB)

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

    2018-04-03

    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.

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

    Science.gov (United States)

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

    2018-01-01

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

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

    Science.gov (United States)

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

    2014-11-21

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

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

    NARCIS (Netherlands)

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

    1989-01-01

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

  10. 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...... of the operational times from days to hours, highly temporal resolution of the leaching process, and the capability for immediate decision for stopping or proceeding with the ongoing extraction. Very importantly, accurate determination of the various orthophosphate pools is ensured by minimization of the hydrolysis...... of extracted organic phosphorus and condensed inorganic phosphates within the time frame of the assay. The potential of the novel system for accommodation of the harmonized protocol from the Standards, Measurement and Testing (SMT) Program of the Commission of the European Communities for inorganic phosphorus...

  11. On-line Incorporation of Cloud Point Extraction in Flame Atomic Absorption Spectrometric Determination of Silver

    OpenAIRE

    DALALI, Nasser; JAVADI, Nasrin; AGRAWAL, Yadvendra KUMAR

    2008-01-01

    A cloud point extraction method was incorporated into a flow injection system, coupled with flame atomic absorption spectrometry, for determination of trace amounts of silver. The analyte in the aqueous solution was acidified with 0.2 mol L-1 sulfuric acid and complexed with dithizone. The cloud point extraction was performed using the non-ionic surfactant Triton X-114. After obtaining the cloud point, the surfactant-rich phase containing the dithizonate complex was collected in a m...

  12. Sorbent suppliers

    International Nuclear Information System (INIS)

    Vedder, M.

    1994-01-01

    Sorbents are used to absorb or contain spilled and leaking chemicals, oils, lubricants and other process fluids. They are commonly used around the base of machinery in industrial applications, and in remediating oil spills on land and water. Sorbents are made from biodegradable, inorganic or synthetic materials. Organic materials include corn cobs, wood pulp, paper fiber and cotton. Inorganic materials include clay, perlite, expanded silicates and expanded mica. Synthetic sorbents are made from petroleum- or plastic-based materials such as polyurethane, polyethylene or polypropylene. Sorbents are available in a variety of forms, including pads, rolls, booms, pillows and loose particulate

  13. On-line gross alpha radiation monitoring of natural waters with extractive scintillating resins

    International Nuclear Information System (INIS)

    Hughes, Lara; De Vol, T.A.

    2003-01-01

    Extractive scintillating resins, which are used to simultaneously separate and quantify radioactivity in aqueous solutions, were developed for low-level alpha radiation monitoring of natural waters. Resins were investigated with bis(2-ethylhexyl)methane-diphosphonic acid (H 2 DEH[MDP], Dipex[reg]) extractant, which has a strong affinity for tri-, tetra- and hexavalent actinides in dilute acids. Extractive scintillating resins were manifested (1) as a mixed bed of scintillating resin and extraction chromatographic resin and (2) by diffusing the organic fluor 2-(1-naphtyl)-5-phenyloxazole into macroporous polystyrene chromatographic resin, then coating with H 2 DEH[MDP], or by coating H 2 DEH[MDP] on scintillating polyvinyltoluene beads. The scintillation light was detected with a modified Hidex Triathler to allow for continuous flow measurements. The average detection efficiencies were 51.7±2.6% and 65.8±10.1% for natural uranium and 241 Am, respectively, for the extractant coated scintillator. The resin was stable for solution flow of up to 1000 ml resulting in rapid real-time quantification of natural uranium in groundwater down to 30 μg/ml

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

    OpenAIRE

    MacFarlane, John D.

    1997-01-01

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

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

  16. Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD) and Dispersive Solid Phase Extraction (d-SPE) of Plant Samples

    Science.gov (United States)

    Sowa, Ireneusz; Wójciak-Kosior, Magdalena; Strzemski, Maciej; Sawicki, Jan; Staniak, Michał; Dresler, Sławomir; Szwerc, Wojciech; Mołdoch, Jarosław; Latalski, Michał

    2018-01-01

    Polyaniline (PANI) is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME). In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI) was used for dispersive solid phase extraction (d-SPE) and matrix solid–phase extraction (MSPD). The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD) quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples. PMID:29565297

  17. Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD and Dispersive Solid Phase Extraction (d-SPE of Plant Samples

    Directory of Open Access Journals (Sweden)

    Ireneusz Sowa

    2018-03-01

    Full Text Available Polyaniline (PANI is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME. In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI was used for dispersive solid phase extraction (d-SPE and matrix solid–phase extraction (MSPD. The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples.

  18. 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

    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...... loop, the content of which is subsequently introduced into the ICP-MS, via a direct injection high efficiency nebulizer (DIHEN), for quantification. Enrichment factors of 29.6 (Cu) and 23.3 (Pb), detection limits of 17 ng/l (Cu) and 11 ng/l (Pb), along with a sampling frequency of 13 s/h were obtained...

  19. Survey of Heavy Metal Contamination in Water Sources in the Municipality of Torola, El Salvador, through In Situ Sorbent Extraction

    Directory of Open Access Journals (Sweden)

    Enriqueta Anticó

    2017-11-01

    Full Text Available The presence of heavy metals in water resources directly affects consumer health. The quality of surface water resources in Central America is usually low due to the presence of metals and other pollutants. The lack of analytical instrumentation to perform routine monitoring of water has encouraged the development of easy tools to facilitate the determination of heavy metals in waters in remote sites. In this study, we evaluated the use of different sorbents, such as Adsorbsia As600 (titanium dioxide, Iontosorb Oxin, 8-hydroxyquinoline bearing functional groups, and Duolite GT-73, with thiol functionality, for Cd, Ni, Cu, Zn, and Al extraction. It was found that both Adsorbsia As600 and Iontosorb Oxin allowed the adsorption of all metals, and the recovery was achieved using either HCl or ethylenediaminetetraacetic sodium salt (EDTA solutions. Hence, Adsorbsia As600 was employed for in situ sampling in the metal contamination evaluation of water samples (from 15 wells and nine storage tanks from the municipality of Torola, Mozarán, El Salvador. The developed procedure allowed all the metals in the samples to be detected, and Ni and Al were found to be above Salvadoran guidelines for drinking water quality.

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

    International Nuclear Information System (INIS)

    Chen Ligang; Ding Lan; Jin Haiyan; Song Daqian; Zhang Huarong; Li Jiantao; Zhang Kun; Wang Yutang; Zhang Hanqi

    2007-01-01

    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 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 -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 -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

  1. Octadecyl functionalized core-shell magnetic silica nanoparticle as a powerful nanocomposite sorbent to extract urinary volatile organic metabolites.

    Science.gov (United States)

    Qiao, Zheng; Perestrelo, Rosa; Reyes-Gallardo, Emilia M; Lucena, R; Cárdenas, S; Rodrigues, João; Câmara, José S

    2015-05-08

    In this present study, magnetic Fe3O4@SiO2 nanoparticles (MNPs) functionalized with octadecyl groups (Fe3O4@SiO2-C18 NPs) were synthesized, characterized and employed, for the first time, as powerful nanosorbent to extract endogenous volatile organic metabolites (EVOMs) namely, hexanal, heptanal, decanal, benzaldehyde, 4-heptanone, 5-methyl-2-furfural and phenol, described as potential biomarkers of cancer, from human urine. By using co-precipitation, surface modification methods, the carbon-ferromagnetic nanocomposite was synthesized and characterized by infrared spectrum (IR) and transmission electron microscopy (TEM). By coupling with gas chromatography-mass spectrometry (GC-qMS), a reliable, sensitive and cost-effective method was validated. To test the extraction efficiency of the carbon-ferromagnetic nanocomposite toward urinary EVOMs experimental variables affecting the extraction performance, including nanosorbent amount, adsorption time, elution time, and nature of elution solvent, were investigated in detail. The extraction process was performed by dispersing Fe3O4@SiO2-C18 NPs into working solution containing targeted VOMs, and into urine samples, and then eluted with an adequate organic solvent. The eluate was collected, concentrated and analyzed by GC-qMS. Under the optimized conditions, the LODs and LOQs achieved were in the range of 9.7-57.3 and 32.4-190.9ng/mL, respectively. Calibration curves were linear (r(2)≥0. 988) over the concentration ranges from 0.25 to 250ng/mL. In addition, a satisfying reproducibility was achieved by evaluating the intra- and inter-day precisions with relative standard deviations (RSDs) less than 3 and 11%, respectively. The method also afforded satisfactory results in terms of the matrix effect (72.8-96.1%) and recoveries (accuracy) higher than 75.1% for most of the studied EVOMs. The Fe3O4@SiO2-C18 NPs-based sorbent extraction combined with GC-qMS revealed that the new nanosorbent had a strong ability to retain the

  2. Quantitation of promethazine and metabolites in urine samples using on-line solid-phase extraction and column-switching

    Science.gov (United States)

    Song, Q.; Putcha, L.; Harm, D. L. (Principal Investigator)

    2001-01-01

    A chromatographic method for the quantitation of promethazine (PMZ) and its three metabolites in urine employing on-line solid-phase extraction and column-switching has been developed. The column-switching system described here uses an extraction column for the purification of PMZ and its metabolites from a urine matrix. The extraneous matrix interference was removed by flushing the extraction column with a gradient elution. The analytes of interest were then eluted onto an analytical column for further chromatographic separation using a mobile phase of greater solvent strength. This method is specific and sensitive with a range of 3.75-1400 ng/ml for PMZ and 2.5-1400 ng/ml for the metabolites promethazine sulfoxide, monodesmethyl promethazine sulfoxide and monodesmethyl promethazine. The lower limits of quantitation (LLOQ) were 3.75 ng/ml with less than 6.2% C.V. for PMZ and 2.50 ng/ml with less than 11.5% C.V. for metabolites based on a signal-to-noise ratio of 10:1 or greater. The accuracy and precision were within +/- 11.8% in bias and not greater than 5.5% C.V. in intra- and inter-assay precision for PMZ and metabolites. Method robustness was investigated using a Plackett-Burman experimental design. The applicability of the analytical method for pharmacokinetic studies in humans is illustrated.

  3. 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.

  4. Evaluation of ultrasound-assisted in situ sorbent formation solid-phase extraction method for determination of arsenic in water, food and biological samples.

    Science.gov (United States)

    Ezoddin, Maryam; Majidi, Behrooz; Abdi, Khosrou

    2015-01-01

    A simple and rapid ultrasound-assisted in situ sorbent formation solid-phase extraction (UAISFSPE) coupled with electrothermal atomic absorption spectrometry detection (ET-AAS) was developed for preconcentration and determination of arsenic (As) in various samples. A small amount of cationic surfactant is dissolved in the aqueous sample containing As ions, which were complexed by ammonium pyrrolidinedithiocarbamate After shaking, a little volume of hexafluorophosphate (NaPF6) as an ion-pairing agent was added into the solution by a microsyringe. Due to the interaction between surfactant and ion-pairing agent, solid particles are formed. The alkyl groups of the surfactant in the solid particles strongly interact with the hydrophobic groups of analytes and become bound. Sonication aids the dispersion of the sorbent into the sample solution and mass transfer of the analyte into the sorbent, thus reducing the extraction time. The solid particles are centrifuged, and the sedimented particles can be dissolved in an appropriate solvent to recover the absorbed analyte. After separation, total arsenic (As(III) and As(V)) was determined by ET-AAS. Several experimental parameters were investigated and optimized. A detection limit of 7 ng L(-1) with preconcentration factor of 100 and relative standard deviation for 10 replicate determinations of 0.1 µg L(-1) As(III) were 4.5% achieved. Consequently, the method was applied to the determination of arsenic in certified reference materials, water, food and biological samples with satisfactory results.

  5. Comparison of several solid-phase extraction sorbents for continuous determination of amines in water by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Jurado-Sánchez, Beatriz; Ballesteros, Evaristo; Gallego, Mercedes

    2009-08-15

    A semiautomatic method has been proposed for the determination of different types of amines in water samples including anilines, chloroanilines, N-nitrosamines and aliphatic amines. The analytes were retained on a solid-phase extraction sorbent column and after elution, 1 microL of the extract was analysed by gas chromatography coupled with electron impact ionization mass spectrometry. A systematic overview is given of the advantages and disadvantages of several sorbents (LiChrolut EN, Oasis HLB, RP-C(18), graphitized carbon black, fullerenes and nanotubes) in the retention of amine compounds and based on sensitivity, selectivity and reliability. The retention efficiency for the studied amines was higher (ca. 100%) with LiChrolut EN and Oasis HLB than it was with RP-C(18) and fullerenes (53 and 62%, respectively, on average). Detection limits of 0.5-16 ng L(-1) for the 27 amines studied were obtained when using a sorbent column containing 75 mg of LiChrolut EN for 100mL of sample, the RSD being lower than 6.5%. The method was applied with good accuracy and precision in the determination of amines in various types of water including river, pond, tap, well, drinking, swimming pool and waste.

  6. 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.

  7. 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

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

    International Nuclear Information System (INIS)

    Lin, Wenbin

    2017-01-01

    Climate disruption is one of the greatest crises the global community faces in the 21st century. Alarming increases in CO_2, NO, SO_2 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 extraction from seawater

  9. Preconcentration of Trace Neonicotinoid Insecticide Residues Using Vortex-Assisted Dispersive Micro Solid-Phase Extraction with Montmorillonite as an Efficient Sorbent

    Directory of Open Access Journals (Sweden)

    Khwankaew Moyakao

    2018-04-01

    Full Text Available In this work, we investigated montmorillonite for adsorption of neonicotinoid insecticides in vortex-assisted dispersive micro-solid phase extraction (VA-d-μ-SPE. High-performance liquid chromatography with photodiode array detection was used for quantification and determination of neonicotinoid insecticide residues, including thiamethoxam, clothianidin, imidacloprid, acetamiprid, and thiacloprid. In this method, the solid sorbent was dispersed into the aqueous sample solution and vortex agitation was performed to accelerate the extraction process. Finally, the solution was filtered from the solid sorbent with a membrane filter. The parameters affecting the extraction efficiency of the proposed method were optimized, such as amount of sorbent, sample volume, salt addition, type and volume of extraction solvent, and vortex time. The adsorbing results show that montmorillonite could be reused at least 4 times and be used as an effective adsorbent for rapid extraction/preconcentration of neonicotinoid insecticide residues. Under optimum conditions, linear dynamic ranges were achieved between 0.5 and 1000 ng mL−1 with a correlation of determination (R2 greater than 0.99. Limit of detection (LOD ranged from 0.005 to 0.065 ng mL−1, while limit of quantification (LOQ ranged from 0.008 to 0.263 ng mL−1. The enrichment factor (EF ranged from 8 to 176-fold. The results demonstrated that the proposed method not only provided a more simple and sensitive method, but also can be used as a powerful alternative method for the simultaneous determination of insecticide residues in natural surface water and fruit juice samples.

  10. 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

  11. 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.

  12. The carbonaceous sorbent based on the secondary silica-containing material from oil extraction industry

    Science.gov (United States)

    Starostina, I. V.; Stolyarov, D. V.; Anichina, Ya N.; Porozhnyuk, E. V.

    2018-01-01

    The object of research in this work is the silica-containing waste of oil extraction industry - the waste kieselghur (diatomite) sludge from precoat filtering units, used for the purification of vegetable oils from organic impurities. As a result of the thermal modification of the sludge, which contains up to 70% of organic impurities, a finely-dispersed low-porous carbonaceous mineral sorption material is formed. The modification of the sludge particles surface causes the substantial alteration of its physical, chemical, adsorption and structural properties - the organic matter is charred, the particle size is reduced, and on the surface of diatomite particles a carbon layer is formed, which deposits in macropores and partially occludes them. The amount of mesopores is increased, along with the specific surface of the obtained product. The optimal temperature of sludge modification is 500°C. The synthesized carbonaceous material can be used as an adsorbing agent for the purification of wastewater from heavy metal ions. The sorption capacity of Cu2+ ions amounted to 14.2 mg·g-1 and for Ni2+ ions - 17.0 mg·g-1. The obtained values exceed the sorption capacity values of the initial kieselghur, used as a filtering charge, for the researched metal ions.

  13. The role of graphene-based sorbents in modern sample preparation techniques.

    Science.gov (United States)

    de Toffoli, Ana Lúcia; Maciel, Edvaldo Vasconcelos Soares; Fumes, Bruno Henrique; Lanças, Fernando Mauro

    2018-01-01

    The application of graphene-based sorbents in sample preparation techniques has increased significantly since 2011. These materials have good physicochemical properties to be used as sorbent and have shown excellent results in different sample preparation techniques. Graphene and its precursor graphene oxide have been considered to be good candidates to improve the extraction and concentration of different classes of target compounds (e.g., parabens, polycyclic aromatic hydrocarbon, pyrethroids, triazines, and so on) present in complex matrices. Its applications have been employed during the analysis of different matrices (e.g., environmental, biological and food). In this review, we highlight the most important characteristics of graphene-based material, their properties, synthesis routes, and the most important applications in both off-line and on-line sample preparation techniques. The discussion of the off-line approaches includes methods derived from conventional solid-phase extraction focusing on the miniaturized magnetic and dispersive modes. The modes of microextraction techniques called stir bar sorptive extraction, solid phase microextraction, and microextraction by packed sorbent are discussed. The on-line approaches focus on the use of graphene-based material mainly in on-line solid phase extraction, its variation called in-tube solid-phase microextraction, and on-line microdialysis systems. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Humic acid-bonded silica as a novel sorbent for solid-phase extraction of benzo[a]pyrene in edible oils

    International Nuclear Information System (INIS)

    Luo Dan; Yu Qiongwei; Yin Hongrui; Feng Yuqi

    2007-01-01

    A novel solid-phase extraction (SPE) sorbent, humic acid-bonded silica (HAS), was prepared. Humic acids (HAs) were grafted onto silica matrices via an amide linkage between humyl chloride and the amido terminus of 3-aminopropyltrimethoxysilane (APTS)-silica gel. The resulting material was characterized by Fourier transform infrared spectrometer, elemental analysis, and nitrogen adsorption analysis. This sorbent exhibits an excellent adsorption capacity for some electron-abundant analytes owing to its peculiar structure. In this paper, we choose benzo[a]pyrene (BaP) in oil as a probe to validate the adsorption capacity of the material. Thus a fast, cheap and simple SPE method with humic acid-bonded silica cartridge for edible oil clean-up, followed by high-performance liquid chromatography (HPLC) with fluorescence detection was established. The effects of experimental variables, such as washing and elution solvents, and the amount of sorbents have been studied. The recoveries of BaP in edible oils spiked at 0.2-100 μg kg -1 were in the range of 78.8-102.7% with relative standard deviations ranging between 1.3 and 9.3%; the limit of detection was -0.06 μg kg -1

  15. 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). Copyright © 2011 Elsevier B.V. All rights reserved.

  16. 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

  17. Evaluation of graphene-based sorbent in the determination of polar environmental contaminants in water by micro-solid phase extraction-high performance liquid chromatography.

    Science.gov (United States)

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

    2016-01-04

    A facile method of extraction using porous membrane protected micro-solid phase extraction (μ-SPE) with a graphene-based sorbent followed by high performance liquid chromatography-ultraviolet detector was developed. The reduced graphene oxide (r-GO) (1mg), synthesized from graphite oxide, was enclosed in a polypropylene bag representing the μ-SPE device, which was used for the extraction of estrogens such as estrone, 17β-estradiol, 17α-ethynylestradiol and diethylstilbestrol in water. The r-GO obtained was identified and characterized by Fourier transform infrared, transmission electron microscopy, scanning electron microscopy and thermogravimetric analysis. The sorbent was loaded with sodium dodecyl sulfate by sonication to prevent agglomeration in aqueous solution. With this method, low limits of detection of between 0.24 and 0.52 ng L(-1) were achieved. For estrogen analysis a linear calibration range of 0.01-100 μg L(-1) was obtained, with the coefficients of determination (r(2)) higher than 0.992. This proposed method was successfully applied to determine estrogens in water. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. Polythiophene-coated Fe{sub 3}O{sub 4} superparamagnetic nanocomposite: Synthesis and application as a new sorbent for solid-phase extraction

    Energy Technology Data Exchange (ETDEWEB)

    Tahmasebi, Elham [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Yamini, Yadollah, E-mail: yyamini@modares.ac.ir [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Moradi, Morteza; Esrafili, Ali [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of)

    2013-04-03

    Graphical abstract: In the present work, polythiophene-coated Fe{sub 3}O{sub 4} nanoparticles (Fe{sub 3}O{sub 4}@PTh NPs) have been successfully synthesized. The synthesized Fe{sub 3}O{sub 4}@PTh NPs were applied as an efficient sorbent for extraction and pre-concentration of several typical plasticizer compounds from environmental water samples. Highlights: ► A novel polythiophene-coated Fe{sub 3}O{sub 4} nanoparticles (Fe{sub 3}O{sub 4}@PTh NPs) was synthesized. ► The synthesized Fe{sub 3}O{sub 4}@PTh NPs were characterized by using different instruments. ► The Fe{sub 3}O{sub 4}@PTh NPs were applied as a sorbent for extraction of several plasticizers. ► After extraction, separation of NPs from solution was achieved by a magnetic field. ► The proposed procedure was applied to analysis of the analytes in real water samples. -- Abstract: In the present work, a novel type of superparamagnetic nanosorbent, polythiophene-coated Fe{sub 3}O{sub 4} nanoparticles (Fe{sub 3}O{sub 4}@PTh NPs), have been successfully synthesized. The synthesized NPs were characterized by scanning electron microscopy (SEM), Fourier transform-infrared (FT-IR) spectroscopy, and thermal gravimetric analysis (TGA). The synthesized Fe{sub 3}O{sub 4}@PTh NPs were applied as an efficient sorbent for extraction and preconcentration of several typical plasticizer compounds (di-n-butyl phthalate (DBP), di-(2-ethylhexyl) phthalate (DEHP), and dioctyl adipate (DOA)) from environmental water samples. Separation of Fe{sub 3}O{sub 4}@PTh NPs from the aqueous solution was simply achieved by applying external magnetic field. Separation and determination of the extracted plasticizers was performed by gas chromatography–flame ionization detection (GC–FID). Several variables affecting the extraction efficiency of the analytes i.e., amount of NPs sorbent, salt concentration, extraction time, and desorption conditions were investigated and optimized. The best working conditions were as follows: amount

  19. Quaternary ammonium-functionalized MCM-48 mesoporous silica as a sorbent for the dispersive solid-phase extraction of endocrine disrupting compounds in water.

    Science.gov (United States)

    Zhang, Shijuan; Lu, Fengli; Ma, Xiaoyun; Yue, Mingbo; Li, Yanxin; Liu, Jiammin; You, Jinmao

    2018-07-06

    MCM-48 mesoporous silica was functionalized with dimethyloctadecyl[3-(trimethoxysilyl)propyl]ammonium chloride, a quaternary ammonium salt with a long hydrophobic chain, to prepare a new sorbent for the dispersive solid-phase extraction (DSPE) of seven endocrine disrupting compounds (EDCs) including 4-hexylphenol, 4-octylphenol, 4-nonylphenol, bisphenol A, estrone, 17β-estradiol and estriol in water. A series of differently functionalized MCM-48 materials were also synthesized, and they served as reference materials to study the mechanism. The developed DSPE method was combined with HPLC with fluorescence detection to evaluate the adsorption performance. The results indicated that the quaternary ammonium-functionalized MCM-48 mesoporous silica can be used as ideal sorbent for EDCs in water with recoveries of higher than 95% due to the electrostatic interactions and hydrophobic effect. Hydrogen bonding and π-π interactions in other synthesized materials could lead to about 25-30% increase in recoveries, but the results for polyhydroxy compounds were still not satisfying. The quaternary ammonium-functionalized MCM-48 mesoporous silica was successfully applied to the DSPE of EDCs in real water samples. The optimum extraction conditions were sorbent amount, 15 mg; desorption time; 5 min; elution volume, 0.8 mL; sample pH 3.0; and salt addition, 5 g/L. The limits of detection were in the range of 1.2-2.6 ng/L, while the limits of quantitation were in the range of 4.3-8.3 ng/L. Copyright © 2018 Elsevier B.V. All rights reserved.

  20. 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/Fe 3 O 4 @Poly(1,8-diaminonaphtalen) (MWCNTs/Fe 3 O 4 @PDAN) composite followed by HPLC-DAD was presented. Imprimis, the comparison among different magnetic nanosorbents including Fe 3 O 4 , MWCNTs/Fe 3 O 4 , Fe 3 O 4 @PDAN and MWCNTs/Fe 3 O 4 @PDAN was conducted. The obtained results, exhibited that the MWCNTs/Fe 3 O 4 @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.

  1. 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 electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Wang Jianhua; Hansen, Elo Harald; Miro, 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 are focused on the applications of SI-BI-LOV protocols for on-line microcolumn based solid phase extraction of ultra-trace levels of heavy metals, employing the so-called renewable surface separation and preconcentration manipulatory scheme. Two types of sorbents have been employed as packing material, 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 (C 18 -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 C 18 -PS/DVB beads entails analogous R.S.D.s and LODs with respect to the conventional approach, while those with PTFE beads result in slightly inferior R.S.D.s and LODs by similar comparison, yet offering a wider dynamic range than when using an external permanent column. Moreover, the hydrophilic materials result in much higher enrichment of the analyte than the hydrophobic ones, although PTFE is the packing material that exhibits the best retention efficiency

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

    NARCIS (Netherlands)

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

    1996-01-01

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

  3. Determination of inorganic arsenic in algae using bromine halogenation and on-line nonpolar solid phase extraction followed by hydride generation atomic flourescence spectrometry

    Science.gov (United States)

    Accurate, stable and fast analysis of toxic inorganic arsenic (iAs) in complicated and arsenosugar-rich algae matrix is always a challenge. Herein, a novel analytical method for iAs in algae was reported, using bromine halogenation and on-line nonpolar solid phase extraction (SPE) followed by hydrid...

  4. 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

  5. An LC-MS Assay with Isocratic Separation and On-Line Solid Phase Extraction to Improve the Routine Therapeutic Drug Monitoring of Busulfan in Plasma

    Directory of Open Access Journals (Sweden)

    Ialongo Cristiano

    2017-04-01

    Full Text Available Background: Busulfan (Bu requires therapeutic drug monitoring (TDM in subjects undergoing a conditioning regimen for hematopoietic stem cell transplantation (HSCT. To speed up the procedure and increase reproducibility, we improved our routine LC-MS/MS assay using the on-line solid-phase extraction (SPE of samples.

  6. A sublimate sorbent for stir-bar sorptive extraction of aqueous endocrine disruptor pesticides for gas chromatography-electron capture detection.

    Science.gov (United States)

    Huang, Yu-Wen; Lee, Hua Kwang; Shih, Hou-Kuang; Jen, Jen-Fon

    2018-06-06

    A dumbbell-shaped magnetic stir-bar with sublimate sorbent was prepared for the stir bar sorptive extraction (SBSE) of pesticides in an aqueous sample prior to gas chromatography-micro-electron capture detection (GC-μECD). Cyclododecane (CDD) was coated onto a magnetic stir-bar surface as a sublimate sorbent, and steel balls were placed on both ends to form a dumbbell-shaped magnetic stir-bar for SBSE. Four EDC pesticides including chlorpyrifos, ethion, bromopropylate, and λ-cyhalothrin in aqueous samples were selected as model species to examine the proposed SBSE and the following desorption. The parameters studied were those affecting the extraction efficiencies including the coating (solvent for CDD and thickness), extraction (sample pH, stirring rate, time, and salting out effect), dissolution solvent volume, and the loss of CDD sublimated in air. The maximum extraction efficiency was obtained under the following conditions. The stir bar (with CDD thickness of 5.2 μm) was added into a 10 mL sample solution (at pH 7) for a 20-min extraction at 600 rpm. Then, the stir bar was gently removed from the sample solution, disassembled, and immersed into a 0.2 mL insert tube consisting of 3 μL hexane to dissolve; 1 μL was used for GC-ECD analysis. The linear ranges were 0.005-5 μg L -1 with coefficients of determination ranging from 0.9950 - 0.9994. Detection limits (based on S/N = 3) of the four EDCs were 0.4-4.5 ngL -1 with a relative standard deviation (RSD) of 2.4-6.3%, and quantitation limits (based on S/N = 5) were 1-15 ngL -1 . The relative recoveries of the spiked samples were in the range of 83.2-98.7% with RSDs of 2.1-8.4% in farm field waters. The proposed sublimation sorbent obtained excellent enrichment factors (101-834) and provided a simple, rapid, sensitive, and eco-friendly sample preparation method. Copyright © 2018 Elsevier B.V. All rights reserved.

  7. Supercritical fluid extraction (SFE) of ketamine metabolites from dried urine and on-line quantification by supercritical fluid chromatography and single mass detection (on-line SFE-SFC-MS).

    Science.gov (United States)

    Hofstetter, Robert; Fassauer, Georg M; Link, Andreas

    2018-02-15

    On-line solid-phase supercritical fluid extraction (SFE) and chromatography (SFC) coupled to mass spectrometry (MS) has been evaluated for its usefulness with respect to metabolic profiling and pharmacological investigations of ketamine in humans. The aim of this study was to develop and validate a rapid, highly selective and sensitive SFE-SFC-MS method for the quantification of ketamine and its metabolites in miniature amounts in human urine excluding liquid-liquid extraction (LLE). Several conditions were optimized systematically following the requirements of the European Medicines Agency: selectivity, carry-over, calibration curve parameters (LLOQ, range and linearity), within- and between-run accuracy and precision, dilution integrity, matrix effect, and stability. The method, which required a relatively small volume of human urine (20 μL per sample), was validated for pharmacologically and toxicologically relevant concentrations ranging from 25.0 to 1000 ng/mL (r 2  > 0.995). The lower limit of quantification (LLOQ) for all compounds was found to be as low as 0.5 ng. In addition, stability of analytes during removal of water from the urine samples using different conditions (filter paper or ISOLUTE® HM-N) was studied. In conclusion, the method developed in this study can be successfully applied to studies of ketamine metabolites in humans, and may pave the way for routine application of on-line SFE-SFC-MS in clinical investigations. Copyright © 2018 Elsevier B.V. All rights reserved.

  8. Speciation analysis of inorganic arsenic by magnetic solid phase extraction on-line with inductively coupled mass spectrometry determination.

    Science.gov (United States)

    Montoro Leal, P; Vereda Alonso, E; López Guerrero, M M; Cordero, M T Siles; Cano Pavón, J M; García de Torres, A

    2018-07-01

    Arsenic, one of the main environmental pollutants and potent natural poison, is a chemical element that is spread throughout the Earth's crust. It is well known that the toxicity of arsenic is highly dependent on its chemical forms. Generally, the inorganic species are more toxic than its organics forms, and As(III) is 60 times more toxic than As(V). In environmental waters, arsenic exists predominantly in two chemical forms: As(III) and As(V). In view of these facts, fast, sensitive, accurate and simple analytical methods for the speciation of inorganic arsenic in environmental waters are required. In this work, a new magnetic solid phase extraction with a hydride generation system was coupled on line with inductively coupled plasma mass spectrometry (MSPE-HG-ICP-MS). The new system was based on the retention of As(III) and As(V) in two knotted reactors filled with (Fe 3 O 4 ) magnetic nanoparticles functionalized with [1,5-bis (2-pyridyl) 3-sulfophenylmethylene] thiocarbonohydrazide (PSTH-MNPs). As(III) and total inorganic As were sequentially eluted in different reduction conditions. The concentration of As(V) was obtained by subtracting As(III) from total As. The system runs in a fully automated way and the method has proved to have a wide linear range and to be precise, sensitive and fast. The detection limits found were 2.7 and 3.2 ng/L for As(III) and total As, respectively; with relative standard deviations (RSDs) of 2.5% and 2.7% and a sample throughput of 14.4 h -1 . In order to validate the developed method, several certified reference samples of environmental waters including sea water, were analyzed and the determined values were in good agreement with the certified values. The proposed method was successfully applied to the speciation analysis of inorganic arsenic in well-water and sea water. Copyright © 2018 Elsevier B.V. All rights reserved.

  9. 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.

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

    Science.gov (United States)

    Mazzoni, Michela; Rusconi, Marianna; Valsecchi, Sara; Martins, Claudia P. B.; Polesello, Stefano

    2015-01-01

    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. PMID:25834752

  11. Determination of haloacetic acids in water using layered double hydroxides as a sorbent in dispersive solid-phase extraction followed by liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Alsharaa, Abdulnaser; Sajid, Muhammad; Basheer, Chanbasha; Alhooshani, Khalid; Lee, Hian Kee

    2016-09-01

    In the present study, highly efficient and simple dispersive solid-phase extraction procedure for the determination of haloacetic acids in water samples has been established. Three different types of layered double hydroxides were synthesized and used as a sorbent in dispersive solid-phase extraction. Due to the interesting behavior of layered double hydroxides in an acidic medium (pH˂4), the analyte elution step was not needed; the layered double hydroxides are simply dissolved in acid immediately after extraction to release the analytes which are then directly introduced into a liquid chromatography with tandem mass spectrometry system for analysis. Several dispersive solid-phase extraction parameters were optimized to increase the extraction efficiency of haloacetic acids such as temperature, extraction time and pH. Under optimum conditions, good linearity was achieved over the concentration range of 0.05-100 μg/L with detection limits in the range of 0.006-0.05 μg/L. The relative standard deviations were 0.33-3.64% (n = 6). The proposed method was applied to different water samples collected from a drinking water plant to determine the concentrations of haloacetic acids. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

  13. Novel ion-imprinted polymer coated on nanoporous silica as a highly selective sorbent for the extraction of ultratrace quantities of gold ions from mine stone samples

    International Nuclear Information System (INIS)

    Ebrahimzadeh, H.; Moazzen, E.; Amini, M.; Sadeghi, O.

    2013-01-01

    We have developed a gold ion-imprinted polymer (GIP) by incorporating a dipyridyl ligand into an ethylene glycol dimethacrylate matrix which then was coated onto porous silica particles. The material was used for the selective extraction of ultratrace quantities of gold ion from mine stones, this followed by its quantitation by FAAS. The effects of concentration and volume of eluent, pH of the solution, flow rates of sample and eluent, and effect of potentially interfering ions, especially palladium and platinum, was investigated. The limit of detection is -1 , the precision (RSD%) is 1.03 %, and recoveries are >99 %. In order to show the high selectivity and efficiency of the new sorbent, the results were compared to those obtained with more simple sorbents possessing the same functional groups. The accuracy of the method was demonstrated by the accurate determination of gold ions in a certified reference material. To the best of our knowledge, there is no report so far on an imprint for gold ions that has such a selectivity over Pd(II) and Pt(II) ions. (author)

  14. Graphene-Derivatized Silica Composite as Solid-Phase Extraction Sorbent Combined with GC–MS/MS for the Determination of Polycyclic Musks in Aqueous Samples

    Directory of Open Access Journals (Sweden)

    Cheng Li

    2018-02-01

    Full Text Available Polycyclic musks (PCMs have recently received growing attention as emerging contaminants because of their bioaccumulation and potential ecotoxicological effects. Herein, an effective method for the determination of five PCMs in aqueous samples is presented. Reduced graphene oxide-derivatized silica (rGO@silica particles were prepared from graphene oxide and aminosilica microparticles and characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy. PCMs were preconcentrated using rGO@silica as the solid-phase extraction sorbent and quantified by gas chromatography–tandem mass spectrometry. Several experimental parameters, such as eluent, elution volume, sorbent amount, pH, and sample volume were optimized. The correlation coefficient (R ranged from 0.9958 to 0.9992, while the limits of detection and quantitation for the five PCMs were 0.3–0.8 ng/L and 1.1–2.1 ng/L, respectively. Satisfactory recoveries were obtained for tap water (86.6–105.9% and river water samples (82.9–107.1%, with relative standard deviations <10% under optimal conditions. The developed method was applied to analyze PCMs in tap and river water samples from Beijing, China. Galaxolide (HHCB and tonalide (AHTN were the main PCM components detected in one river water sample at concentrations of 18.7 for HHCB, and 11.7 ng/L for AHTN.

  15. Application of Box-Behnken design to optimize multi-sorbent solid phase extraction for trace neonicotinoids in water containing high level of matrix substances.

    Science.gov (United States)

    Zhang, Junjie; Wei, Yanli; Li, Huizhen; Zeng, Eddy Y; You, Jing

    2017-08-01

    Extensive use of neonicotinoid insecticides has raised great concerns about their ecological risk. A reliable method to measure trace neonicotinoids in complicated aquatic environment is a premise for assessing their aquatic risk. To effectively remove matrix interfering substances from field water samples before instrumental analysis with HPLC/MS/MS, a multi-sorbent solid phase extraction method was developed using Box-Behnken design. The optimized method employed 200mg HLB/GCB (w/w, 8/2) as the sorbents and 6mL of 20% acetone in acetonitrile as the elution solution. The method was applied for measuring neonicotinoids in water at a wide range of concentrations (0.03-100μg/L) containing various amounts of matrix components. The recoveries of acetamiprid, imidacloprid, thiacloprid and thiamethoxam from the spiked samples ranged from 76.3% to 107% while clothianidin and dinotefuran had relatively lower recoveries. The recoveries of neonicotinoids in water with various amounts of matrix interfering substances were comparable and the matrix removal rates were approximately 50%. The method was sensitive with method detection limits in the range of 1.8-6.8ng/L for all target neonicotinoids. Finally, the developed method was validated by measurement of trace neonicotinoids in natural water. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2018-06-05

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

  17. Rapid identification and quantification of methamphetamine and amphetamine in hair by gas chromatography/mass spectrometry coupled with micropulverized extraction, aqueous acetylation and microextraction by packed sorbent.

    Science.gov (United States)

    Miyaguchi, Hajime; Iwata, Yuko T; Kanamori, Tatsuyuki; Tsujikawa, Kenji; Kuwayama, Kenji; Inoue, Hiroyuki

    2009-05-01

    We developed a rapid identification and quantification method for the toxicological analysis of methamphetamine and amphetamine in human hair by gas chromatography/mass spectrometry coupled with a novel combination of micropulverized extraction, aqueous acetylation and microextraction by packed sorbent (MEPS) named MiAMi-GC/MS. A washed hair sample (1-5 mg) was micropulverized for 5 min in a 2 mL plastic tube with 250 microL of water. An anion-exchange sorbent was added to adsorb anionic interferences. After removing the residue with a membrane-filter unit, sodium carbonate and acetic anhydride was admixed in turn. Acetylation was completed in approximately 20 min at room temperature. The acetylated analytes in the reaction liquid were concentrated to an octadecylsilica sorbent packed in the needle of a syringe by a CombiPAL autosampler. Elution was carried out with 50 microL of methanol, and the entire eluate injected into a gas chromatograph using a programmable temperature vaporizing (PTV) technique. The time required for sample preparation and GC/MS analysis was approximately 1 h from a washed hair sample, and an evaporation process was not required. Ranges for quantification were 0.20-50 (ng/mg) each for methamphetamine and amphetamine using 1 mg of hair. Accuracy and relative standard deviation (RSD) were evaluated intraday and interday at three concentrations, and the results were within the limit of a guidance issued by U.S. Food and Drug Administration. For identification, full-scan mass spectra of methamphetamine and amphetamine were obtained using 5 mg of fortified hair samples at 0.2 ng/mg. The extraction device of MEPS was durable for at least 300 extractions, whereas the liner of the gas chromatograph should be replaced after 20-30 times use. The carry over was estimated to be about 1-2%. This sample-preparation method coupled with GC/MS is fast and labor-saving in comparison with conventional methods.

  18. Development of an on-line mixed-mode gel liquid chromatography×reversed phase liquid chromatography method for separation of water extract from Flos Carthami.

    Science.gov (United States)

    Wang, Yu-Qing; Tang, Xu; Li, Jia-Fu; Wu, Yun-Long; Sun, Yu-Ying; Fang, Mei-Juan; Wu, Zhen; Wang, Xiu-Min; Qiu, Ying-Kun

    2017-10-13

    A novel on-line comprehensive two-dimensional liquid chromatography (2D-LC) method by coupling mixed-mode gel liquid chromatography (MMG-LC) with reversed phase liquid chromatography (RPLC) was developed. A mixture of 17 reference compounds was used to study the separation mechanism. A crude water extract of Flos Carthami was applied to evaluate the performance of the novel 2D-LC system. In the first dimension, the extract was eluted with a gradient of water/methanol over a cross-linked dextran gel Sephadex LH-20 column. Meanwhile, the advantages of size exclusion, reversed phase partition and adsorption separation mechanism were exploited before further on-line reversed phase purification on the second dimension. This novel on-line mixed-mode Sephadex LH-20×RPLC method provided higher peak resolution, sample processing ability (2.5mg) and better orthogonality (72.9%) versus RPLC×RPLC and hydrophilic interaction liquid chromatography (HILIC)×RPLC. To the best of our knowledge, this is the first report of a mixed-mode Sephadex LH-20×RPLC separation method with successful applications in on-line mode, which might be beneficial for harvesting targets from complicated medicinal plants. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Dispersive solid-phase extraction for the determination of trace organochlorine pesticides in apple juices using reduced graphene oxide coated with ZnO nanocomposites as sorbent.

    Science.gov (United States)

    Sun, Ting; Sun, Hefeng; Zhao, Feng

    2017-09-01

    In this work, reduced graphene oxide coated with ZnO nanocomposites was used as an efficient sorbent of dispersive solid-phase extraction and successfully applied for the extraction of organochlorine pesticides from apple juice followed by gas chromatography with mass spectrometry. Several experimental parameters affecting the extraction efficiencies, including the amount of adsorbent, extraction time, and the pH of the sample solution, as well as the type and volume of eluent solvent, were investigated and optimized. Under the optimal experimental conditions, good linearity existed in the range of 1.0-200.0 ng/mL for all the analytes with the correlation coefficients (R 2 ) ranging from 0.9964 to 0.9994. The limits of detection of the method for the compounds were 0.011-0.053 ng/mL. Good reproducibilities were acquired with relative standard deviations below 8.7% for both intraday and interday precision. The recoveries of the method were in the range of 78.1-105.8% with relative standard deviations of 3.3-6.9%. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. 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...

  1. 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.

  2. 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.

  3. Rapid Determination of Two Triterpenoid Acids in Chaenomelis Fructus Using Supercritical Fluid Extraction On-line Coupled with Supercritical Fluid Chromatography.

    Science.gov (United States)

    Zhang, Xiaotian; Ji, Feng; Li, Yueqi; He, Tian; Han, Ya; Wang, Daidong; Lin, Zongtao; Chen, Shizhong

    2018-01-01

    In this study, an on-line supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC) method was developed for the rapid determination of oleanoic acid and ursolic acid in Chaenomelis Fructus. After optimization of the conditions, the two triterpenoid acids was obtained by SFE using 20% methanol as a modifier at 35°C in 8 min. They were resolved on a Shim-pack UC-X Diol column (4.6 × 150 mm, 3 μm) in 14 min (0 - 10 min, 5 - 10%; 10 - 14 min, 10% methanol in CO 2 ) with a backpressure of 15 MPa at 40°C. The on-line SFE-SFC method could be completed within 40 min (10.79 mg/g dry plant, R s = 2.36), while the ultrasound-assisted extraction and HPLC method required at least 90 min (3.55 mg/g dry plant, R s = 1.92). This on-line SFE-SFC method is powerful to simplify the pre-processing and quantitative analysis of natural products.

  4. Solid-phase extraction of chlorophenols in seawater using a magnetic ionic liquid molecularly imprinted polymer with incorporated silicon dioxide as a sorbent.

    Science.gov (United States)

    Ma, Wanwan; Row, Kyung Ho

    2018-07-20

    A type of magnetic ionic liquid based molecularly imprinted polymer coated on SiO 2 (Fe 3 O 4 @SiO 2 @IL-MIPs) was prepared with 1-vinyl-3-ethylimidazole ionic liquid as functional monomer, and 1,4-butane-3,3'-bis-1-ethylimidazole ionic liquid as cross linker, 4-Chlorophenol as template was successfully applied as a selective adsorbent for selective extraction of 5 chlorophenols in seawater samples by using the magnetic solid-phase extraction (MSPE) method. 11 types of Fe 3 O 4 @SiO 2 @IL-MIPs were synthesized and investigated for their different compositions of functional monomer (such as [C 2 min][Br], [C 2 min][BF 4 ], [C 2 min][PF 6 ], acrylamide, methacrylic acid and 4-vinyl pyridine) and cross-linker (such as [C 4 min 2 ][Br], [C 4 min 2 ][BF 4 ], [C 4 min 2 ][PF 6 ], divinylbenzene, and ethylene glycol dimethacrylate), respectively. The [C 2 min][BF 4 ] and [C 4 min 2 ][PF 6 ] based Fe 3 O 4 @SiO 2 @IL-MIP with the highest extraction efficiencies was applied to the optimization experiment of MSPE process (including extraction time, adsorbent mass and desorption solvents). Good linearity was obtained with correlation coefficients (R 2 ) over 0.9990 and the relative standard deviations for the intra-day and inter-day determination were less than 3.10% with the extraction recoveries ranged from 85.0% to 98.4%. The results indicated that the proposed Fe 3 O 4 @SiO 2 @IL-MIPs possesses great identification and adsorption properties, and could be used as a good sorbent for selective extraction of CPs in environment waters. Copyright © 2018 Elsevier B.V. All rights reserved.

  5. 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.

  6. Low-cost humic acid-bonded silica as an effective solid-phase extraction sorbent for convenient determination of aflatoxins in edible oils

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Neng-Zhi [Guangxi Zhuang Autonomous Region Center for Disease Prevention and Control, Nanning, Guangxi 530028 (China); Liu, Ping [School of Pharmaceutical Science, Guangxi Medical University, Nanning, Guangxi 530021 (China); Su, Xiao-Chuan; Liao, Yan-Hua; Lei, Ning-Sheng [Guangxi Zhuang Autonomous Region Center for Disease Prevention and Control, Nanning, Guangxi 530028 (China); Liang, Yong-Hong [School of Pharmaceutical Science, Guangxi Medical University, Nanning, Guangxi 530021 (China); Zhou, Shao-Huan; Lin, Wen-Si; Chen, Jie [Guangxi Zhuang Autonomous Region Center for Disease Prevention and Control, Nanning, Guangxi 530028 (China); Feng, Yu-Qi [Key Laboratory of Analytical Chemistry for Biology and Medicine, Ministry of Education, Department of Chemistry, Wuhan University, Wuhan 430072 (China); Tang, Yang, E-mail: tycarson2@163.com [Guangxi Zhuang Autonomous Region Center for Disease Prevention and Control, Nanning, Guangxi 530028 (China)

    2017-06-01

    Aflatoxins (AFs) are highly toxic, mutagenic, carcinogenic, and teratogenic secondary metabolites produced by the toxigenic fungi Aspergillus flavus and Aspergillus parasiticus. AFs tend to contaminate a wide range of foods which is a serious and recurring food safety problem worldwide. Currently, immunoaffinity chromatography (IAC) has become the most conventional sample clean-up method for determining AFs in foodstuffs. However, IAC method is limited in the large-scale food analysis because it requires the use of expensive disposable cartridges and the IA procedure is time-consuming. Herein, to achieve the cost-effective determination of AFs in edible oils, we developed a promising solid-phase extraction (SPE) method based on commercially available humic acid-bonded silica (HAS) sorbent, followed by high performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS) analysis. In HAS-SPE, AFs can be captured by the HAS sorbent with both hydrophobic and hydrophilic interactions, whereas the oil matrix was captured only with the hydrophobic interactions. The oil matrix can be sufficiently washed off with isopropanol, while the AFs were still retained on the SPE packing, thus achieving selective extraction of AFs and clean-up of oil matrices. Under the optimal conditions of HAS-SPE, satisfactory recoveries ranging from 82% to 106% for four AFs (B{sub 1}, B{sub 2}, G{sub 1}, and G{sub 2}) were achieved in various oil matrices, containing blended oil, tea oil, rapeseed oil, peanut oil, sunflower seed oil, corn oil, blended olive oil, rice oil, soybean oil, and sesame oil. Only minor matrix effects ranging from 99% to 105% for four AFs were observed. Moreover, the LODs of AFs between 0.012 and 0.035 μg/kg completely meet the regulatory levels fixed by the EU, China or other countries. The methodology was further validated for assaying the naturally contaminated peanut oils, and consistent results between the HAS-SPE and the referenced IAC were

  7. High-Efficiency On-Line Solid-Phase Extraction Coupling to 15-150 um I.D. Column Liquid Chromatography for Proteomic Analysis

    International Nuclear Information System (INIS)

    Shen, Yufeng; Moore, Ronald J.; Zhao, Rui; Blonder, Josip; Auberry, Deanna L.; Masselon, Christophe D.; Pasa Tolic, Ljiljana; Hixson, Kim K.; Auberry, Kenneth J.; Smith, Richard D.

    2003-01-01

    Flexible manipulation of various properties of proteomic samples is important for proteomic analyses, but it has been little explored for newly developed approaches based on liquid chromatography (LC) in combination with mass spectrometry (MS). With miniaturization of the LC column inner diameter dimensions (required for improving the analysis sensitivity), this issue becomes more challenging due to the small flow rates and the increasing effects of extra column volume on the separation quality and its use for resolving complex proteomic mixtures. In this study, we used commercial switching valves (150-mm channels) to implement the on-line coupling of capillary LC columns with relatively large solid phase extraction (SPE) columns operated at 10,000 psi. With optimized column connections, switching modes, and SPE column dimensions, high-efficiency on-line SPE-capillary and nanoscale LC separations were obtained with peak capacities of ∼1000 for capillaries having inner diameters between 15 to 150 mm. The on-line coupled SPE columns increased the sample processing capabilities by ∼400-fold for sample solution volume and ∼10-fold for sample mass. The proteomic applications of this on-line SPE-capillary LC system were evaluated for analysis of both soluble and membrane protein tryptic digests. Used with an ion trap tandem MS we could typically identify 1100-1500 peptides for analyses in a single 5-hour run. Peptides extracted on the SPE column and eluted from the LC column covered a hydrophilicity/hydrophobicity range that include an estimated ∼98% of all the tryptic peptides. The present implementation also facilitates automation and enables use of both disposable SPE columns and electrospray emitters, providing a robust basis for routine proteomic analyses.

  8. On-Line Junction Temperature Monitoring of Switching Devices with Dynamic Compact Thermal Models Extracted with Model Order Reduction

    Directory of Open Access Journals (Sweden)

    Fabio Di Napoli

    2017-02-01

    Full Text Available Residual lifetime estimation has gained a key point among the techniques that improve the reliability and the efficiency of power converters. The main cause of failures are the junction temperature cycles exhibited by switching devices during their normal operation; therefore, reliable power converter lifetime estimation requires the knowledge of the junction temperature time profile. Since on-line dynamic temperature measurements are extremely difficult, in this work an innovative real-time monitoring strategy is proposed, which is capable of estimating the junction temperature profile from the measurement of the dissipated powers through an accurate and compact thermal model of the whole power module. The equations of this model can be easily implemented inside a FPGA, exploiting the control architecture already present in modern power converters. Experimental results on an IGBT power module demonstrate the reliability of the proposed method.

  9. On-line separation of Pu(III) and Am(III) using extraction and ion chromatography

    International Nuclear Information System (INIS)

    Jernstroem, J.; Lehto, J.; Betti, M.

    2007-01-01

    An on-line method developed for separating plutonium and americium was developed. The method is based on the use of HPLC pump with three analytical chromatographic columns. Plutonium is reduced throughout the procedure to trivalent oxidation state, and is recovered in the various separation steps together with americium. Light lanthanides and trivalent actinides are separated with TEVA resin in thiocyanate/formic acid media. Trivalent plutonium and americium are pre-concentrated in a TCC-II cation-exchange column, after which the separation is performed in CS5A ion chromatography column by using two different eluents. Pu(III) is eluted with a dipicolinic acid eluent, and Am(III) with oxalic acid eluent. Radiochemical and chemical purity of the eluted plutonium and americium fractions were ensured with alpha-spectrometry. (author)

  10. Low-cost humic acid-bonded silica as an effective solid-phase extraction sorbent for convenient determination of aflatoxins in edible oils.

    Science.gov (United States)

    Zhou, Neng-Zhi; Liu, Ping; Su, Xiao-Chuan; Liao, Yan-Hua; Lei, Ning-Sheng; Liang, Yong-Hong; Zhou, Shao-Huan; Lin, Wen-Si; Chen, Jie; Feng, Yu-Qi; Tang, Yang

    2017-06-01

    Aflatoxins (AFs) are highly toxic, mutagenic, carcinogenic, and teratogenic secondary metabolites produced by the toxigenic fungi Aspergillus flavus and Aspergillus parasiticus. AFs tend to contaminate a wide range of foods which is a serious and recurring food safety problem worldwide. Currently, immunoaffinity chromatography (IAC) has become the most conventional sample clean-up method for determining AFs in foodstuffs. However, IAC method is limited in the large-scale food analysis because it requires the use of expensive disposable cartridges and the IA procedure is time-consuming. Herein, to achieve the cost-effective determination of AFs in edible oils, we developed a promising solid-phase extraction (SPE) method based on commercially available humic acid-bonded silica (HAS) sorbent, followed by high performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS) analysis. In HAS-SPE, AFs can be captured by the HAS sorbent with both hydrophobic and hydrophilic interactions, whereas the oil matrix was captured only with the hydrophobic interactions. The oil matrix can be sufficiently washed off with isopropanol, while the AFs were still retained on the SPE packing, thus achieving selective extraction of AFs and clean-up of oil matrices. Under the optimal conditions of HAS-SPE, satisfactory recoveries ranging from 82% to 106% for four AFs (B 1 , B 2 , G 1 , and G 2 ) were achieved in various oil matrices, containing blended oil, tea oil, rapeseed oil, peanut oil, sunflower seed oil, corn oil, blended olive oil, rice oil, soybean oil, and sesame oil. Only minor matrix effects ranging from 99% to 105% for four AFs were observed. Moreover, the LODs of AFs between 0.012 and 0.035 μg/kg completely meet the regulatory levels fixed by the EU, China or other countries. The methodology was further validated for assaying the naturally contaminated peanut oils, and consistent results between the HAS-SPE and the referenced IAC were obtained. In

  11. 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

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

    International Nuclear Information System (INIS)

    Hsieh, Kai-Ta; Liu, Pei-Han; Urban, Pawel L.

    2015-01-01

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

  13. Facile synthesis of new nano sorbent for magnetic solid-phase extraction by self assembling of bis-(2,4,4-trimethyl pentyl)-dithiophosphinic acid on Fe3O4-Ag core-shell nanoparticles: Characterization and application

    International Nuclear Information System (INIS)

    Tahmasebi, Elham; Yamini, Yadollah

    2012-01-01

    Graphical abstract: Self assembling of bis-(2,4,4-trimethylpentyl)-dithiophosphinic acid on Fe 3 O 4 -Ag core-shell nanoparticles and application of it for solid phase extraction of PAHs. Highlights: ► A novel sorbent for magnetic solid-phase extraction of PAHs was introduced. ► Silver was coated on Fe 3 O 4 nanoparticles (MNPs) by reduction of AgNO 3 with NaBH 4 . ► Bis-(2,4,4-trimethylpentyl)-dithiophosphinic acid self-assembled on silver coated MNPs. ► Size, morphology, composition and properties of the nanoparticles were characterized. ► Extraction efficiency of the sorbent was investigated by extraction of five PAHs. - Abstract: A novel sorbent for magnetic solid-phase extraction by self-assembling of organosulfur compound, (bis-(2,4,4-trimethylpentyl)-dithiophosphinic acid), onto the silver-coated Fe 3 O 4 nanoparticles was introduced. Due to the formation of covalent bond of S-Ag, the new coating on the silver surface was very stable and showed high thermal stability (up to 320 °C). The size, morphology, composition, and properties of the prepared nanoparticles have also been characterized and determined using scanning electron microscopy (SEM), energy-dispersive X-ray analyzer (EDX), dynamic light scattering (DLS), Fourier transform-infrared (FT-IR) spectroscopy, and thermal gravimetric analysis (TGA). Extraction efficiency of the new sorbent was investigated by extraction of five polycyclic aromatic hydrocarbons (PAHs) as model compounds. The optimum extraction conditions for PAHs were obtained as of extraction time, 20 min; 50 mg sorbent from 100 mL of the sample solution, and elution with 100 μL of 1-propanol under fierce vortex for 2 min. Under the optimal conditions, the calibration curves were obtained in the range of 0.05–100 μg L −1 (R 2 > 0.9980) and the LODs (S/N = 3) were obtained in the range of 0.02–0.10 μg L −1 . Relative standard deviations (RSDs) for intra- and inter-day precision were 2.6–4.2% and 3.6–8

  14. Quantitative analysis of higher hydrocarbons in natural gas using coupled solid-phase extraction / supercritiacal fluid extraction with on-line GC analysis

    NARCIS (Netherlands)

    Janssen, J.G.M.; Cramers, C.A.M.G.; Meulen-Kuijk, van der L.; Smit, A.L.C.; Sandra, P.; Devos, G.

    1993-01-01

    Characterisation of natural gas with respect to the hydrocarbon content is a challenging analytical problem due to the extremely low concentrations and the complexity of the matrix. In this publication a method is described for fully on-line preconcentration and analysis of n-nonane and higher

  15. Automation of radiochemical analysis by flow injection techniques. Am-Pu separation using TRU-resinTM sorbent extraction column

    International Nuclear Information System (INIS)

    Egorov, O.; Washington Univ., Seattle, WA; Grate, J.W.; Ruzicka, J.

    1998-01-01

    A rapid automated flow injection analysis (FIA) procedure was developed for efficient separation of Am and Pu from each other and from interfering matrix and radionuclide components using a TRU-resin TM column. Selective Pu elution is enabled via on-column reduction. The separation was developed using on-line radioactivity detection. After the separation had been developed, fraction collection was used to obtain the separated fractions. In this manner, a FIA instrument functions as an automated separation workstation capable of unattended operation. (author)

  16. Homogenate-assisted Vacuum-powered Bubble Extraction of Moso Bamboo Flavonoids for On-line Scavenging Free Radical Capacity Analysis.

    Science.gov (United States)

    Sun, Yinnan; Yang, Kui; Cao, Qin; Sun, Jinde; Xia, Yu; Wang, Yinhang; Li, Wei; Ma, Chunhui; Liu, Shouxin

    2017-07-11

    A homogenate-assisted vacuum-powered bubble extraction (HVBE) method using ethanol was applied for extraction of flavonoids from Phyllostachys pubescens (P. pubescens) leaves. The mechanisms of homogenate-assisted extraction and vacuum-powered bubble generation were discussed in detail. Furthermore, a method for the rapid determination of flavonoids by HPLC was established. HVBE followed by HPLC was successfully applied for the extraction and quantification of four flavonoids in P. pubescens , including orientin, isoorientin, vitexin, and isovitexin. This method provides a fast and effective means for the preparation and determination of plant active components. Moreover, the on-line antioxidant capacity, including scavenging positive ion and negative ion free radical capacity of different fractions from the bamboo flavonoid extract was evaluated. Results showed that the scavenging DPPH ˙ free radical capacity of vitexin and isovitexin was larger than that of isoorientin and orientin. On the contrary, the scavenging ABTS⁺ ˙ free radical capacity of isoorientin and orientin was larger than that of vitexin and isovitexin.

  17. 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

    International Nuclear Information System (INIS)

    Anthemidis, Aristidis N.; Mitani, Constantina; Balkatzopoulou, Paschalia; Tzanavaras, Paraskevas D.

    2012-01-01

    Highlights: ► A dispersive liquid–liquid micro extraction method for lead and copper determination. ► A micro-volume transportation system for extractant solvent lighter than water. ► 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 μg L −1 and 3.3% for lead and 0.12 μg L −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.

  18. Liquid chromatography mass spectrometry determination of perfluoroalkyl acids in environmental solid extracts after phospholipid removal and on-line turbulent flow chromatography purification.

    Science.gov (United States)

    Mazzoni, M; Polesello, S; Rusconi, M; Valsecchi, S

    2016-07-01

    An on-line TFC (Turbulent Flow Chromatography) clean up procedures coupled with UHPLC-MS/MS (Ultra High Performance Liquid Chromatography Mass Spectrometry) multi-residue method was developed for the simultaneous determination of 8 perfluroalkyl carboxylic acids (PFCA, from 5 to 12 carbon atoms) and 3 perfluoroalkyl sulfonic acids (PFSA, from 4 to 8 carbon atoms) in environmental solid matrices. Fast sample preparation procedure was based on a sonication-assisted extraction with acetonitrile. Phospholipids in biological samples were fully removed by an off-line SPE purification before injection, using HybridSPE(®) Phospholipid Ultra cartridges. The development of the on-line TFC clean-up procedure regarded the choice of the stationary phase, the optimization of the mobile phase composition, flow rate and injected volume. The validation of the optimized method included the evaluation of matrix effects, accuracy and reproducibility. Signal suppression in the analysis of fortified extracts ranged from 1 to 60%, and this problem was overcome by using isotopic dilution. Since no certified reference materials were available for PFAS in these matrices, accuracy was evaluated by recoveries on spiked clam samples which were 98-133% for PFCAs and 40-60% for PFSAs. MLDs and MLQs ranged from 0.03 to 0.3ngg(-1) wet weight and from 0.1 to 0.9ngg(-1) wet weight respectively. Repeatability (intra-day precision) and reproducibility (inter-day precision) showed RSD from 3 to 13% and from 4 to 27% respectively. Validated on-line TFC/UHPLC-MS/MS method has been applied for the determination of perfluoroalkyl acids in different solid matrices (sediment, fish, bivalves and bird yolk). Copyright © 2016 Elsevier B.V. All rights reserved.

  19. 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.

  20. An automated flow injection system for metal determination by flame atomic absorption spectrometry involving on-line fabric disk sorptive extraction technique.

    Science.gov (United States)

    Anthemidis, A; Kazantzi, V; Samanidou, V; Kabir, A; Furton, K G

    2016-08-15

    A novel flow injection-fabric disk sorptive extraction (FI-FDSE) system was developed for automated determination of trace metals. The platform was based on a minicolumn packed with sol-gel coated fabric media in the form of disks, incorporated into an on-line solid-phase extraction system, coupled with flame atomic absorption spectrometry (FAAS). This configuration provides minor backpressure, resulting in high loading flow rates and shorter analytical cycles. The potentials of this technique were demonstrated for trace lead and cadmium determination in environmental water samples. The applicability of different sol-gel coated FPSE media was investigated. The on-line formed complex of metal with ammonium pyrrolidine dithiocarbamate (APDC) was retained onto the fabric surface and methyl isobutyl ketone (MIBK) was used to elute the analytes prior to atomization. For 90s preconcentration time, enrichment factors of 140 and 38 and detection limits (3σ) of 1.8 and 0.4μgL(-1) were achieved for lead and cadmium determination, respectively, with a sampling frequency of 30h(-1). The accuracy of the proposed method was estimated by analyzing standard reference materials and spiked water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. On-line anti-acetylcholine esterase activity of extracts of oxystelma esculentum, aerva javanica and zanthoxylum armatum

    International Nuclear Information System (INIS)

    Murtaza, S.; Ullah, R. S.; Abbas, A.; Riaz, T.; Ghous, T.; Altaf, Y.; Khan, M.; Ahmed, S.

    2013-01-01

    Alzheimer's disease (AD), a disease of brain, resulting in memory impairment and the loss of thinking. The main reason of Alzheimer's disease is firmly associated with some impairment in cholinergic transmission. This impairment may be improved by diminishing the breakdown of acetylcholine at the synaptic site in the brain by inhibiting acetylcholinesterase (AChE). In this work, extracts of three different plants Oxystelma esculentum (OEM), Aerva javanica (AJM) and Zanthoxylum armatum (ZAA) have been screened for their anti-AchE activity. Results of the study demonstrate that of the studied extracts, ZAA (IC/sub 50/ 55.5 micro g/ml) acquired stronger anti-AChE activity. While OEM with IC/sub 50/ 107.2 micro g/ml showed moderate and ZAE and AJM showed weaker action (IC/sub 50/ 182.5 and 275.2 micro g/ml). Galanthamine was used as a positive control (IC/sub 50/ 1.47 micro g/ml). (author)

  2. 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.

  3. 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. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. On-line extraction of the variance caused by burn-up in in-core three-dimensional power distribution

    International Nuclear Information System (INIS)

    Wang Yaqi; Luo Zhengpei; Li Fu; Liu Wenfeng

    2001-01-01

    In most of PWRs, the ex-core ion-chambers are the sole real-time sensors to respond to in-core power and its axial offset. However, the calibration coefficient of the ion-chambers depends on the (3D) power distribution and varies with the burn-up. People expect to know the variance in distribution caused by burn-up directly from the signals of ion-chambers. This expectation is not realized as yet, because an ion-chamber almost only responds to its nearest fuel assemblies. The authors then developed a two-step method for burn-up characteristic extraction: the harmonics synthesis method and harmonics' burn-up grouping. Using the extracted burn-up characteristics, the relationship between the readings of the ex-core ion-chambers and the in-core 3D power distribution is set up. Through the simulation on the heating reactor, the method of burn-up characteristic extraction is verified under engineering conditions. It is possible to on-line extract the variance caused by burn-up in 3D power distribution

  5. Ternary mixed-mode silica sorbent of solid-phase extraction for determination of basic, neutral and acidic drugs in human serum.

    Science.gov (United States)

    Jin, Shupei; Qiao, Yinghua; Xing, Jun

    2018-06-01

    In this study, a ternary mixed-mode silica sorbent (TMSS) with octamethylene, carboxyl, and amino groups was prepared via Cu(I)-catalyzed azide-alkyne cycloaddition (CuAAC) click reaction and a subsequent reduction of azide to primary amine. While used in solid-phase extraction (SPE), the retention behavior of TMSS towards a total of nine kinds of basic, neutral, and acidic drugs was investigated in detail. The results revealed that hydrophobic, ion-exchange interaction, and electrostatic repulsion between TMSS and the analytes were closely related to the retention behavior of TMSS. Besides, the log K ow value of the analyte was also a factor influencing the retention behavior of analytes on TMSS. The nine analytes could be retained by TMSS simultaneously and then, were eluted into two fractions according to the acid-base property of the analytes for further determinations. The acidic and neutral analytes were in one fraction, and the basic ones in the other fraction. When used to treat the human serum spiked with the nine drugs, TMSS offered higher recoveries than BakerBond CBA and comparable recoveries to Oasis WCX. It should be noted TMSS had better purifying capability for human serum than Oasis WCX. Under the optimized SPE conditions, a method of SPE hyphenated to high-performance liquid chromatography-ultraviolet detection (HPLC-UV) for determination of the basic, neutral, and acidic drugs spiked in human serum was established. For the nine drugs, the linear ranges were all between 5.0 and 1000 μg L -1 with correlation coefficients (R 2 ) above 0.9990, and the limits of detection (LODs) were in the range of 0.8-2.3 μg L -1 . The intra-day and inter-day relative standard deviations (RSDs) were less than 5.3 and 8.8%, respectively. Graphical abstract Treating drugs in human serum by SPE with ternary mixed-mode silica sorbent.

  6. Carbon nanofibers extracted from soot as a sorbent for the determination of aromatic amines from wastewater effluent samples.

    Science.gov (United States)

    Vadukumpully, Sajini; Basheer, Chanbasha; Jeng, Cheng Suh; Valiyaveettil, Suresh

    2011-06-10

    The isolation and characterization of carbon nanofibers from soot obtained by burning natural oil is reported. The fibers were extracted from the soot with tetrahydrofuran followed by sonication. The carbon nanofibers were mixed with poly(vinyl alcohol) and electrospun to get the nanofiber mat. The extraction ability of electrospun nanofibers for the separation and preconcentration of aromatic compounds such as 3-nitroaniline, 4-chloroaniline, 4-bromoaniline and 3,4-dichloroaniline were tested and efficiently evaluated using high performance liquid chromatography. Under optimized conditions, the method showed good linearity in a range of 0.5-50 μg L⁻¹ with correlation coefficient ranging from 0.989 to 0.998. High precision of the extraction with RSD values of 4.5-5.8% and low LOD value in a range of 0.009-0.081μg L⁻¹ for all aniline compounds were achieved. The proposed microextraction method offers advantages such as easy operation, high recovery, fast extraction, minimal use of organic solvent and elimination of tedious solvent evaporation and reconstitution steps. Copyright © 2011 Elsevier B.V. All rights reserved.

  7. Solid-phase extraction of the alcohol abuse biomarker phosphatidylethanol using newly synthesized polymeric sorbent materials containing quaternary heterocyclic groups.

    Science.gov (United States)

    Duarte, Mariana; Jagadeesan, Kishore Kumar; Billing, Johan; Yilmaz, Ecevit; Laurell, Thomas; Ekström, Simon

    2017-10-13

    Phosphatidylethanol (PEth) is an interesting biomarker finding increased use for detecting long term alcohol abuse with high specificity and sensitivity. Prior to detection, sample preparation is an unavoidable step in the work-flow of PEth analysis and new protocols may facilitate it. Solid-phase extraction (SPE) is a versatile sample preparation method widely spread in biomedical laboratories due to its simplicity of use and the possibility of automation. In this work, SPE was used for the first time to directly extract PEth from spiked human plasma and spiked human blood. A library of polymeric SPE materials with different surface functionalities was screened for PEth extraction in order to identify the surface characteristics that control PEth retention and recovery. The plasma samples were diluted 1:10 (v/v) in water and spiked at different concentrations ranging from 0.3 to 5μM. The library of SPE materials was then evaluated using the proposed SPE method and detection was done by LC-MS/MS. One SPE material efficiently retained and recovered PEth from spiked human plasma. With this insight, four new SPE materials were formulated and synthesized based on the surface characteristics of the best SPE material found in the first screening. These new materials were tested with spiked human blood, to better mimic a real clinical sample. All the newly synthetized materials outperformed the pre-existing commercially available materials. Recovery values for the new SPE materials were found between 29.5% and 48.6% for the extraction of PEth in spiked blood. A material based on quaternized 1-vinylimidazole with a poly(trimethylolpropane trimethacrylate) backbone was found suitable for PEth extraction in spiked blood showing the highest analyte recovery in this experiment, 48.6%±6.4%. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. 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}.

  9. New Functionalized Sol-Gel Hybrid Sorbent Coating for Stir Bar Sorptive Extraction of Selected Non-Steroidal Anti Inflammatory Drugs in Human Urine Samples

    International Nuclear Information System (INIS)

    Mashkurah Abd Rahim; Wan Aini Wan Ibrahim; Zainab Ramli; Mohd Marsin Sanagi

    2015-01-01

    A new sol-gel hybrid material, methyltrimethoxysilane-cyanopropyltriethoxysilane (MTMOS-CNPrTEOS) was successfully synthesized and used as a coating material in stir bar sorptive extraction (SBSE) of selected non-steroidal anti-inflammatory drugs (NSAIDs) in urine samples. The MTMOS-CNPrTEOS hybrid was synthesized by hydrolysis and condensation of MTMOS and CNPrTEOS in the presence of trifluoroacetic acid as catalyst via sol-gel method. Several factors influencing the synthesized sol-gel hybrid MTMOS-CNPrTEOS process such as mole ratio of MTMOS-CNPrTEOS, NaOH concentrations as etching solution, etching time, coating time and water content were investigated and optimized in this study. The optimum synthesis conditions obtained were 1:1 mol ratio of MTMOS-CNPrTEOS, 1 M NaOH as etching solution, 60 min etching time, 2 h coating time and 6 mmol water. The sol-gel hybrid MTMOS-CNPrTEOS synthesized under the optimum conditions was used to determine selected NSAIDs in human urine samples using normal stacking mode capillary electrophoresis with ultraviolet detection. MTMOS-CNPrTEOS SBSE method demonstrated good linearity (60 to 20,000 μg L -1 ) with excellent coefficient of determination (r 2 > 0.9990). The sol-gel hybrid MTMOS-CNPrTEOS SBSE method showed low limit of detection (35 - 41 μg L -1 ) with good precision (RSD < 6 %, n = 3) and excellent extraction recoveries (83.5 - 98.9 %) for the selected NSAIDs. The sol-gel hybrid MTMOS-CNPrTEOS SBSE method demonstrated good potential as an alternative sorbent in SBSE method for NSAIDs. (author)

  10. On-line dynamic fractionation and automatic determination of inorganic phosphorous in environmental solid substrates exploiting sequential injection microcolumn extraction and flow injection analysi

    DEFF Research Database (Denmark)

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

    2006-01-01

    Sequential injection microcolumn extraction (SI-MCE) based on the implementation of a soil containing microcartridge as external reactor in a sequential injection network is, for the first time, proposed for dynamic fractionation of macronutrients in environmental solids, as exemplified by the pa......Sequential injection microcolumn extraction (SI-MCE) based on the implementation of a soil containing microcartridge as external reactor in a sequential injection network is, for the first time, proposed for dynamic fractionation of macronutrients in environmental solids, as exemplified...... by the partitioning of inorganic phosphorous in agricultural soils. The on-line fractionation method capitalises on the accurate metering and sequential exposure of the various extractants to the solid sample by application of programmable flow as precisely coordinated by a syringe pump. Three different soil phase...... associations for phosphorus, that is, exchangeable, Al- and Fe-bound and Ca-bound fractions, were elucidated by accommodation in the flow manifold of the 3 steps of the Hietjles-Litjkema (HL) scheme involving the use of 1.0 M NH4Cl, 0.1 M NaOH and 0.5 M HCl, respectively, as sequential leaching reagents...

  11. Supercritical fluid extraction as an on-line clean-up technique for determination of riboflavin vitamins in food samples by capillary electrophoresis with fluorimetric detection.

    Science.gov (United States)

    Zougagh, Mohammed; Ríos, Angel

    2008-08-01

    An automatic method for the separation and determination of riboflavin (RF) vitamins (RF, flavin mononucleotide and flavin adenine dinucleotide) in food samples (chicken liver, tablet and powder milk) is proposed. The method is based on the on-line coupling of a supercritical fluid extractor (SFE) with a continuous flow-CE system with guided optical fiber fluorimetric detection (CF-CE-FD). The whole SFE-CF-CE-FD arrangement allowed the automatic treatment of food samples (clean-up of the sample followed by the extraction of the analytes), and the direct introduction of a small volume of the extracted plug to the CE-FD system for the determination of RF vitamins. Fluorescence detection introduced an appropriated sensitivity and contributed to avoid interferences of nonfluorescent polar compounds coming from the matrix samples in the extracted plug. Electrophoretic responses were linear within the 0.05-1 microg/g range, whereas the detection limits of RF vitamins were in the 0.036-0.042 microg/g range. The proposed arrangement opens up interesting prospects for the direct determination of polar analytes in complex samples with a good throughput and high level of automation.

  12. Characterisation of organic compounds in aerosol particles from a finnish forest by on-line coupled supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Shimmo, Masahiko; Jaentti, Jaana; Hartonen, Kari; Hyoetylaeinen, Tuulia; Riekkola, Marja-Liisa [Laboratory of Analytical Chemistry, Department of Chemistry, University of Helsinki, P.O. Box 55, 00014, Helsinki (Finland); Aalto, Pasi; Kulmala, Markku [Division of Atmospheric Sciences, Department of Physical Sciences, University of Helsinki, P.O. Box 64, 00014, Helsinki (Finland)

    2004-04-01

    During the European Union project Quantification of Aerosol Nucleation in the European Boundary Layer (QUEST), which began in spring 2003, atmospheric aerosol particles were collected in a Finnish Scots pine forest using a high-volume sampler. The organic compounds in the filter samples were then analysed by on-line coupled supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry (SFE-LC-GC-MS). The sample was first extracted by SFE. During LC the extracts were fractionated into three fractions according to polarity. The final separation was carried out by GC-MS. A fraction volume as high as 840 {mu}L was transferred to the GC, using the partial concurrent eluent evaporation technique. The same instrumentation, with an in-situ SFE derivatisation method, was used to analyse organic acids. Major compounds such as n-alkanes and PAH were analysed quantitatively. Their concentrations were lower than those usually observed in urban areas or in other forest areas in Europe. The wind direction was one of the most important factors affecting changes in the daily concentrations of these compounds. Scots pine needles were analysed with the same system to obtain reference data for identification of biogenic compounds in aerosol particles. Other organic compounds found in this study included hopanes, steranes, n-alkanals, n-alkan-2-ones, oxy-PAH, and alkyl-PAH; some biogenic products, including oxidation products of monoterpenes, were also identified. (orig.)

  13. Determination of etoricoxib in human plasma using automated on-line solid-phase extraction coupled with LC-APCI/MS/MS

    Directory of Open Access Journals (Sweden)

    Sérgio Luiz Dalmora

    2008-01-01

    Full Text Available A liquid chromatography-tandem mass spectrometry method with atmospheric pressure chemical ionization (LC-APCI/MS/MS was validated for the determination of etoricoxib in human plasma using antipyrin as internal standard, followed by on-line solid-phase extraction. The method was performed on a Luna C18 column and the mobile phase consisted of acetonitrile:water (95:5, v/v/ammonium acetate (pH 4.0; 10 mM, run at a flow rate of 0.6 mL/min. The method was linear in the range of 1-5000 ng/mL (r²>0.99. The lower limit of quantitation was 1 ng/mL. The recoveries were within 93.72-96.18%. Moreover, method validation demonstrated acceptable results for the precision, accuracy and stability studies.

  14. 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

  15. Evaluation of ionic liquids supported on silica as a sorbent for fully automated online solid-phase extraction with LC-MS determination of sulfonamides in bovine milk samples.

    Science.gov (United States)

    da Silva, Meire Ribeiro; Mauro Lanças, Fernando

    2018-03-10

    Sulfonamides are antibiotics widely used in the treatment of diseases in dairy cattle. However, their indiscriminate use for disease control may lead to their presence in tissues and milk and their determination requires a sample preparation step as part of an analytical approach. Among the several sample preparation techniques available, those based upon the use of sorptive materials have been widely employed. Recently, the application of ionic liquids immobilized on silica surfaces or polymeric materials has been evaluated for such an application. This manuscript addresses the evaluation of silica-based ionic liquid obtained by a sol-gel synthesis process by basic catalysis as sorbent for online solid-phase extraction with liquid chromatography and electrospray ionization time-of-flight mass spectrometry for sulfonamides determination. Infrared vibrational spectroscopy confirmed the presence of the ionic liquid on the silica surface, suggesting that the ionic liquid was anchored on to the silica surface. Other sorbents varying the ionic liquid alkyl chain were also synthesized and evaluated by off-line solid-phase extraction in the sulfonamide extraction. As the length of the alkyl chain increased, the amount of extracted sulfonamides decreased, possibly due to a decrease in the electrostatic interaction caused by the reduction in the polarity, as well as the presence of a hexafluorophosphate anion that increases the hydrophobic character of the material. The use of 1-butyl-3-methylimidazolium hexafluorophosphate as a selective ionic liquid sorbent enabled the isolation and sulfonamide preconcentration in bovine milk by online solid-phase extraction with liquid chromatography and electrospray ionization time-of-flight mass spectrometry. The limit of quantification for the method developed was 5-7, 5 μg/mL, with extraction recoveries ranging between 74 and 93% and intra- and interassay between 1.5-12.5 and 2.3-13.1, respectively. © 2018 WILEY-VCH Verlag Gmb

  16. Determination of enrofloxacin by room-temperature phosphorimetry after solid phase extraction on an acrylic polymer sorbent

    Science.gov (United States)

    de Souza, Cabrini F.; Martins, Renata K. S.; da Silva, Andrea R.; da Cunha, Alessandra L. M. C.; Aucélio, Ricardo Q.

    A phosphorimetric method was developed to enable the determination of enrofloxacin using photochemical derivatization which was used to both improve detection limits and to minimize the uncertainty of measurements. Phosphorescence was induced on cellulose containing TlNO3. Absolute limit of detection at the ng range and linear analytical response over three orders of magnitude were achieved. A metrological study was made to obtain the combined uncertainty value and to identify that the precision was mainly affected by the changing of substrates when measuring the signal from each replicate. Pharmaceutical formulations containing enrofloxacin were successfully analyzed by the method and the results were similar to the ones achieved using a HPLC method. A solid phase extraction on an acrylic polymer was optimized to separate enrofloxacin from interferents such as diclofenac and other components from biological matrices, which allowed the successful use of the method in urine analysis.

  17. Organically Modified Silica with Pyrazole-3-carbaldehyde as a New Sorbent for Solid-Liquid Extraction of Heavy Metals

    Directory of Open Access Journals (Sweden)

    Smaail Radi

    2013-12-01

    Full Text Available 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.

  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. Automated on-line solid phase extraction coupled to HPLC-APCI-MS detection as a versatile tool for the analysis of phenols in water samples

    International Nuclear Information System (INIS)

    Wissiack, R.

    2001-05-01

    In this work a liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (HPLC-APCI-MS) technique was developed for the determination of phenols and anilines in waste water samples. All relevant parameters were optimized for liquid chromatographic (LC) separation and mass spectrometric (MS) detection. Mass spectrometric detection was used in either negative ionization (NI) or positive ionization (PI) mode, which was depending on the physicochemical properties of the analyte. For screening analysis, full scan mode (SCAN) was used, while selected ion monitoring (SIM) mode of acquisition was used for maximum sensitivity. The optimal interface parameters and solvent compositions were evaluated, which mainly determined the ionization of analytes thus strongly influencing the sensitivity. The quasi-molecular ions were the most abundant signals both for phenols ([M-H]- in NI) and for anilines ([M+H]+ in PI). In general, fragmentation was hardly observed for one-ring phenols. Only fragmentation due to neutral losses of NO, HCl, NH3, CO2, CHO or CO from the functional groups were obtained via collision induced dissociation (CID) in a single quadrupole mass spectrometer. A further source of structural information was the relative intensity of positive and negative ions for one analyte: Only in the case of para-methyl substituted phenols, detection was also possible in positive ionization mode with reasonable sensitivity. In contrast to the phenols, anilines offered somewhat higher structural information due to increased fragmentation through CID, when detected in the positive ionization mode. The main goal of this work was the development of a method for the determination of US EPA priority phenols in different environmental matrices. As highest sensitivity and selectivity was required for this task, a preconcentrating step was necessary, and consequently solid phase extraction (SPE) was coupled on-line to HPLC-APCI-MS. The optimized method allowed the

  20. Determination of 18 veterinary antibiotics in environmental water using high-performance liquid chromatography-q-orbitrap combined with on-line solid-phase extraction.

    Science.gov (United States)

    Kim, Chansik; Ryu, Hong-Duck; Chung, Eu Gene; Kim, Yongseok

    2018-05-01

    The use of antibiotics and their occurrence in the environment have received significant attention in recent years owing to the generation of antibiotic-resistant bacteria. Antibiotic residues in water near livestock farming areas should be monitored to establish effective strategies for reducing the use of veterinary antibiotics. However, environmental water contamination resulting from veterinary antibiotics has not been studied extensively. In this work, we developed an analytical method for the simultaneous determination of multiple classes of veterinary antibiotic residues in environmental water using on-line solid-phase extraction (SPE)-high performance liquid chromatography (HPLC)-high resolution mass spectrometry (HRMS). Eighteen popular antibiotics (eight classes) were selected as target analytes based on veterinary antibiotics sales in South Korea in 2015. The developed method was validated by calibration-curve linearities, precisions, relative recoveries, and method detection limits (MDLs)/limits of quantification (LOQs) of the selected antibiotics, and applied to the analysis of environmental water samples (groundwater, river water, and wastewater-treatment-plant effluent). All calibration curves exhibited r 2  > 0.995 with MDLs ranging from 0.2 to 11.9 ng/L. Relative recoveries were between 50 and 150% with coefficients of variation below 20% for all analytes (spiked at 500 ng/L) in groundwater and river water samples. Relative standard deviations (RSDs) of standard-spiked samples were lower than 7% for all antibiotics. The on-line SPE system eliminates human-based SPE errors and affords excellent method reproducibility. Amoxicillin, ampicillin, clopidol, fenbendazole, flumequine, lincomycin, sulfadiazine, and trimethoprim were detected in environmental water samples in concentrations ranging from 1.26 to 127.49 ng/L. The developed method is a reliable analytical technique for the potential routine monitoring of veterinary antibiotics

  1. Determination of six microcystins and nodularin in surface and drinking waters by on-line solid phase extraction-ultra high pressure liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Beltrán, Eduardo; Ibáñez, María; Sancho, Juan Vicente; Hernández, Félix

    2012-11-30

    Microcystins and nodularin are cyclic peptides hepatotoxins produced by cyanobacterial genera (blue-green algae). Toxic cyanobacterial blooms are a worldwide problem, as reported in several countries, like China, Australia, or the United States. Therefore, it is necessary to develop sensitive and reliable analytical methodology to determine this type of toxins in water at parts per billion levels, or even lower. In this work, the potential of solid-phase extraction coupled on-line to ultra-high-pressure liquid chromatography/electrospray tandem mass spectrometry (SPE-UHPLC-MS/MS) has been investigated for the efficient quantification and confirmation of microcystins LR, RR, YR, LY, LW, LF and nodularin in surface and drinking water samples, at sub-ppb levels. The method developed involves the injection of only 1 mL of water sample into the on-line SPE-UHPLC-MS/MS system and allows the rapid determination of the compounds selected (8 min of chromatographic run), avoiding laborious sample treatment. The method was validated in surface and drinking water by means of recovery experiments at 0.25 and 1 μg L(-1). Average recoveries (n=5) ranged from 71 to 116%, with relative standard deviations (RSDs) lower than 15%. For microcystins LR, RR, YR and nodularin, a third level was also assayed (0.1 μg L(-1)) obtaining satisfactory data too. Limits of detection between 0.002 and 0.0405 μg L(-1) were estimated (0.0005 μg L(-1) for nodularin). The developed method was applied to the analysis of water samples collected in the province of Castellón (Spain). The acquisition of three MS/MS transitions for each compound allowed the unequivocal confirmation of positive samples, which was supported by the accomplishment of ion intensity ratios and retention time when compared with reference standards. Copyright © 2012 Elsevier B.V. All rights reserved.

  2. A comparative study of homemade C18 and commercial C18 sorbents for preconcentration of lead by minicolumn solid phase extraction

    International Nuclear Information System (INIS)

    Maltez, H.F.; Curtius, A.J.; Carasek, E.; Melo, L.F.C.; Sales Fontes Jardim, I.C.; Nascimento de Queiroz do, S.C.

    2004-01-01

    A comparative study of commercial C 18 chemically immobilized on silica and homemade C 18 , as sorbents for Pb complexed with 0,0-diethyl-dithiophosphate (DDTP) in a flow injection preconcentration system is reported. The homemade C 18 sorbent was obtained by sorption of poly(methyloctadecylsiloxane) (PMODS) on the silica support followed by immobilization using thermal treatment. The method follows the concept of green chemistry, since there are no toxic residues after synthesis. The complexed Pb was formed in 1.0 mol L -1 HCI medium and retained on the minicolumn filled with the sorbents. The elution was carried out using ethanol, and the richest 210 μL fraction was collected and analyzed by flame atomic absorption spectrometry. Chemical and flow variables were optimized for each sorbent. The results demonstrated that the performance of the proposed homemade C 18 sorbent for preconcentration of Pb complexed with DDTP is very similar to commercial C 18 chemically bonded on silica. By processing 25 mL, the enrichment factors were 129 and 125 for commercial C 18 and homemade C 18 , respectively. The limit of detection for commercial and homemade C 18 was 0.2 μg L -1 and 0.6 μg L -1 , respectively. The relative standard deviation (RSD) was lower than 1.2 % for both sorbents for a Pb concentration of 100 μg L -1 . The method was also applied successfully to the analysis of water samples, and the accuracy was tested by recovery measurements on spiked samples and biological reference material. (author)

  3. 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

  4. Desulfurization sorbent regeneration

    Science.gov (United States)

    Jalan, V.M.; Frost, D.G.

    1982-07-07

    A spent solid sorbent resulting from the removal of hydrogen sulfide from a fuel gas flow is regenerated with a steam-air mixture. The mixture of steam and air may also include additional nitrogen or carbon dioxide. The gas mixture contacts the spent sorbent containing metal sulfide at a temperature above 500/sup 0/C to regenerate the sulfide to metal oxide or carbonate. Various metal species including the period four transition metals and the lanthanides are suitable sorbents that may be regenerated by this method. In addition, the introduction of carbon dioxide gas permits carbonates such as those of strontium, barium and calcium to be regenerated. The steam permits regeneration of spent sorbent without formation of metal sulfate. Moreover, the regeneration will proceed with low oxygen concentrations and will occur without the increase in temperature to minimize the risk of sintering and densification of the sorbent. This method may be used for high-temperature fuel cells.

  5. Analysis of particulate polycyclic aromatic hydrocarbons by on-line coupled supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry

    Science.gov (United States)

    Shimmo, Masahiko; Adler, Heidi; Hyötyläinen, Tuulia; Hartonen, Kari; Kulmala, Markku; Riekkola, Marja-Liisa

    An on-line supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry (SFE-LC-GC-MS) method was developed for the analysis of the particulate polycyclic aromatic hydrocarbons (PAHs). The limits of detection of the system for the quantification standards were in the range of 0.25-0.57 ng, while the limits of determinations for filter samples varied from 0.02 to 0.04 ng m -3 (24 h sampling). The linearity was excellent from 5 to 300 ng ( R2>0.967). The analysis could be carried out in a closed system without tedious manual sample pretreatment and with no risk of errors by contamination or loss of the analytes. The results of the SFE-LC-GC-MS method were comparable with those for Soxhlet and shake-flask extractions with GC-MS. The new method was applied to the analysis of PAHs collected by high-volume filter in the Helsinki area to study the seasonal trend of the concentrations. The individual PAH concentrations varied from 0.015 to more than 1 ng m -3, while total PAH concentrations varied from 0.81 to 5.68 ng m -3. The concentrations were generally higher in winter than in summer. The mass percentage of the total PAHs in total suspended particulates ranged from 2.85×10 -3% in July to 15.0×10 -3% in December. Increased emissions in winter, meteorological conditions, and more serious artefacts during the sampling in summer season may explain the concentration profiles.

  6. Derivative spectrum chromatographic method for the determination of trimethoprim in honey samples using an on-line solid-phase extraction technique.

    Science.gov (United States)

    Uchiyama, Kazuhisa; Kondo, Mari; Yokochi, Rika; Takeuchi, Yuri; Yamamoto, Atsushi; Inoue, Yoshinori

    2011-07-01

    A simple, selective and rapid analytical method for determination of trimethoprim (TMP) in honey samples was developed and validated. This method is based on a SPE technique followed by HPLC with photodiode array detection. After dilution and filtration, aliquots of 500 μL honey samples were directly injected to an on-line SPE HPLC system. TMP was extracted on an RP SPE column, and separated on a hydrophilic interaction chromatography column during HPLC analysis. At the first detection step, the noise level of the photodiode array data was reduced with two-dimensional equalizer filtering, and then the smoothed data were subjected to derivative spectrum chromatography. On the second-derivative chromatogram at 254 nm, the limit of detection and the limit of quantification of TMP in a honey sample were 5 and 10 ng/g, respectively. The proposed method showed high accuracy (60-103%) with adequate sensitivity for TMP monitoring in honey samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    International Nuclear Information System (INIS)

    Singer, Heinz; Jaus, Sylvia; Hanke, Irene; Lueck, Alfred; Hollender, Juliane; Alder, Alfredo C.

    2010-01-01

    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.

  8. 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.

  9. Grafting the sol-gel based sorbents by diazonium salts: a novel approach toward unbreakable capillary microextraction.

    Science.gov (United States)

    Bagheri, Habib; Bayat, Parisa; Piri-Moghadam, Hamed

    2013-11-29

    The present work deals with a novel approach for grafting a sol-gel based sorbent, using diazonium salts for preparation of an unbreakable capillary microextraction (CME) device in on-line combination with high performance liquid chromatography (HPLC). The use of diazonium salts modifier allowed all types of metallic and non-metallic substrates to be used without any limitation. Substrates including copper, brass, stainless steel and polytetrafluoroethylene (PTFE) were chosen to be functionalized by chemical or electrochemical reduction of 4-amino phenyl acetic acid. Then, 3-(trimethoxysilyl)propylamine (3TMSPA) was selected as the precursor and the only reagent for preparation of the desired surface chemical bonded sorbent. The presence of chemical bond between substrate, diazonium salts and 3TMSPA is more probably responsible for thermal and solvent stability and long lifetime of the prepared sorbent. Characterization of the aryl group formation on the various substrates along with the prepared sorbents was thoroughly investigated by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and thermogravimetry analysis (TGA). Typically, one of the prepared sorbents, deposited on the inner surface of the copper tube, was selected for assessing the developed method. The CME device was used for on-line extraction of atrazine, ametryn and terbutryn, as model compounds, from the aquatic media. After extraction, the HPLC mobile phase was used for on-line desorption and elution of the extracted analytes from the CME loop, containing the grafted sol-gel based sorbent, through the HPLC column. Figures of merit of the developed method were also obtained in which the linearity for the analytes was in the range of 30-1000μgL(-1). The value of LOD (S/N=3) for all analytes was 10μgL(-1) and the RSD% values (n=5) were all below 9.4% at the 500μgL(-1) level. Applicability of the developed method was examined by analyzing some real water samples in

  10. Modified Activated Carbon Prepared from Acorn Shells as a New Solid-Phase Extraction Sorbent for the Preconcentration and Determination of Trace Amounts of Nickel in Food Samples Prior to Flame Atomic Absorption Spectrometry.

    Science.gov (United States)

    Ebrahimi, Bahram

    2017-03-01

    A new solid-phase extraction (SPE) sorbent was introduced based on acidic-modified (AM) activated carbon (AC) prepared from acorn shells of native oak trees in Kurdistan. Hydrochloric acid (15%, w/w) and nitric acid (32.5%, w/w) were used to condition and modify AC. The IR spectra of AC and AM-AC showed that AM lead to the formation of increasing numbers of acidic functional groups on AM-AC. AM-AC was used in the SPE method for the extraction and preconcentration of Ni+2 prior to flame atomic absorption spectrometric determination at ng/mL levels in model and real food samples. Effective parameters of the SPE procedure, such as the pH of the solutions, sorbent dosage, extraction time, sample volume, type of eluent, and matrix ions, were considered and optimized. An enrichment factor of 140 was obtained. The calibration curve was linear with an R2 of 0.997 in the concentration range of 1-220 ng/mL. The RSD was 5.67% (for n = 7), the LOD was 0.352 ng/mL, and relative recoveries in vegetable samples ranged from 96.7 to 103.7%.

  11. Sorbent Scoping Studies

    International Nuclear Information System (INIS)

    Chancellor, Christopher John

    2016-01-01

    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, to conduct scoping studies on the oxidizers and sorbents identified in AK review to inform the Quality Level 1 (QL1) testing, and to 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.

  12. 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, to conduct scoping studies on the oxidizers and sorbents identified in AK review to inform the Quality Level 1 (QL1) testing, and to 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.

  13. Profiling of tryptophan-related plasma indoles in patients with carcinoid tumors by automated, on-line, solid-phase extraction and HPLC with fluorescence detection.

    Science.gov (United States)

    Kema, I P; Meijer, W G; Meiborg, G; Ooms, B; Willemse, P H; de Vries, E G

    2001-10-01

    Profiling of the plasma indoles tryptophan, 5-hydroxytryptophan (5-HTP), serotonin, and 5-hydroxyindoleacetic acid (5-HIAA) is useful in the diagnosis and follow-up of patients with carcinoid tumors. We describe an automated method for the profiling of these indoles in protein-containing matrices as well as the plasma indole concentrations in healthy controls and patients with carcinoid tumors. Plasma, cerebrospinal fluid, and tissue homogenates were prepurified by automated on-line solid-phase extraction (SPE) in Hysphere Resin SH SPE cartridges containing strong hydrophobic polystyrene resin. Analytes were eluted from the SPE cartridge by column switching. Subsequent separation and detection were performed by reversed-phase HPLC combined with fluorometric detection in a total cycle time of 20 min. We obtained samples from 14 healthy controls and 17 patients with metastasized midgut carcinoid tumors for plasma indole analysis. In the patient group, urinary excretion of 5-HIAA and serotonin was compared with concentrations of plasma indoles. Within- and between-series CVs for indoles in platelet-rich plasma were 0.6-6.2% and 3.7-12%, respectively. Results for platelet-rich plasma serotonin compared favorably with those obtained by single-component analysis. Plasma 5-HIAA, but not 5-HTP was detectable in 8 of 17 patients with carcinoid tumors. In the patient group, platelet-rich plasma total tryptophan correlated negatively with platelet-rich plasma serotonin (P = 0.021; r = -0.56), urinary 5-HIAA (P = 0.003; r = -0.68), and urinary serotonin (P manual, single-component analyses.

  14. 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

  15. Solid-phase extraction of polar pesticides from environmental water samples on graphitized carbon and Empore-activated carbon disks and on-line coupling to octadecyl-bonded silica analytical columns.

    NARCIS (Netherlands)

    Slobodník, J.; Oztekizan, O.; Lingeman, H.; Brinkman, U.A.T.

    1996-01-01

    The suitability of Empore-activated carbon disks (EACD), Envi-Carb graphitized carbon black (GCB) and CPP-50 graphitized carbon for the trace enrichment of polar pesticides from water samples was studied by means of off-line and on-line solid-phase extraction (SPE). In the off-line procedure, 0.5-2

  16. Rapid and simple one-step membrane extraction for the determination of 8-hydroxy-2'-deoxyguanosine in human plasma by a combination of on-line solid phase extraction and LC-MS/MS.

    Science.gov (United States)

    Wang, Chien-Jen; Yang, Ning-Hsiang; Chang, Chia-Chi; Liou, Saou-Hsing; Lee, Hui-Ling

    2011-11-15

    A quantitative analytical method using automated on-line solid phase extraction (SPE) and liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS) for the determination of 8-OHdG (8-hydroxy-2'-deoxyguanosine) in human plasma was developed and validated. A one-step membrane extraction method for the plasma sample preparation and a C18 SPE column with simple extraction and purification were used for the on-line extraction. A C18 column was employed for LC separation and ESI-MS/MS was utilized for detection. (15)N(5)-8-OHdG ((15)N(5)-8-hydroxy-2'-deoxyguanosine) was used as an internal standard for quantitative determination. The extraction, clean-up and analysis procedures were controlled by a fully automated six-port switch valve as one strategy to reduce the matrix effect and simultaneously improve detection sensitivity. Identification and quantification were based on the following transitions: m/z 284→168 for 8-OHdG and m/z 289→173 for (15)N(5)-8-OHdG. Satisfactory recovery was obtained, and the recovery ranged from 95.1 to 106.1% at trace levels in human plasma and urine, with a CV lower than 5.4%. Values for intraday and interday precision were between 2.3 and 6.8% for plasma and between 2.7 and 4.5% for urine, respectively. Values for the method accuracy of intraday and interday assays ranged from 93.0 and 100.5% for plasma and 110.2 and 119.4% for urine, respectively. The limits of detection (LOD) and LOQ were 0.008 ng/mL and 0.02 ng/mL, respectively.The applicability of this newly developed method was demonstrated by analysis of human plasma samples for an evaluation of the future risk of oxidative stress status in human exposure to nanoparticles and other diseases. Crown Copyright © 2011. Published by Elsevier B.V. All rights reserved.

  17. Mercury removal sorbents

    Science.gov (United States)

    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.

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

    Science.gov (United States)

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

    2017-07-01

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

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

    Science.gov (United States)

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

    2015-08-07

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

  20. Zero valent Fe-reduced graphene oxide quantum dots as a novel magnetic dispersive solid phase microextraction sorbent for extraction of organophosphorus pesticides in real water and fruit juice samples prior to analysis by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Akbarzade, Samaneh; Chamsaz, Mahmoud; Rounaghi, Gholam Hossein; Ghorbani, Mahdi

    2018-01-01

    A selective and sensitive magnetic dispersive solid-phase microextraction (MDSPME) coupled with gas chromatography-mass spectrometry was developed for extraction and determination of organophosphorus pesticides (Sevin, Fenitrothion, Malathion, Parathion, and Diazinon) in fruit juice and real water samples. Zero valent Fe-reduced graphene oxide quantum dots (rGOQDs@ Fe) as a new and effective sorbent were prepared and applied for extraction of organophosphorus pesticides using MDSPME method. In order to study the performance of this new sorbent, the ability of rGOQDs@ Fe was compared with graphene oxide and magnetic graphene oxide nanocomposite by recovery experiments of the organophosphorus pesticides. Several affecting parameters in the microextraction procedure, including pH of donor phase, donor phase volume, stirring rate, extraction time, and desorption conditions such as the type and volume of solvents and desorption time were thoroughly investigated and optimized. Under the optimal conditions, the method showed a wide linear dynamic range with R-square between 0.9959 and 0.9991. The limit of detections, the intraday and interday relative standard deviations (n = 5) were less than 0.07 ngmL -1 , 4.7, and 8.6%, respectively. The method was successfully applied for extraction and determination of organophosphorus pesticides in real water samples (well, river and tap water) and fruit juice samples (apple and grape juice). The obtained relative recoveries were in the range of 82.9%-113.2% with RSD percentages of less than 5.8% for all the real samples.

  1. Evaluation of bi-functionalized mesoporous silicas as reversed phase/cation-exchange mixed-mode sorbents for multi-residue solid phase extraction of veterinary drug residues in meat samples.

    Science.gov (United States)

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

    2017-04-01

    A SBA-15 type mesoporous silica was synthesized and bi-functionalized with octadecylsilane (C18) or octylsilane (C8), and sulfonic acid (SO 3 - ) groups in order to obtain materials with reversed-phase/strong cation-exchange mixed-mode retention mechanism. The resulting hybrid materials (SBA-15-C18-SO 3 - and SBA-15-C8-SO 3 - ) were comprehensively characterized. They showed high surface area, high pore volume and controlled porous size. Elemental analysis of the materials revealed differences in the amount of C18 and C8. SBA-15-C18-SO 3 - contained 0.19mmol/g of C18, while SBA-15-C8-SO 3 - presented 0.54mmol/g of C8. The SO 3 - groups anchored to the silica surface of the pore walls were 0.20 and 0.09mmol/g, respectively. The bi-functionalized materials were evaluated as SPE sorbents for the multi-residue extraction of 26 veterinary drug residues in meat samples using ultra-high-performance liquid chromatography coupled to mass spectrometry detector (UHPLC-MS/MS). Different sorbent amounts (100 and 200mg) and organic solvents were tested to optimize the extraction procedure. Both silicas showed big extraction potential and were successful in the extraction of the target analytes. The mixed-mode retention mechanism was confirmed by comparing both silicas with SBA-15 mesoporous silica mono-functionalized with C18 and C8. Best results were achieved with 200mg of SBA-15-C18-SO 3 - obtaining recoveries higher than 70% for the majority of analytes. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. On-line solid phase extraction-liquid chromatography-tandem mass spectrometry for insect repellent residue analysis in surface waters using atmospheric pressure photoionization.

    Science.gov (United States)

    Molins-Delgado, Daniel; García-Sillero, Daniel; Díaz-Cruz, M Silvia; Barceló, Damià

    2018-04-06

    Insect repellents (IRs) are a group of organic chemicals whose function is to prevent the ability of insects of landing in a surface. These compounds have been found in the environment and may pose a risk to non-target organisms. In this study, an on-line solid phase extraction - high performance liquid chromatography-tandem mass spectrometry multiresidue method was developed using an atmospheric photoionization source (SPE-HPLC-(APPI)-MS/MS). The use of the APPI as an alternative ionization technique to electrospray (ESI) and atmospheric pressure chemical ionization (APCI) allowed expanding the range of analytical techniques suitable for the analysis of IRs, so far relied in gas chromatography. High sensitivity and precision was reached with method limits of quantification between 0.2 and 4.6 ng l -1 and interday and intraday precision equal or below 15%. The validated method was applied to the study of surface water samples from three European river basins with different flow regime (Adige River in Italy, Sava River in the Balkans, and Evrotas River in Greece). The results showed that two IRs (DEET and Bayrepel) were ubiquitous in the Sava and Evrotas basins, reaching concentrations as high as 105 μg l -1 of Bayrepel in the Sava River, and 5 μg l -1 of DEET in the Evrotas River. Densely populated areas and effluent waste waters are pointed out as the responsible for this pollution. In the alpine river Adige, only three samples showed low levels of IRs (6.01-37.8 ng l -1 ). The concentrations measured were used to perform an environmental risk assessment based on the hazard quotients (HQs) estimation approach by using the chronic and acute eco-toxicity data available. The results revealed that despite the high frequency and eventually high concentrations of these IRs determined in the three basins, only few sites were at risk, with 1 < HQs < 3.3. Copyright © 2018 The Author(s). Published by Elsevier B.V. All rights reserved.

  3. 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

  4. 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

    International Nuclear Information System (INIS)

    Sigrist, Mirna; Albertengo, Antonela; Beldomenico, Horacio; Tudino, Mabel

    2011-01-01

    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 3 generation using 3.5 mol L -1 HCl as carrier solution and 0.35% (m/v) NaBH 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 - , SO 4 2- , NO 3 - , HPO 4 2- , HCO 3 - 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 6 H 8 O 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 μg L -1 and 0.6 μg L -1 for As(III) and inorganic total As, respectively, were obtained for a 500 μL 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 -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 separation was performed through the employ of a serial connection of membrane filters and

  5. Per- and polyfluoroalkyl substances and fluorinated alternatives in urine and serum by on-line solid phase extraction-liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Kato, Kayoko; Kalathil, Akil A; Patel, Ayesha M; Ye, Xiaoyun; Calafat, Antonia M

    2018-06-14

    Per- and polyfluoroalkyl substances (PFAS), man-made chemicals with variable length carbon chains containing the perfluoroalkyl moiety (C n F 2n+1 -), are used in many commercial applications. Since 1999-2000, several long-chain PFAS, including perfluorooctane sulfonate (PFOS) and perfluorooctanoate (PFOA), have been detected at trace levels in the blood of most participants of the National Health and Nutrition Examination Survey (NHANES)-representative samples of the U.S. general population-while short-chain PFAS have not. Lower detection frequencies and concentration ranges may reflect lower exposure to short-chain PFAS than to PFOS or PFOA or that, in humans, short-chain PFAS efficiently eliminate in urine. We developed on-line solid phase extraction-HPLC-isotope dilution-MS/MS methods for the quantification in 50 μL of urine or serum of 15 C 3 -C 11 PFAS (C 3 only in urine), and three fluorinated alternatives used as PFOA or PFOS replacements: GenX (ammonium salt of 2,3,3,3,-tetrafluoro-2-(1,1,2,2,3,3,3-heptafluoropropoxy)-propanoate, also known as HFPO-DA), ADONA (ammonium salt of 4,8-dioxa-3H-perfluorononanoate), and 9Cl-PF3ONS (9-chlorohexadecafluoro-3-oxanonane-1-sulfonate), main component of F53-B. Limit of detection for all analytes was 0.1 ng/mL. To validate the method, we analyzed 50 commercial urine/serum paired samples collected in 2016 from U.S. volunteers with no known exposure to the chemicals. In serum, detection frequency and concentration patterns agreed well with those from NHANES. By contrast, except for perfluorobutanoate, we did not detect long-chain or short-chain PFAS in urine. Also, we did not detect fluorinated alternatives in either urine or serum. Together, these results suggest limited exposure to both short-chain PFAS and select fluorinated alternatives in this convenience population. Copyright © 2018. Published by Elsevier Ltd.

  6. 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 (CoFe 2 O 4 -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.

  7. On-line separation and preconcentration of lead(II) by solid-phase extraction using activated carbon loaded with xylenol orange and its determination by flame atomic absorption spectrometry.

    Science.gov (United States)

    Ensafi, Ali A; Shiraz, A Zendegi

    2008-02-11

    Activated carbon loaded with xylenol orange in a mini-column was used for the highly selective separation and preconcentration of Pb(II) ions. An on-line system for enrichment and the determination of Pb(II) was carried out on flame atomic absorption spectrometry. The conditions of preconcentration and quantitative recovery of Pb(II) from diluted solution, such as pH of aqueous phase, amount of the sorbent, volume of the solutions and flow variables were studied as well as effect of potential interfering ions. Under the optimum conditions, Pb(II) in an aqueous sample was concentrated about 200-fold and the detection limit was 0.4 ng mL(-1) Pb(II). The adsorption capacity of the solid phase was 0.20mg of lead per one gram of the modified activated carbon. The modified activated carbon is stable for several treatments of sample solutions without the need for using any chemical reagent. The recovery of lead(II) from river water, waste water, tap water, and in the following reference materials: SRM 2711 Montana soil and GBW-07605 tea were obtained in the range of 97-104% by the proposed method.

  8. On-line separation and preconcentration of lead(II) by solid-phase extraction using activated carbon loaded with xylenol orange and its determination by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Ensafi, Ali A.; Shiraz, A. Zendegi

    2008-01-01

    Activated carbon loaded with xylenol orange in a mini-column was used for the highly selective separation and preconcentration of Pb(II) ions. An on-line system for enrichment and the determination of Pb(II) was carried out on flame atomic absorption spectrometry. The conditions of preconcentration and quantitative recovery of Pb(II) from diluted solution, such as pH of aqueous phase, amount of the sorbent, volume of the solutions and flow variables were studied as well as effect of potential interfering ions. Under the optimum conditions, Pb(II) in an aqueous sample was concentrated about 200-fold and the detection limit was 0.4 ng mL -1 Pb(II). The adsorption capacity of the solid phase was 0.20 mg of lead per one gram of the modified activated carbon. The modified activated carbon is stable for several treatments of sample solutions without the need for using any chemical reagent. The recovery of lead(II) from river water, waste water, tap water, and in the following reference materials: SRM 2711 Montana soil and GBW-07605 tea were obtained in the range of 97-104% by the proposed method

  9. On-line separation and preconcentration of lead(II) by solid-phase extraction using activated carbon loaded with xylenol orange and its determination by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ensafi, Ali A. [College of Chemistry, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of)], E-mail: Ensafi@cc.iut.ac.ir; Shiraz, A. Zendegi [College of Chemistry, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of)

    2008-02-11

    Activated carbon loaded with xylenol orange in a mini-column was used for the highly selective separation and preconcentration of Pb(II) ions. An on-line system for enrichment and the determination of Pb(II) was carried out on flame atomic absorption spectrometry. The conditions of preconcentration and quantitative recovery of Pb(II) from diluted solution, such as pH of aqueous phase, amount of the sorbent, volume of the solutions and flow variables were studied as well as effect of potential interfering ions. Under the optimum conditions, Pb(II) in an aqueous sample was concentrated about 200-fold and the detection limit was 0.4 ng mL{sup -1} Pb(II). The adsorption capacity of the solid phase was 0.20 mg of lead per one gram of the modified activated carbon. The modified activated carbon is stable for several treatments of sample solutions without the need for using any chemical reagent. The recovery of lead(II) from river water, waste water, tap water, and in the following reference materials: SRM 2711 Montana soil and GBW-07605 tea were obtained in the range of 97-104% by the proposed method.

  10. Space-filling polyhedral sorbents

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

  12. Application of polyurethane foam as a sorbent for trace metal pre-concentration — A review

    Science.gov (United States)

    Lemos, V. A.; Santos, M. S.; Santos, E. S.; Santos, M. J. S.; dos Santos, W. N. L.; Souza, A. S.; de Jesus, D. S.; das Virgens, C. F.; Carvalho, M. S.; Oleszczuk, N.; Vale, M. G. R.; Welz, B.; Ferreira, S. L. C.

    2007-01-01

    The first publication on the use of polyurethane foam (PUF) for sorption processes dates back to 1970, and soon after the material was applied for separation processes. The application of PUF as a sorbent for solid phase extraction of inorganic analytes for separation and pre-concentration purposes is reviewed. The physical and chemical characteristics of PUF (polyether and polyester type) are discussed and an introduction to the characterization of these sorption processes using different types of isotherms is given. Separation and pre-concentration methods using unloaded and loaded PUF in batch and on-line procedures with continuous flow and flow injection systems are presented. Methods for the direct solid sampling analysis of the PUF after pre-concentration are discussed as well as approaches for speciation analysis. Thermodynamic proprieties of some extraction processes are evaluated and the interpretation of determined parameters, such as enthalpy, entropy and Gibbs free energy in light of the physico-chemical processes is explained.

  13. PROCEEDINGS: MULTIPOLLUTANT SORBENT REACTIVITY ...

    Science.gov (United States)

    The report is a compilation of technical papers and visual aids presented by representatives of industry, academia, and government agencies at a workshop on multipollutant sorbent reactivity that was held at EPA's Environmental Research Center in Research Triangle Park, NC, on July 19-20, 1994. There were 16 technical presentations in three sessions, and a panel discussion between six research experts. The workshop was a forum for the exchange of ideas and information on the use of sorbents to control air emissions of acid gases (sulfur dioxide, nitrogen oxides, and hydrogen chloride); mercury and dioxins; and toxic metals, primarily from fossil fuel combustion. A secondary purpose for conducting the workshop was to help guide EPA's research planning activities. A general theme of the workshop was that a strategy of controlling many pollutants with a single system rather than systems to control individual pollutants should be a research goal. Some research needs cited were: hazardous air pollutant removal by flue gas desulfurization systems, dioxin formation and control, mercury control, waste minimization, impact of ash recycling on metals partitioning, impact of urea and sorbents on other pollutants, high temperature filtration, impact of coal cleaning on metals partitioning, and modeling dispersion of sorbents in flue gas. information

  14. 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...... the Measurements and Testing Programme of the European Commission) sequential extraction scheme. Employing a peristaltic pump as liquid driver, alternate directional flows of the extractants are used to overcome compression of the solid particles within the extraction unit to ensure a steady partitioning flow rate...... and thus to maintain constant operationally defined extraction conditions. The proposed flow set-up is proven to allow for trouble-free handling of soil samples up to 1 g and flow rates ≤ 10 mL min–1. The miniaturized extraction system was coupled to ICP-MS through a flow injection interface in order...

  15. Tantala-based sol-gel coating for capillary microextraction on-line coupled to high-performance liquid chromatography.

    Science.gov (United States)

    Tran, MinhPhuong; Turner, Erica B; Segro, Scott S; Fang, Li; Seyyal, Emre; Malik, Abdul

    2017-11-03

    A sol-gel organic-inorganic hybrid sorbent, consisting of chemically integrated tantalum (V) ethoxide (TaEO) and polypropylene glycol methacrylate (PPGM), was developed for capillary microextraction (CME). The sol-gel sorbent was synthesized within a fused silica capillary through hydrolytic polycondensation of TaEO and chemical incorporation of PPGM into the evolving sol-gel tantala network. A part of the organic-inorganic hybrid sol-gel network evolving in the vicinity of the capillary walls had favorable conditions to get chemically bonded to the silanol groups on the capillary surface forming a surface-bonded coating. The newly developed sol-gel sorbent was employed to isolate and enrich a variety of analytes from aqueous samples for on-line analysis by high-performance liquid chromatography (HPLC) equipped with a UV detector. CME was performed on aqueous samples containing trace concentrations of analytes representing polycyclic aromatic hydrocarbons, ketones, alcohols, amines, nucleosides, and nucleotides. This sol-gel hybrid coating provided efficient extraction with CME-HPLC detection limits ranging from 4.41pM to 28.19 pM. Due to direct chemical bonding between the sol-gel sorbent coating and the fused silica capillary inner surface, this sol-gel sorbent exhibited enhanced solvent stability. The sol-gel tantala-based sorbent also exhibited excellent pH stability over a wide pH range (pH 0-pH 14). Furthermore, it displayed great performance reproducibility in CME-HPLC providing run-to-run HPLC peak area relative standard deviation (RSD) values between 0.23% and 3.83%. The capillary-to-capillary RSD (n=3), characterizing capillary preparation method reproducibility, ranged from 0.24% to 4.11%. The results show great performance consistency and application potential for the sol-gel tantala-PPGM sorbent in various fields including biomedical, pharmaceutical, and environmental areas. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Design of engineered sorbent barriers

    International Nuclear Information System (INIS)

    Jones, E.O.; Freeman, H.D.

    1988-08-01

    A sorbent barrier uses sorbent material such as activated carbon or natural zeolites to prevent the migration of radionuclides from a low-level waste site to the aquifer. The sorbent barrier retards the movement of radioactive contaminants, thereby providing time for the radionuclides to decay. Sorbent barriers can be a simple, effective, and inexpensive method for reducing the migration of radionuclides to the environment. Designing a sorbent barrier consists of using soil and sorbent material properties and site conditions as input to a model which will determine the necessary sorbent barrier thickness to meet contaminant limits. The paper will cover the following areas: techniques for measuring sorption properties of barrier materials and underlying soils, use of a radionuclide transport model to determine the required barrier thickness and performance under a variety of site conditions, and cost estimates for applying the barrier. 8 refs., 6 figs., 1 tab

  17. Design of engineered sorbent barriers

    International Nuclear Information System (INIS)

    Jones, E.O.; Freeman, H.D.

    1988-01-01

    A sorbent barrier uses sorbent material such as activated carbon or natural zeolites to prevent the migration of radionuclides from a low-level waste site to the aquifer. The sorbent barrier retards the movement of radioactive contaminants, thereby providing time for the radionuclides to decay. Sorbent barriers can be a simple, effective, and inexpensive method for reducing the migration of radionuclides to the environment. Designing a sorbent barrier consists of using soil and sorbent material properties and site conditions as input to a model which will determine the necessary sorbent barrier thickness to meet contaminant limits. The paper covers the following areas: techniques for measuring sorption properties of barrier materials and underlying soils, use of a radionuclide transport model to determine the required barrier thickness and performance under a variety of site conditions, and cost estimates for applying the barrier

  18. Multiresidue analysis of oestrogenic compounds in cow, goat, sheep and human milk using core-shell polydopamine coated magnetic nanoparticles as extraction sorbent in micro-dispersive solid-phase extraction followed by ultra-high-performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Socas-Rodríguez, Bárbara; Hernández-Borges, Javier; Herrera-Herrera, Antonio V; Rodríguez-Delgado, Miguel Ángel

    2018-03-01

    In this work, the suitability of Fe 3 O 4 nanoparticles coated with polydopamine was evaluated as sorbent for the extraction of a group of 21 compounds with oestrogenic activity including seven phytoestrogens, six mycotoxins as well as four synthetic and four natural oestrogens from different types of milk, including sheep milk, in which the evaluation of oestrogenic compounds have never been developed before. Extraction was carried out using magnetic micro-dispersive solid-phase extraction after a previous deproteinisation step. Separation, determination and quantification of the target analytes were achieved by ultra-high-performance liquid chromatography coupled to triple quadrupole-tandem mass spectrometry. The methodology was validated for five milk samples using 17β-estradiol-2,4,16,16,17-d 5 as internal standard for natural and synthetic oestrogens, β-zearalanol-10,10,11,12,12-d 5 for mycotoxins and prunetin for phytoestrogens. Recovery values ranged from 70 to 120% for the five types of matrices with relative standard deviation values lower than 18%. Limits of quantification of the method were in the range 0.55-11.8 μg L -1 for all samples. Graphical abstract General scheme of the multiresidue analysis of oestrogenic compounds in milk using core-shell polydopamine coated magnetic nanoparticles as extraction sorbent in μ-dSPE.

  19. Application of sunflower stalk-carbon nitride nanosheets as a green sorbent in the solid-phase extraction of polycyclic aromatic hydrocarbons followed by high-performance liquid chromatography.

    Science.gov (United States)

    Marzi Khosrowshahi, Elnaz; Razmi, Habib

    2018-02-08

    A green biocomposite of sunflower stalks and graphitic carbon nitride nanosheets has been applied as a solid-phase extraction adsorbent for sample preparation of five polycyclic aromatic hydrocarbons in different solutions using high-performance liquid chromatography with ultraviolet detection. Before the modification, sunflower stalks exhibited relatively low adsorption to the polycyclic aromatic hydrocarbons extraction. The modified sunflower stalks showed increased adsorption to the analytes extraction due to the increase in surface and existence of a π-π interaction between the analytes and graphitic carbon nitride nanosheets on the surface. Under the optimal conditions, the limits of detection and quantification for five polycyclic aromatic hydrocarbons compounds could reach 0.4-32 and 1.2-95 ng/L, respectively. The method accuracy was evaluated using recovery measurements in spiked real samples and good recoveries from 71 to 115% with relative standard deviations of polycyclic aromatic hydrocarbons determination in various samples-well water, tap water, soil, vegetable, and barbequed meat (kebab)-with analytes contents ranging from 0.065 to 13.3 μg/L. The prepared green composite as a new sorbent has some advantages including ease of preparation, low cost, and good reusability. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Effects of push/pull perfusion and ultrasonication on the extraction efficiencies of phthalate esters in sports drink samples using on-line hollow-fiber liquid-phase microextraction.

    Science.gov (United States)

    Chao, Yu-Ying; Lee, Chien-Hung; Chien, Tzu-Yang; Shih, Yu-Hsuan; Lu, Yin-An; Kuo, Ting-Hsuan; Huang, Yeou-Lih

    2013-08-28

    In previous studies, we developed a process, on-line ultrasound-assisted push/pull perfusion hollow-fiber liquid-phase microextraction (UA-PPP-HF-LPME), combining the techniques of push/pull perfusion (PPP) and ultrasonication with hollow-fiber liquid-phase microextraction (HF-LPME), to achieve rapid extraction of acidic phenols from water samples. In this present study, we further evaluated three more-advanced and novel effects of PPP and ultrasonication on the extraction efficiencies of neutral high-molecular-weight phthalate esters (HPAEs) in sports drinks. First, we found that inner-fiber fluid leakage occurs only in push-only perfusion-based and pull-only perfusion-based HF-LPME, but not in the PPP mode. Second, we identified a significant negative interaction between ultrasonication and temperature. Third, we found that the extraction time of the newly proposed system could be shortened by more than 93%. From an investigation of the factors affecting UA-PPP-HF-LPME, we established optimal extraction conditions and achieved acceptable on-line enrichment factors of 92-146 for HPAEs with a sampling time of just 2 min.

  1. Ultra-trace levels analysis of microcystins and nodularin in surface water by on-line solid-phase extraction with high-performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Balest, Lydia; Murgolo, Sapia; Sciancalepore, Lucia; Montemurro, Patrizia; Abis, Pier Paolo; Pastore, Carlo; Mascolo, Giuseppe

    2016-06-01

    An on-line solid phase extraction coupled with high-performance liquid chromatography in tandem with mass spectrometry (on-line SPE/HPLC/MS-MS) method for the determination of five microcystins and nodularin in surface waters at submicrogram per liter concentrations has been optimized. Maximum recoveries were achieved by carefully optimizing the extraction sample volume, loading solvent, wash solvent, and pH of the sample. The developed method was also validated according to both UNI EN ISO IEC 17025 and UNICHIM guidelines. Specifically, ten analytical runs were performed at three different concentration levels using a reference mix solution containing the six analytes. The method was applied for monitoring the concentrations of microcystins and nodularin in real surface water during a sampling campaign of 9 months in which the ELISA method was used as standard official method. The results of the two methods were compared showing good agreement when the highest concentration values of MCs were found. Graphical abstract An on-line SPE/HPLC/MS-MS method for the determination of five microcystins and nodularin in surface waters at sub μg L(-1) was optimized and compared with ELISA assay method for real samples.

  2. Primary secondary amine as a sorbent material in dispersive solid-phase extraction clean-up for the determination of indicator polychlorinated biphenyls in environmental water samples by gas chromatography with electron capture detection.

    Science.gov (United States)

    Guo, Yuanming; Hu, Hongmei; Li, Tiejun; Xue, Lijian; Zhang, Xiaoning; Zhong, Zhi; Zhang, Yurong; Jin, Yanjian

    2017-08-01

    A simple, rapid, and novel method has been developed and validated for determination of seven indicator polychlorinated biphenyls in water samples by gas chromatography with electron capture detection. 1 L of water samples containing 30 g of anhydrous sodium sulfate was first liquid-liquid extracted with an automated Jipad-6XB vertical oscillator using n-hexane/dichloromethane (1:1, v/v). The concentrated extract was cleaned up by dispersive solid-phase extraction with 100 mg of primary secondary amine as sorbent material. The linearity of this method ranged from 1.25 to 100 μg/L, with regression coefficients ranging between 0.9994 and 0.9999. The limits of detection were in the ng/L level, ranging between 0.2 and 0.3 ng/L. The recoveries of seven spiked polychlorinated biphenyls with external calibration method at different concentration levels in tap water, lake water, and sea water were in the ranges of 85-112, 76-116, and 72-108%, respectively, and with relative standard deviations of 3.3-4.5, 3.4-5.6, and 3.1-4.8% (n = 5), respectively. The performance of the proposed method was compared with traditional liquid-liquid extraction and solid-phase extraction clean-up methods, and comparable efficiencies were obtained. It is concluded that this method can be successfully applied for the determination of polychlorinated biphenyls in different water samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. On-line solid-phase extraction coupled to liquid chromatography tandem mass spectrometry for the analysis of cyanotoxins in algal blooms.

    Science.gov (United States)

    Fayad, Paul B; Roy-Lachapelle, Audrey; Duy, Sung Vo; Prévost, Michèle; Sauvé, Sébastien

    2015-12-15

    An analytical method based on on-line SPE-LC-HESI-MS/MS has been developed for the detection and quantification of eight selected cyanotoxins in algal bloom waters that include mycrocystins, anatoxin-a and cylindrospermopsin. The injection volume was 2 mL according to the expected concentration of cyanotoxins in matrix. The method provides an analysis time of 7 min per sample, acceptable recovery values (91-101%), good precision (RSD cyanotoxins. All of the targeted cyanotoxins were detected with the exception of cylindrospermopsin. In addition, it was found that total microcystin concentrations in several surface water samples exceeded the proposed guidelines established by the province of Québec in Canada of 1.5 μg L(-1) as well as the World Health Organization of 1 μg L(-1) for both free and cell-bound microcystin-LR equivalent. Copyright © 2015 Elsevier Ltd. All rights reserved.

  4. A novel hierarchical nanobiocomposite of graphene oxide-magnetic chitosan grafted with mercapto as a solid phase extraction sorbent for the determination of mercury ions in environmental water samples.

    Science.gov (United States)

    Ziaei, Ehsan; Mehdinia, Ali; Jabbari, Ali

    2014-11-19

    New mercapto-grafted graphene oxide-magnetic chitosan (GO-MC) has been developed as a novel biosorbent for the preconcentration and extraction of mercury ion from water samples. A facile and ecofriendly synthesis procedure was also developed for modification of GO-MC with 3-mercaptopropyltrimethoxysilane. The prepared nanocomposite material (mercapto/GO-MC) was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and energy-dispersive X-ray spectroscopy (EDX). The mercury analysis was performed by continuous-flow cold vapor atomic absorption spectrometry. The parameters affecting the extraction and preconcentration processes were carried out. The optimum conditions were found to be 60mg of sorbent, pH of 6.5, 10min for adsorption time, 3mL of HCl (0.1mol L(-1))/thiourea (2% w/v) as the eluent and 250mL for breakthrough volume. An excellent linearity was achieved in the range of 0.12-80ng mL(-1) (R(2)=0.999) at a preconcentration factor of 80. The limit of detection and quantification were achieved as 0.06ng mL(-1) and 0.12ng mL(-1), respectively. A good repeatability was obtained with the relative standard deviation (RSD) of 4.7%. Furthermore, real water samples were analyzed and good recoveries were obtained from 95 to 100%. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Halloysite nanotubes as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction for the determination of bismuth in water samples using high-resolution continuum source graphite-furnace atomic absorption spectrometry

    Science.gov (United States)

    Krawczyk-Coda, Magdalena

    2017-03-01

    In this research, a simple, accurate, and inexpensive preconcentration procedure was developed for the determination of bismuth in water samples, using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). During the preconcentration step, halloysite nanotubes (HNTs) were used as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction (USA DMSPE). The influence of the pH of the sample solution, amount of HNTs, and extraction time, as well as of the main parameters of HR CS GFAAS, on absorbance was investigated. The limit of detection was 0.005 μg L- 1. The preconcentration factor achieved for bismuth was 32. The relative standard deviation (RSD) was 4%. The accuracy of this method was validated by analyses of NIST SRM 1643e (Trace elements in water) and TMDA-54.5 (A high level fortified sample for trace elements) certified reference materials. The measured bismuth contents in these certified reference materials were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. The proposed method has been successfully applied to the determination of bismuth in five different real water samples (seawater, lake water, river water, stream water and rain water).

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

    International Nuclear Information System (INIS)

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

    2013-01-01

    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.

  7. 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

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

  9. Evaluation of a new carbon/zirconia-based sorbent for the 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...

  10. Rapid and automated on-line solid phase extraction HPLC-MS/MS with peak focusing for the determination of ochratoxin A in wine samples.

    Science.gov (United States)

    Campone, Luca; Piccinelli, Anna Lisa; Celano, Rita; Pagano, Imma; Russo, Mariateresa; Rastrelli, Luca

    2018-04-01

    This study reports a fast and automated analytical procedure based on an on-line SPE-HPLC-MS/MS method for the automatic pre-concentration, clean up and sensitive determination of OTA in wine. The amount of OTA contained in 100μL of sample (pH≅5.5) was retained and concentrated on an Oasis MAX SPE cartridge. After a washing step to remove matrix interferents, the analyte was eluted in back-flush mode and the eluent from the SPE column was diluted through a mixing Tee, using an aqueous solution before the chromatographic separation achieved on a monolithic column. The developed method has been validated according to EU regulation N. 519/2014 and applied for the analysis of 41 red and 17 white wines. The developed method features minimal sample handling, low solvent consumption, high sample throughput, low analysis cost and provides an accurate and highly selective results. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Magnetite nanoparticles coated with covalently immobilized ionic liquids as a sorbent for extraction of non-steroidal anti-inflammatory drugs from biological fluids

    International Nuclear Information System (INIS)

    Amiri, Maryam; Yadollah, Yamini; Safari, Meysam; Asiabi, Hamid

    2016-01-01

    Magnetic core-shell nanoparticles (mag-NPs) of type SiO_2-Fe_3O_4 were covalently modified with the ionic liquid dimethyl octadecyl[3-(trimethoxysilyl propyl)]ammonium chloride. The NPs were characterized via FTIR and scanning electron microscopy and evaluated with respect to the extraction of the nonsteroidal anti-inflammatory drugs (NSAIDs) tolmetin, indometacin and naproxen from blood samples. Supercritical fluid extraction was used to eliminate matrix effects before extraction with the mag-NPs. The effects of pH value of sample solution, amount of adsorbent, times of adsorption and desorption, salt effect, type and volume of suitable solvent for desorption were optimized. Under optimum conditions, magnetic solid phase extraction (MSPE) resulted in limits of detection that range between 0.1 and 0.3 μg L"−"1. In case of supercritical fluid extraction along with magnetic solid phase extraction (SFE- MSPE), the LODs ranged from 0.2 to 0.3 mg kg"−"1. The analytical ranges for all of the NSAIDs varied within 0.2–15 mg kg"-"1 and 0.1–250 μg L"−"1 in the SFE-MSPE and MSPE methods, respectively. The relative standard deviations for the extraction of the NSAIDs from blood samples via SFE-MSPE are <10.2%. (author)

  12. 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.

  13. On-line nuclear orientation

    International Nuclear Information System (INIS)

    Krane, K.S.

    1990-01-01

    This grant has as its overall goal the pursuit of on-line nuclear orientation experiments for the purpose of eliciting details of nuclear structure from the decays of neutron-deficient nuclei, such as those produced by the Holifield Heavy-Ion Research Facility at Oak Ridge and extracted by the UNISOR Isotope Separator. This paper discusses: refrigerator development; the decay of 184 Au; the decay of 191 Hg to 191 Au; the decay of 189 Pt to 189 Ir; the decays of 109,111 Pd; the decay of 172 Er; and solid angle corrections

  14. 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...... polluted agricultural soil material (San Joaquin Soil-Baseline Trace Element Concentrations) with water-soluble Cr(VI) salts at different concentration levels. The potential of the μSI-BI-LOV set-up with renewable surfaces for flame-AAS determination of high levels of readily bioavailable chromate...

  15. A fast and sensitive method for the simultaneous analysis of a wide range of per- and polyfluoroalkyl substances in indoor dust using on-line solid phase extraction-ultrahigh performance liquid chromatography-time-of-flight-mass spectrometry.

    Science.gov (United States)

    Padilla-Sánchez, Juan Antonio; Haug, Line Småstuen

    2016-05-06

    A fast and sensitive method for simultaneous determination of 18 traditional and 6 alternative per- and polyfluoroalkyl substances (PFASs) using solid-liquid extraction (SLE), off-line clean-up using activated carbon and on-line solid phase extraction-ultrahigh performance liquid chromatography-time-of-flight-mass spectrometry (on-line SPE-UHPLC-TOF-MS) was developed. The extraction efficiency was studied and recoveries in range the 58-114% were obtained. Extraction and injection volumes were also optimized to 2mL and 400μL, respectively. The method was validated by spiking dust from a vacuum cleaner bag that had been found to contain low levels of the PFASs in focus. Low method detection limits (MDLs) and method quantification limits (MQLs) in the range 0.008-0.846ngg(-1) and 0.027-2.820ngg(-1) were obtained, respectively. For most of the PFASs, the accuracies were between 70 and 125% in the range from 2 to100ngg(-1) dust. Intra-day and inter-day precisions were in general well below 30%. Analysis of a Standard Reference Material (SRM 2585) showed high accordance with results obtained by other laboratories. Finally, the method was applied to seven indoor dust samples, and PFAS concentrations in the range 0.02-132ngg(-1) were found. The highest median concentrations were observed for some of the alternative PFASs, such as 6:2-diPAP (25ngg(-1)), 8:2-diPAP (49ngg(-1)), and PFOPA (23ngg(-1)), illustrating the importance of inclusion of new PFASs in the analytical methods. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. 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.

  17. Extraction of Some Divalent Metal Ions (Cadmium, Nickel and Lead from Different Tea and Rice Samples Using Ghezeljeh Nanoclay (Geleh-Sar-Shoor as a New Natural Sorbent

    Directory of Open Access Journals (Sweden)

    Zahra Hassanzadeh Siahpoosh

    2016-12-01

    Full Text Available This article presents the method of extraction-preconcentration of Lead, Cadmium, and Nickel ions from food samples using the Ghezeljeh montmorillonite nanoclay (Geleh-Sar-Shoor as a new native adsorbent in batch single component systems. The extraction-preconcentration of heavy metals were carried out by applying the solid phase extraction (SPE method followed by atomic absorption spectroscopy (AAS, and inductively coupled with plasma atomic emission spectroscopy (ICP-AES. The Ghezeljeh nanoclay was characterized by using Fourier transform infrared spectroscopy (FT-IR, Scanning electron microscopy-energy dispersive spectrometer operating (SEM-EDS, X-ray diffractometry (XRD, X-ray fluorescence (XRF, Cation Exchange Capacity (CEC measurements, BET specific surface area and Zeta potential. According to BET theory, the specific surface areas of the Ghezeljeh nanoclay was calculated to be 19.8 m2 g-1 whereas the cation exchange capacity was measured to be 150 meq/100 g. The results of XRD, XRF, FT-IR, Zeta potential and BET surface area of the nanoclay confirmed that montmorillonite was the dominant mineral phase. Based on SEM images of this clay, it can be seen that the distance between the plates is nm level. For all three ions, the detection and quantification limits, dynamic linear range, preconcentration factor, and adsorption capacity were obtained. The effect of various interfering ions was studied. The experimental method was successfully applied for the extraction of heavy metals in different tea and rice samples.

  18. 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.

  19. 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

    International Nuclear Information System (INIS)

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

    2009-01-01

    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 1.0 mol L -1 HNO 3 was used as eluent. The metal ions in 300 mL solution can be concentrated to 1.0 mL, representing an enrichment factor of 300 was achieved. The recoveries of analytes at pH 8.0 with 1.0 g 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 1.4 ng L -1 for Cr(III), 1.0 ng L -1 for Ni(II), 0.85 ng L -1 for Ag(I), 1.2 ng L -1 for Co(II), 1.0 ng L -1 for Cu(II), 1.2 ng L -1 for Cd(II) and 1.3 ng L -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)

  20. 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.

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

  2. Facile green synthesis of graphene-Au nanorod nanoassembly for on-line extraction and sensitive stripping analysis of methyl parathion

    International Nuclear Information System (INIS)

    Zhu, Wenxin; Liu, Wei; Li, Tianbao; Yue, Xiaoyue; Liu, Tao; Zhang, Wentao; Yu, Shaoxuan; Zhang, Daohong; Wang, Jianlong

    2014-01-01

    Graphical abstract: Schematic illustration for the facile green fabrication of GN-AuNRs/GCE and its application for the extraction and electroanalysis of MP. - Highlights: • This paper described a facile green electrochemical approach to synthesize graphene-AuNRs nanocomposite. • The as-synthesized sensor shows low LOD and wide linear concentration range towards MP. • The sensor can be well used for the determination of MP in water and kiwi fruits samples. • This paper further enlarges the scope of facile green synthetic methods of GN-based hybrids. - Abstract: This paper described a facile green electrochemical approach to synthesize graphene-AuNRs nanocomposite (GN-AuNRs) onto glassy carbon electrode (GCE) for electrocatalytic analysis of methyl parathion (MP). This electrochemical synthesis of GN-AuNRs hybrid is environmentally friendly for not involving the chemical reduction of graphene oxide (GO) and facile for just on the basis of electrostatic interaction between GO and AuNRs, as well as electrochemical reduction of GO-AuNRs to GN-AuNRs. Combined the high conductivity, large surface area, good adsorption capacity towards aromatic rings and high catalytic ability of graphene with the excellent electronic properties and adsorption capacity of AuNRs, the high sensitive methyl parathion sensor was fabricated with the GN-AuNRs nanocomposite. The limit of detection (LOD) of the proposed sensor was calculated to be 0.82 ng/mL, which was lower than many previously reported enzyme or nonenzyme-based sensors. In the meantime, the linear detection range of this sensor was from 10 to 500 ng/mL and 750 to 4000 ng/mL, which was also wider than many other enzyme or enzymeless sensors. Furthermore, the facile and green electrochemical reduction strategy provided here could also be used to construct more GN-based hybrids. And the GN-based hybrid might be a new and highly efficient SPE factor, which opens new opportunities for green, facile and sensitive analysis of

  3. Development and validation of a rapid HPLC method for the determination of cefdinir in beagle dog plasma integrated with an automatic on-line solid-phase extraction following protein precipitation in the 96-well plate format.

    Science.gov (United States)

    Li, Ji; Wang, Li; Chen, Zhao; Xie, Rui; Li, You; Hang, Taijun; Fan, Guorong

    2012-05-01

    The high-performance liquid chromatography (HPLC) coupled with on-line solid phase extraction (SPE) and ultraviolet (UV) detection was developed for determining cefdinir in beagle dog plasma. After simple pretreatment for plasma with 6% perchloric acid, a volume of 100 μL upper layer of the plasma sample was injected into the self-made on-line SPE column. The analytes were retained on the trap column (Lichrospher C(18), 4.6 mm × 37 mm, 25 μm), and the biological matrix was washed out with the solvent (20mM KH(2)PO(4) adjusted pH 3.0) at flow rate of 2 mL/min. By rotation of the switching valve, the target analytes could be eluted from trap column to analytical column in the back-flush mode by the mobile phase (methanol-acetonitrile-20mM KH(2)PO(4) adjusted pH 3.0, 11.25:6.75:82, v/v/v) at flow rate of 1.5 mL/min, and then separated on the analytical column (Ultimate XB-C(18), 4.6 mm × 50 mm, 5 μm). The complete cycle of the on-line SPE preconcentration, purification and HPLC separation of the analytes was 4 min. The UV detection was performed at 286 nm. The calibration curves showed excellent linear relationship (R(2)=0.9995) over the concentration range of 0.05-50 μg/mL. The optimized method showed good performance in terms of specificity, linearity, detection and quantification limits, precision and accuracy. This method was successfully applied to quantify cefdinir in beagle dog plasma to support the pre-clinical pharmacokinetic trial. Copyright © 2012. Published by Elsevier B.V.

  4. Electrospun UiO-66/polyacrylonitrile nanofibers as efficient sorbent for pipette tip solid phase extraction of phytohormones in vegetable samples.

    Science.gov (United States)

    Yan, Zhiming; Wu, Mei; Hu, Biqing; Yao, Minna; Zhang, Lan; Lu, Qiaomei; Pang, Jie

    2018-03-23

    In this work, metal-organic framework particles incorporated fibers (UiO-66/PAN nanofibers) were used as adsorbent in pipette tip solid phase extraction (PT-SPE) for the first time. The UiO-66/PAN nanofibers were fabricated by a facile electrospinning method and characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction and nitrogen adsorption-desorption experiments. The UiO-66/PAN nanofibers were applied to assemble a novel PT-SPE cartridge for determination of four phytohormones followed by high performance liquid chromatography (HPLC). Several experimental parameters such as kinds of UiO-66/PAN nanofibers, the amount of UiO-66/PAN nanofibers, the effect of solution pH, ionic strength and desorption conditions were intensively investigated. Under the optimal conditions, the linear ranges of the phytohormones were in the range of 0.06-60 ng/mL with correlation coefficients above 0.992. The limits of detection were between 0.01 ng/mL to 0.02 ng/mL. The interday and intraday precision (RSD) for three replicate extractions of the four phytohormones (15 ng/mL for each) was in the range of 1.5-5.6%. The established method was successfully applied for the determination of phytohormones in watermelon and mung bean sprouts samples. The results showed that the electrostatic interaction between the positively charged UiO-66 and anionic forms of phytohormones played an important role in the extraction of the phytohormones. Copyright © 2018 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

    Altun, Zeki; Abdel-Rehim, Mohamed

    2008-01-01

    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 μL) 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 μL 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 μL elution solution and then with 3 x 250 μL 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

  6. 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.

  7. Magnetic solid-phase extraction of non-steroidal anti-inflammatory drugs from environmental water samples using polyamidoamine dendrimer functionalized with magnetite nanoparticles as a sorbent.

    Science.gov (United States)

    Alinezhad, Heshmatollah; Amiri, Amirhassan; Tarahomi, Mehrasa; Maleki, Behrooz

    2018-06-01

    A novel polyamidoamine dendrimer functionalized with Fe 3 O 4 nanoparticles (Fe 3 O 4 @PAMAM) had been fabricated and used as magnetic solid-phase extraction (MSPE) adsorbent. The Fe 3 O 4 @PAMAM nanocomposites were characterized by X-ray powder diffraction, Fourier transform infrared spectroscopy, field-emission scanning electron spectroscopy, elemental analytical, and thermal gravimetric analysis. The MSPE method coupled with high-performance liquid chromatography with an ultraviolet detection system was applied for the separation/analysis of non-steroidal anti-inflammatory drugs (NSAIDs). Major parameters affecting the extraction efficiency of the selected drugs were optimized. Under optimal conditions, the enrichment factors for the proposed method were 701835. The linear range, limit of detection, correlation coefficient (r), and relative standard deviation (RSD) were found to be 0.15-500 ng mL -1 , 0.050.08 ng mL -1 , 0.99320.9967, and 4.5-7.0% (n = 5, 0.2, 10 and 300 ng mL -1 ), respectively. The method was successfully applied to the determination of NSAIDs in the real water samples. The recoveries of spiked water samples were in the range of 93.6-98.9% with RSDs varying from 6.1% to 9.0%, showing the good accuracy of the method. Copyright © 2018 Elsevier B.V. All rights reserved.

  8. Core-shell Fe3O4 polydopamine nanoparticles as sorbent for magnetic dispersive solid-phase extraction of copper from food samples.

    Science.gov (United States)

    Yavuz, Emre; Tokalıoğlu, Şerife; Patat, Şaban

    2018-10-15

    In the present study, core-shell Fe 3 O 4 polydopamine nanoparticles were synthesized and used for the first time as an adsorbent for the vortex assisted magnetic dispersive solid phase extraction of copper from food samples. After elution, copper in the solutions was determined by FAAS. The adsorbent was characterized using X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller surface area, and zeta potential measurements. Various parameters affecting the magnetic dispersive solid-phase extraction were evaluated. The optimum pH and magnetic adsorbent amount were found to be 5 and 40 mg, respectively. Elution was made by 3 mL of 2 mol L -1 HNO 3 .The major advantage of the method is the fast equilibration during adsorption without the need for vortexing or shaking. The preconcentration factor and detection limit of the method were found to be 150 and 0.22 mg L -1 , respectively. The precision (as RSD%) and adsorption capacity of the method were 3.7% and 28 mg g -1 , respectively. The method was successfully verified by analyzing four certified reference materials (SPS-WW1 Batch 114 Wastewater, TMDA-53.3 Lake water, BCR-482 Lichen and 1573a Tomato Leaves) and by addition/recovery tests of copper standard solution in organic baby food, muesli, macaroni, honey, and milk samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

  9. Measurement of trace levels of antibiotics in river water using on-line enrichment and triple-quadrupole LC-MS/MS.

    Science.gov (United States)

    Dinh, Quoc Tuc; Alliot, Fabrice; Moreau-Guigon, Elodie; Eurin, Joëlle; Chevreuil, Marc; Labadie, Pierre

    2011-09-15

    This study presents the development of an automated on-line solid phase extraction (SPE)-liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of 23 antibiotics in environmental water samples. After optimisation of LC-MS/MS conditions, SPE parameters such as sorbent type, sample pH or sample volume were optimised. Antibiotic recoveries ranged from 64% to 98% and compared favourably with those achieved using off-line SPE. Limits of detection were in the range 0.5-13.7 ng L(-1). This on-line SPE-LC-MS/MS procedure was applied to the analysis of water samples taken in three rivers within the Seine River basin, near Paris (France). The obtained results revealed the occurrence of 12 antibiotics, including tylosin, erythromycin, tetracycline, amoxicillin, trimethoprim, sulfamethoxazole, oxolinic acid, flumequine, norfloxacin, ciprofloxacin, ofloxacin, and vancomycin (2-1435 ng L(-1)). Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Solid-phase extraction of polar pesticides from environmental water samples on graphitized carbon and Empore-activated carbon disks and on-line coupling to octadecyl-bonded silica analytical columns.

    Science.gov (United States)

    Slobodník, J; Oztezkizan, O; Lingeman, H; Brinkman, U A

    1996-10-25

    The suitability of Empore-activated carbon disks (EACD), Envi-Carb graphitized carbon black (GCB) and CPP-50 graphitized carbon for the trace enrichment of polar pesticides from water samples was studied by means of off-line and on-line solid-phase extraction (SPE). In the off-line procedure, 0.5-2 l samples spiked with a test mixture of oxamyl, methomyl and aldicarb sulfoxide were enriched on EnviCarb SPE cartridges or 47 mm diameter EACD and eluted with dichloromethane-methanol. After evaporation, a sample was injected onto a C18-bonded silica column and analysed by liquid chromatography with ultraviolet (LC-UV) detection. EACD performed better than EnviCarb cartridges in terms of breakthrough volumes (> 2 l for all test analytes), reproducibility (R.S.D. of recoveries, 4-8%, n = 3) and sampling speed (100 ml/min); detection limits in drinking water were 0.05-0.16 microgram/l. In the on-line experiments, 4.6 mm diameter pieces cut from original EACD and stacked onto each other in a 9 mm long precolumn, and EnviCarb and CPP-50 packed in 10 x 2.0 mm I.D. precolumn, were tested, and 50-200 ml spiked water samples were preconcentrated. Because of the peak broadening caused by the strong sorption of the analytes on carbon, the carbon-packed precolumns were eluted by a separate stream of 0.1 ml/min acetonitrile which was mixed with the gradient LC eluent in front of the C18 analytical column. The final on-line procedure was also applied for the less polar propoxur, carbaryl and methiocarb. EnviCarb could not be used due to its poor pressure resistance. CPP-50 provided less peak broadening than EACD: peak widths were 0.1-0.3 min and R.S.D. of peak heights 4-14% (n = 3). In terms of analyte trapping efficiency on-line SPE-LC-UV with a CPP-50 precolumn also showed better performance than when Bondesil C18/OH or polymeric PLRP-S was used, but chromatographic resolution was similar. With the CPP-50-based system, detection limits of the test compounds were 0.05-1 microgram

  11. Affinity extraction of emerging contaminants from water based on bovine serum albumin as a binding agent.

    Science.gov (United States)

    Papastavros, Efthimia; Remmers, Rachael A; Snow, Daniel D; Cassada, David A; Hage, David S

    2018-03-01

    Affinity sorbents using bovine serum albumin as a binding agent were developed and tested for the extraction of environmental contaminants from water. Computer simulations based on a countercurrent distribution model were also used to study the behavior of these sorbents. Several model drugs, pesticides, and hormones of interest as emerging contaminants were considered in this work, with carbamazepine being used as a representative analyte when coupling the albumin column on-line with liquid chromatography and tandem mass spectrometry. The albumin column was found to be capable of extracting carbamazepine from aqueous solutions that contained trace levels of this analyte. Further studies of the bovine serum albumin sorbent indicated that it had higher retention under aqueous conditions than a traditional C 18 support for most of the tested emerging contaminants. Potential advantages of using these protein-based sorbents included the low cost of bovine serum albumin and its ability to bind to a relatively wide range of drugs and related compounds. It was also shown how simulations could be used to describe the elution behavior of the model compounds on the bovine serum albumin sorbents as an aid in optimizing the retention and selectivity of these supports for use with liquid chromatography or methods such as liquid chromatography with tandem mass spectrometry. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. 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. Copyright © 2010. Published by Elsevier B.V.

  13. 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. Copyright © 2012 Elsevier Ltd. All rights reserved.

  14. Modified carbon nanotubes as a sorbent for solid-phase extraction of gold, and its determination by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Moghaddam, Firouzeh Hassani; Behzadi, Mansoureh; Naghizadeh, Matin; Taher, Mohammad Ali

    2015-01-01

    A simple, sensitive and accurate method was developed for solid-phase extraction and preconcentration of trace levels of gold in various samples. It is based on the adsorption of gold on modified oxidized multi-walled carbon nanotubes prior to its determination by graphite furnace atomic absorption spectrometry. The type and volume of eluent solution, sample pH value, flow rates of sample and eluent, sorption capacity and breakthrough volume were optimized. Under these conditions, the method showed linearity in the range of 0.2–6.0 ng L −1 with coefficients of determination of >0.99 in the sample. The relative standard deviation for seven replicate determinations of gold (at a level of 0.6 ng L −1 ) is ±3.8 %, the detection limit is 31 pg L −1 (in the initial solution and at an S/N ratio of 3; for n = 8), and the enrichment factor is 200. The sorption capacity of the modified MWCNTs for gold(III) is 4.15 mg g −1 . The procedure was successfully applied to the determination of gold in (spiked) water samples, human hair, human urine and standard reference material with recoveries ranging from 97.0 to 104.2 %. (author)

  15. Use of on-line supercritical fluid extraction-supercritical fluid chromatography/tandem mass spectrometry to analyze disease biomarkers in dried serum spots compared with serum analysis using liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Suzuki, Makoto; Nishiumi, Shin; Kobayashi, Takashi; Sakai, Arata; Iwata, Yosuke; Uchikata, Takato; Izumi, Yoshihiro; Azuma, Takeshi; Bamba, Takeshi; Yoshida, Masaru

    2017-05-30

    The analytical stability and throughput of biomarker assays based on dried serum spots (DSS) are strongly dependent on the extraction process and determination method. In the present study, an on-line system based on supercritical fluid extraction-supercritical fluid chromatography coupled with tandem mass spectrometry (SFE-SFC/MS/MS) was established for analyzing the levels of disease biomarkers in DSS. The chromatographic conditions were investigated using the ODS-EP, diol, and SIL-100A columns. Then, we optimized the SFE-SFC/MS/MS method using the diol column, focusing on candidate biomarkers of oral, colorectal, and pancreatic cancer that were identified using liquid chromatography (LC)/MS/MS. By using this system, four hydrophilic metabolites and 17 hydrophobic metabolites were simultaneously detected within 15 min. In an experiment involving clinical samples, PC 16:0-18:2/16:1-18:1 exhibited 93.8% sensitivity and 64.3% specificity, whereas PC 17:1-18:1/17:0-18:2 showed 81.3% sensitivity and 92.9% specificity for detecting oral cancer. In addition, assessments of the creatine levels demonstrated 92.3% sensitivity and 78.6% specificity for detecting colorectal cancer. The results of this study indicate that our method has great potential for clinical diagnosis and would be suitable for large-scale screening. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  16. A simple and highly sensitive on-line column extraction liquid chromatography-tandem mass spectrometry method for the determination of protein-unbound tacrolimus in human plasma samples.

    Science.gov (United States)

    Bittersohl, Heike; Schniedewind, Björn; Christians, Uwe; Luppa, Peter B

    2018-04-27

    Therapeutic drug monitoring (TDM) of the immunosuppressive drug tacrolimus is essential to avoid side effects and rejection of the allograft after transplantation. In the blood circulation, tacrolimus is largely located inside erythrocytes or bound to plasma proteins and less than 0.1% is protein-unbound (free). One basic principle of clinical pharmacology is that only free drug is pharmacologically active and monitoring this portion has the potential to better reflect the drug effect than conventional measurements of total tacrolimus in whole blood. To address this, a highly sensitive and straightforward on-line liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed, validated and applied to patient plasma samples. The sample preparation included ultracentrifugation and addition of the stable isotope labeled drug analogue D2,13C-tacrolimus, followed by on-line sample extraction and measurement using a Sciex QTRAP ® 6500 in the multiple reaction monitoring mode. Due to very low concentrations of protein-unbound tacrolimus, it was important to develop a highly sensitive, precise and accurate assay. Here, we first report the efficient formation of tacrolimus lithium adduct ions, which greatly increased assay sensitivity. A lower limit of quantification (LLOQ) of 1 pg/mL (10 fg on column) was achieved and the assay was linear between 1 and 200 pg/mL. There was no carry-over detected. The inaccuracy ranged from -9.8 to 7.4% and the greatest imprecision was 7.5%. The matrix factor was found to be smaller than 1.1%. In summary, this method represents a suitable tool to investigate the potential clinical value of free tacrolimus monitoring in organ transplant recipients. Copyright © 2018 Elsevier B.V. All rights reserved.

  17. Deep Bed Iodine Sorbent Testing FY 2011 Report

    International Nuclear Information System (INIS)

    Soelberg, Nick; Watson, Tony

    2011-01-01

    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

  18. Simultaneous multi-mycotoxin determination in nutmeg by ultrasound-assisted solid-liquid extraction and immunoaffinity column clean-up coupled with liquid chromatography and on-line post-column photochemical derivatization-fluorescence detection.

    Science.gov (United States)

    Kong, Wei-Jun; Liu, Shu-Yu; Qiu, Feng; Xiao, Xiao-He; Yang, Mei-Hua

    2013-05-07

    A simple and sensitive analytical method based on ultrasound-assisted solid-liquid extraction and immunoaffinity column clean-up coupled with high performance liquid chromatography and on-line post-column photochemical derivatization-fluorescence detection (USLE-IAC-HPLC-PCD-FLD) has been developed for simultaneous multi-mycotoxin determination of aflatoxins B1, B2, G1, G2 (AFB1, AFB2, AFG1, AFG2) and ochratoxin A (OTA) in 13 edible and medicinal nutmeg samples marketed in China. AFs and OTA were extracted from nutmeg samples by ultrasonication using a methanol : water (80 : 20, v/v) solution, followed by an IAC clean-up step. Different USL extraction conditions, pre-processing ways for nutmeg sample and clean-up columns for mycotoxins, as well as HPLC-PCD-FLD parameters (mobile phase, column temperature, elution procedure, excitation and emission wavelengths) were optimized. This method, which was appraised for analyzing nutmeg samples, showed satisfactory results with reference to limits of detection (LODs) (from 0.02 to 0.25 μg kg(-1)), limits of quantification (LOQs) (from 0.06 to 0.8 μg kg(-1)), linear ranges (up to 30 ng mL(-1) for AFB1, AFG1 and OTA and 9 ng mL(-1) for AFB2 and AFG2), intra- and inter-day variability (all application of developed method in nutmeg samples have elucidated that four samples were detected with contamination of AFs and one with OTA. AFB1 was the most frequently found mycotoxin in 30.8% of nutmeg samples at contamination levels of 0.73-16.31 μg kg(-1). At least two different mycotoxins were co-occurred in three samples, and three AFs were simultaneously detected in one sample.

  19. 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

  20. On-line filtering

    International Nuclear Information System (INIS)

    Verkerk, C.

    1978-01-01

    Present day electronic detectors used in high energy physics make it possible to obtain high event rates and it is likely that future experiments will face even higher data rates than at present. The complexity of the apparatus increases very rapidly with time and also the criteria for selecting desired events become more and more complex. So complex in fact that the fast trigger system cannot be designed to fully cope with it. The interesting events become thus contaminated with multitudes of uninteresting ones. To distinguish the 'good' events from the often overwhelming background of other events one has to resort to computing techniques. Normally this selection is made in the first part of the analysis of the events, analysis normally performed on a powerful scientific computer. This implies however that many uninteresting or background events have to be recorded during the experiment for subsequent analysis. A number of undesired consequences result; and these constitute a sufficient reason for trying to perform the selection at an earlier stage, in fact ideally before the events are recorded on magnetic tape. This early selection is called 'on-line filtering' and it is the topic of the present lectures. (Auth.)

  1. On line portal imaging

    International Nuclear Information System (INIS)

    Munro, Peter

    1997-01-01

    Purpose/Objective: The purpose of this presentation is to examine the various imaging devices that have been developed for portal imaging, describe some of the image registration methods that have been developed to determine geometric errors quantitatively, and discuss how portal imaging has been incorporated into clinical practice. Discussion: Verification of patient positioning has always been an important aspect of external beam radiation therapy. Over the past decade many portal imaging devices have been developed by individual investigators and most accelerator manufacturers now offer 'on-line' portal imaging systems. The commercial devices include T.V. camera-based systems, liquid ionisation chamber systems, and shortly, flat panel systems. The characteristics of these imaging systems will be discussed. In addition, other approaches such as the use of kilovoltage x-ray sources, video monitoring, and ultrasound have been proposed for improving patient positioning. Some of the advantages of these approaches will be discussed. One of the major advantages of on-line portal imaging is that many quantitative techniques have been developed to detect errors in patient positioning. The general approach is to register anatomic structures on a portal image with the same structures on a digitized simulator film. Once the anatomic structures have been registered, any discrepancies in the position of the patient can be identified. One problem is finding a common frame of reference for the simulator and portal images, since the location of the radiation field within the pixel matrix may differ for the two images. As a result, a common frame of reference has to be established before the anatomic structures in the images can be registered - generally by registering radiation field edges identified in the simulator and portal images. In addition, distortions in patient geometry or rotations out of the image plane can confound the image registration techniques. Despite the

  2. On line portal imaging

    International Nuclear Information System (INIS)

    Munro, Peter

    1996-01-01

    Purpose/Objective: The purpose of this presentation is to examine the various imaging devices that have been developed for portal imaging; describe some of the image registration methods that have been developed to determine geometric errors quantitatively; discuss some of the ways that portal imaging has been incorporated into routine clinical practice; describe quality assurance procedures for these devices, and discuss the use of portal imaging devices for dosimetry applications. Discussion: Verification of patient positioning has always been an important aspect of external beam radiation therapy. Over the past decade many portal imaging devices have been developed by individual investigators and most accelerator manufacturers now offer 'on-line' portal imaging systems. The commercial devices can be classified into three categories: T.V. camera-based systems, liquid ionisation chamber systems, and amorphous silicon systems. Many factors influence the quality of images generated by these portal imaging systems. These include factors which are unavoidable (e.g., low subject contrast), factors which depend upon the individual imaging device forming the image (e.g., dose utilisation, spatial resolution) as well as factors which depend upon the characteristics of the linear accelerator irradiating the imaging system (x-ray source size, image magnification). The characteristics of individual imaging systems, such as spatial resolution, temporal response, and quantum utilisation will be discussed. One of the major advantages of on-line portal imaging is that many quantitative techniques have been developed to detect errors in patient positioning. The general approach is to register anatomic structures on a portal image with the same structures on a digitized simulator film. Once the anatomic structures have been registered, any discrepancies in the position of the patient can be identified. However, the task is not nearly as straight-forward as it sounds. One problem

  3. 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.

  4. 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

  5. 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.

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

  7. The study of sorption of cesium radionuclides by 'T-55' ferrocyanide sorbent from various types of liquid radioactive wastes

    International Nuclear Information System (INIS)

    Semenischev, V.S.; Voronina, A.V.; Bykov, A.A.

    2013-01-01

    The sorption of caesium by T-55 sorbent from different types of liquid radioactive wastes is studied. It is shown that the sorbent can be used for extraction of cesium from high level acidic and saline solutions and also for decontamination of caesium contaminated waters containing surfactants and EDTA. (author)

  8. On line portal imaging

    International Nuclear Information System (INIS)

    Munro, Peter

    1995-01-01

    Purpose/Objective: The purpose of this presentation is to review the physics of imaging with high energy x-ray beams; examine the various imaging devices that have been developed for portal imaging; describe some of the image registration methods that have been developed to determine errors in patient positioning quantitatively; and discuss some of the ways that portal imaging has been incorporated into routine clinical practice. Verification of patient positioning has always been an important aspect of external beam radiation therapy. Checks of patient positioning have generally been done with film, however, film suffers from a number of drawbacks, such as poor image display and delays due to film development. Over the past decade many portal imaging devices have been developed by individual investigators and most accelerator manufacturers now offer 'on-line' portal imaging systems, which are intended to overcome the limitations of portal films. The commercial devices can be classified into three categories: T.V. camera-based systems, liquid ionisation chamber systems, and amorphous silicon systems. Many factors influence the quality of images generated by these portal imaging systems. These include factors which are unavoidable (e.g., low subject contrast), factors which depend upon the individual imaging device forming the image (e.g., dose utilisation, spatial resolution) as well as factors which depend upon the characteristics of the linear accelerator irradiating the imaging system (x-ray source size, image magnification). The fundamental factors which limit image quality and the characteristics of individual imaging systems, such as spatial resolution, temporal response, and quantum utilisation will be discussed. One of the major advantages of on-line portal imaging is that many quantitative techniques have been developed to detect errors in patient positioning. The general approach is to register anatomic structures on a portal image with the same

  9. Release of iodine radionuclides from gas media in a system of selective block sorbents

    International Nuclear Information System (INIS)

    Moskvin, L.N.; Miroshnikov, V.S.; Mel'nikov, V.A.; Chetverikov, V.V.

    1979-01-01

    A scheme of extracting iodine radionuclides from gas flows in a system of selective sorbents has been developed. The method provides separation of three forms of iodine: the aerosol component, the elementary iodine and organic-iodine compounds. Aerosols are trapped by a mechanical filter made of porous polytetrafluoroethylene with pores of no more than 1 μm. Silver-based sorbents for the elementary iodine are made by sintering the granular polytetrafluoroethylene (the size of granules is 0.1-0.5 mm) with of finely dispersed solver (5% mass). Organic iodine compounds are extracted by a silica sorbent impregnated with silver nitrate. The efficiency of sorbents was tested in gas flows with a known content of 131 I in the form of elementary iodine and methyl iodide. The results of experiments show that the efficiency of sorption of elementary iodine by a metallic-silver sorbent and of methyl iodide by a SiO 2 /AgNO 3 sorbent constitutes no less than 99% at a flow rate of up to 200 l/h. The iodine has been extracted at a flow rate of 100 l/h during 100 hours and for that time the efficiency of the iodine sorbtion has not changed. The suggested variant of extracting iodine radionuclides from gaseous media can be used both for fast control of iodine content in gas blowoffs and for researches aimed at studying the distribution of iodine forms in steam-and-gas media depending on nuclear plant operating conditions

  10. 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

  11. High capacity carbon dioxide sorbent

    Science.gov (United States)

    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.

  12. Decontamination formulation with sorbent additive

    Science.gov (United States)

    Tucker; Mark D. , Comstock; Robert H.

    2007-10-16

    A decontamination formulation and method of making that neutralizes the adverse health effects of both chemical and biological compounds, especially chemical warfare (CW) and biological warfare (BW) agents, and toxic industrial chemicals. The formulation provides solubilizing compounds that serve to effectively render the chemical and biological compounds, particularly CW and BW compounds, susceptible to attack, and at least one reactive compound that serves to attack (and detoxify or kill) the compound. The formulation includes at least one solubilizing agent, a reactive compound, a bleaching activator, a sorbent additive, and water. The highly adsorbent, water-soluble sorbent additive (e.g., sorbitol or mannitol) is used to "dry out" one or more liquid ingredients, such as the liquid bleaching activator (e.g., propylene glycol diacetate or glycerol diacetate) and convert the activator into a dry, free-flowing powder that has an extended shelf life, and is more convenient to handle and mix in the field.

  13. Ionic liquids: solvents and sorbents in sample preparation.

    Science.gov (United States)

    Clark, Kevin D; Emaus, Miranda N; Varona, Marcelino; Bowers, Ashley N; Anderson, Jared L

    2018-01-01

    The applications of ionic liquids (ILs) and IL-derived sorbents are rapidly expanding. By careful selection of the cation and anion components, the physicochemical properties of ILs can be altered to meet the requirements of specific applications. Reports of IL solvents possessing high selectivity for specific analytes are numerous and continue to motivate the development of new IL-based sample preparation methods that are faster, more selective, and environmentally benign compared to conventional organic solvents. The advantages of ILs have also been exploited in solid/polymer formats in which ordinarily nonspecific sorbents are functionalized with IL moieties in order to impart selectivity for an analyte or analyte class. Furthermore, new ILs that incorporate a paramagnetic component into the IL structure, known as magnetic ionic liquids (MILs), have emerged as useful solvents for bioanalytical applications. In this rapidly changing field, this Review focuses on the applications of ILs and IL-based sorbents in sample preparation with a special emphasis on liquid phase extraction techniques using ILs and MILs, IL-based solid-phase extraction, ILs in mass spectrometry, and biological applications. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Inorganic sorbents for radiostrontium removal from waste solutions: selectivity and role of calixarenes

    International Nuclear Information System (INIS)

    Vijayan, S.; Belikov, K.; Drapailo, A.

    2011-01-01

    The challenge in the remediation of 90 Sr-contaminated waters arises from the need to achieve very high removal efficiencies to meet discharge targets from waste effluents containing relatively high concentrations of non-radioactive cations. Low-cost natural zeolites are not selective for strontium over other divalent cations, notably such ions as calcium; and produce low 90 Sr removal performance, and large volumes of spent sorbent waste. The synthesis and use of selective, synthetic inorganic sorbents could prove to be a feasible approach for high 90 Sr removal efficiencies, and much smaller volumes of secondary solid waste generation. The essential advantages of inorganic sorbents include their stability and resistance to radiation, and the potential for producing stable waste forms such as vitrified glass or ceramics for disposal. However, the cost of strontium-specific sorbents is prohibitive for large-scale applications at present. This paper is a review of the reported information on removal mechanisms and performance of Sr-specific inorganic sorbents. The analysis has revealed promising performance, efficiency and selectivity for strontium removal from solutions containing low and high concentrations of salts. The leading sorbents are crystalline silicotitanate and oxides of metals such as titanium. An initial assessment has also been made of the performance of calixarene-based macrocyclic compounds. These are known for their selectivity for strontium in solvent extraction processes. From the initial strontium removal results in bench-scale tests using different solid substrates, impregnated with calixarene derivatives, only sodium-mordenite impregnated with calyx[8]arene octamide gave an overall strontium removal efficiency in the range of 90 to 95% in the presence of 3.5 ppm calcium. There was no improvement observed for strontium-removal efficiency or selectivity over calcium in the calixarene-impregnated inorganic sorbent matrix. In several tests, the

  15. Sorbent Nanotechnologies for Water Cleaning

    Science.gov (United States)

    Ahmed, Snober

    Despite decades of regulatory efforts to mitigate water pollution, many chemicals, particularly heavy metals, still present risks to human health. In addition to direct exposure, certain metals such as mercury threaten public health due to its persistence, bioaccumulation and bioamplification throughout the food chain. A number of U.S. Federal and State regulations have been established to reduce the levels of mercury in water. Activated carbon (AC) has been widely explored for the removal of mercury. However, AC suffers from many limitations inherent to its chemical properties, and it becomes increasingly challenging to meet current and future regulations by simply modifying AC to enhance its performance. Recently, the performance of nanosorbents have been studied in order to removal pollutants. Nanosorbents utilize the ultra-high reactive surface of nanoparticles for rapid, effective and even permanent sequestration of heavy metals from water and air, thus showed promising results as compared to AC. The goal of this thesis research is to develop nanomaterial-based sorbents for the removal of mercury from water. It describes the development of a new solid-support assisted growth of selenium nanoparticles, their use for water remediation, and the development of a new nanoselenium-based sorbent sponge for fast and efficient mercury removal. The nanoselenium sorbent not only shows irreversible interaction with mercury but also exhibits remarkable properties by overcoming the limitations of AC. The nanoselenium sponge was shown to remove mercury to undetectable levels within one minute. This new sponge technology would have an impact on inspiring new stringent regulations and lowering costs to help industries meet regulatory requirements, which will ultimately help improve air and water quality, aquatic life and public health.

  16. 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.

  17. 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

  18. Sol-gel niobia sorbent with a positively charged octadecyl ligand providing enhanced enrichment of nucleotides and organophosphorus pesticides in capillary microextraction for online HPLC analysis.

    Science.gov (United States)

    Kesani, Sheshanka; Malik, Abdul

    2018-04-01

    A niobia-based sol-gel organic-inorganic hybrid sorbent carrying a positively charged C 18 ligand (Nb 2 O 5 -C 18 (+ve)) was synthesized to achieve enhanced enrichment capability in capillary microextraction of organophosphorus compounds (which include organophosphorus pesticides and nucleotides) before their online analysis by high-performance liquid chromatography. The sorbent was designed to simultaneously provide three different types of molecular level interactions: electrostatic, Lewis acid-base, and van der Waals interactions. To understand relative contributions of various molecular level analyte-sorbent interactions in the extraction process, two other sol-gel niobia sorbents were also created: (a) a purely inorganic sol-gel niobia sorbent (Nb 2 O 5 ) and (b) an organic-inorganic hybrid sol-gel niobia sorbent carrying an electrically neutral-bonded octadecyl ligand (Nb 2 O 5 -C 18 ). The extraction efficiency of the created sol-gel niobia sorbent (Nb 2 O 5 -C 18 (+ve)) was compared with that of analogously designed and synthesized titania-based sol-gel sorbent (TiO 2 -C 18 (+ve)), taking into consideration that titania-based sorbents present state-of-the-art extraction media for organophosphorus compounds. In capillary microextraction with high-performance liquid chromatography analysis, Nb 2 O 5 -C 18 (+ve) had shown 40-50% higher specific extraction values (a measure of extraction efficiency) over that of TiO 2 -C 18 (+ve). Compared to TiO 2 -C 18 (+ve), Nb 2 O 5 -C 18 (+ve) also provided superior analyte desorption efficiency (96 vs. 90%) during the online release of the extracted organophosphorus pesticides from the sorbent coating in the capillary microextraction capillary to the chromatographic column using reversed-phase high-performance liquid chromatography mobile phase. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. 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...

  20. Recovery of Lithium from Geothermal Brine with Lithium-Aluminum Layered Double Hydroxide Chloride Sorbents.

    Science.gov (United States)

    Paranthaman, Mariappan Parans; Li, Ling; Luo, Jiaqi; Hoke, Thomas; Ucar, Huseyin; Moyer, Bruce A; Harrison, Stephen

    2017-11-21

    We report a three-stage bench-scale column extraction process to selectively extract lithium chloride from geothermal brine. The goal of this research is to develop materials and processing technologies to improve the economics of lithium extraction and production from naturally occurring geothermal and other brines for energy storage applications. A novel sorbent, lithium aluminum layered double hydroxide chloride (LDH), is synthesized and characterized with X-ray powder diffraction, scanning electron microscopy, inductively coupled plasma optical emission spectrometry (ICP-OES), and thermogravimetric analysis. Each cycle of the column extraction process consists of three steps: (1) loading the sorbent with lithium chloride from brine; (2) intermediate washing to remove unwanted ions; (3) final washing for unloading the lithium chloride ions. Our experimental analysis of eluate vs feed concentrations of Li and competing ions demonstrates that our optimized sorbents can achieve a recovery efficiency of ∼91% and possess excellent Li apparent selectivity of 47.8 compared to Na ions and 212 compared to K ions, respectively in the brine. The present work demonstrates that LDH is an effective sorbent for selective extraction of lithium from brines, thus offering the possibility of effective application of lithium salts in lithium-ion batteries leading to a fundamental shift in the lithium supply chain.

  1. Sorbents for the oxidation and removal of mercur

    Science.gov (United States)

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

    2017-09-12

    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.

  2. Sorbents for the oxidation and removal of mercury

    Science.gov (United States)

    Olson, Edwin S [Grand Forks, ND; Holmes, Michael J [Thompson, ND; Pavlish, John H [East Grand Forks, MN

    2008-10-14

    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.

  3. Sorbents for the oxidation and removal of mercury

    Science.gov (United States)

    Olson, Edwin S [Grand Forks, ND; Holmes, Michael J [Thompson, ND; Pavlish, John H [East Grand Forks, MN

    2012-05-01

    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.

  4. 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.

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

    Science.gov (United States)

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

    2018-04-01

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

  6. On line ultrasonic integrated backscatter

    International Nuclear Information System (INIS)

    Landini, L.; Picano, E.; Mazzarisi, A.; Santarelli, F.; Benassi, A.; De Pieri, G.

    1988-01-01

    A new equipment for on-line evaluation of index based on two-dimensional integrated backscatter from ultrasonic images is described. The new equipment is fully integrated into a B-mode ultrasonic apparatus which provides a simultaneous display of conventional information together with parameters of tissue characterization. The system has been tested with a backscattering model of microbubbles in polysaccharide solution, characterized by a physiological exponential time decay. An exponential fitting to the experimental data was performed which yielded r=0.95

  7. Low-Cost Sorbents: A Literature Summary

    National Research Council Canada - National Science Library

    Bailey, Susan

    1997-01-01

    The capital and regeneration costs of activated carbon and ion exchange media suggest that better process economics may be achieved with disposable sorbents for the treatment of metals-contaminated...

  8. Development of a system for simultaneous - sequential determinations of major and minor actinides (Th, Np, U, Pu, Am, Cm) by on-line extraction chromatography - ion concentration - inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Trivellone, E.; Mariani, M.; Carlos-Marquez, R.; Aldave de las Heras, L.; Betti, M.; )

    2009-01-01

    Full text: Because of the great complexity and time consuming of traditional methods for actinides determination, a procedure for their simultaneous and sequential separation and quantification was developed. A complete circuit constituted by three analytical chromatographic columns packed with TEVA, UTEVA and TRU resins (Eichrom Inc) for retention of tetra-, hexa- and tri-valent actinides and three cation concentrator columns TCC-II (from Dionex Corporation) connected by six (4-way and 6-way) valves is coupled on-line to an ICPMS detector. The use of TCC-II columns just prior of the ICPMS determination allows to improve sensitivity and detection limits down to the ng/l level. The use of a coupled HPLC to an ICPMS system enables the complete analysis of all the six actinides in almost 2 hours. (author)

  9. Preparation and investigation of ion exchange properties of sorbent based on activated carbon BAU and zirconium hydroxide

    International Nuclear Information System (INIS)

    Blokhin, A.A.; Semenov, M.I.; Taushkanov, V.P.; Andronov, E.A.

    1978-01-01

    The method of obtaining the sorbent based on the activated carbon and zirconium hydroxide, performed by carbon soaking by zirconium salt solution, hydrolytic decomposition, being in salt pores by ammonia solution and drying of the obtained sorbet in the air at the temperature of 105-115 deg. The kinetic characteristics of the obtained sorbent in the wide range of pH value of solutions are studied; sodium, chloride, fluoride and phosphate ion sorbtion taken as examples. A high selectivity of the sorbent to phosphate and fluoride ions has been established. The usefullness of the obtained sorbent for extraction of phosphorus microquantities from 1M sodium chloride solution and its concentration at the elution stage is shown

  10. On-line moisture analysis

    International Nuclear Information System (INIS)

    Cutmore, N.G.; Mijak, D.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 material. Nuclear-based analysers measure the total hydrogen content in the sample and do not differentiate between free and combined moisture. Such analysers may also be sensitive to material presentation and elemental composition. Very low frequency electromagnetic probes, such as capacitance or conductance probes, operate in the frequency region where the DC conductivity dominates much of the response, which is a function not only of moisture content but also of ionic composition and chemistry. These problems are overcome using microwave transmission techniques, which also have the following advantages, as a true bulk moisture analysis is obtained, because a high percentage of the bulk material is analysed; the moisture estimate is mostly insensitive to any biased presentation of moisture, for example due to stratification of bulk material with different moisture content and because no physical contact is made between the sensor and the bulk material. This is

  11. Development of an on-line solid phase extraction ultra-high-performance liquid chromatography technique coupled to tandem mass spectrometry for quantification of bisphenol S and bisphenol S glucuronide: Applicability to toxicokinetic investigations.

    Science.gov (United States)

    Grandin, Flore; Picard-Hagen, Nicole; Gayrard, Véronique; Puel, Sylvie; Viguié, Catherine; Toutain, Pierre-Louis; Debrauwer, Laurent; Lacroix, Marlène Z

    2017-12-01

    Regulatory measures and public concerns regarding bisphenol A (BPA) have led to its replacement by structural analogues, such as Bisphenol S (BPS), in consumer products. At present, no toxicokinetic investigations have been conducted to assess the factors determining human internal exposure to BPS for subsequent risk assessment. Toxicokinetic studies require reliable analytical methods to measure the plasma concentrations of BPS and its main conjugated metabolite, BPS-glucuronide (BPS-G). An efficient on-line SPE-UPLC-MS/MS method for the simultaneous quantification of BPS and BPS-G in ovine plasma was therefore developed and validated in accordance with the European Medicines Agency guidelines for bioanalytical method validation. This method has a limit of quantification of 3ngmL -1 for BPS and 10ngmL -1 for BPS-G, an analytical capacity of 200 samples per day, and is particularly well suited to toxicokinetic studies. Use of this method in toxicokinetic studies in sheep showed that BPS, like BPA, is efficiently metabolized into its glucuronide form. However, the clearances and distributions of BPS and BPS-G were lower than those of the corresponding unconjugated and glucuroconjugated forms of BPA. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    Araujo, Lilia; Prieto, Avismelsi; Navalón, Alberto; Vílchez, José Luis; Valera, Paola; Zambrano, Ana; Dugas, Vincent

    2017-01-01

    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. PMID:28686186

  13. 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.

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

    Science.gov (United States)

    Espina-Benitez, Maria; Araujo, Lilia; Prieto, Avismelsi; Navalón, Alberto; Vílchez, José Luis; Valera, Paola; Zambrano, Ana; Dugas, Vincent

    2017-07-07

    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.

  15. A simulation of the SDC on-line processing farm

    International Nuclear Information System (INIS)

    Wang, C.; Chen, Y.; Dorenbosch, J.; Lee, J.; Sayle, R.

    1993-10-01

    In the Solenoidal Detector Collaboration (SDC) data acquisition system (DAQ), an enormous amount of data flows into a processor farm for extraction of interesting physics events. To design an efficient on-line filter, the operations in the farm must be carefully modeled. The authors present a simulation model developed at the Superconducting Super Collider Laboratory which efficiently allocates physics events to the farm

  16. On-line data display

    Science.gov (United States)

    Lang, Sherman Y. T.; Brooks, Martin; Gauthier, Marc; Wein, Marceli

    1993-05-01

    A data display system for embedded realtime systems has been developed for use as an operator's user interface and debugging tool. The motivation for development of the On-Line Data Display (ODD) have come from several sources. In particular the design reflects the needs of researchers developing an experimental mobile robot within our laboratory. A proliferation of specialized user interfaces revealed a need for a flexible communications and graphical data display system. At the same time the system had to be readily extensible for arbitrary graphical display formats which would be required for data visualization needs of the researchers. The system defines a communication protocol transmitting 'datagrams' between tasks executing on the realtime system and virtual devices displaying the data in a meaningful way on a graphical workstation. The communication protocol multiplexes logical channels on a single data stream. The current implementation consists of a server for the Harmony realtime operating system and an application written for the Macintosh computer. Flexibility requirements resulted in a highly modular server design, and a layered modular object- oriented design for the Macintosh part of the system. Users assign data types to specific channels at run time. Then devices are instantiated by the user and connected to channels to receive datagrams. The current suite of device types do not provide enough functionality for most users' specialized needs. Instead the system design allows the creation of new device types with modest programming effort. The protocol, design and use of the system are discussed.

  17. Application of inorganic sorbents for sewage purification from copper

    International Nuclear Information System (INIS)

    Yelizarova, I.A.; Tomchuk, T.K.; Kalinin, N.F.; Vol'khin, V.V.; Levichek, M.S.; Gulyaeva, E.I.

    1986-01-01

    Article presents the results of elaboration of synthesis methods of sorbent on the base of phosphate and magnesium hydroxide. As a result of study the technology of sorbent production with optimal properties was elaborated.

  18. Box-Behnken design for optimum extraction of biogenetic chemicals from P. lanceolata with an energy audit (thermal × microwave × acoustic): a case study of HPTLC determination with additional specificity using on-line/off-line coupling with DAD/NIR/ESI-MS.

    Science.gov (United States)

    Srivastava, Pooja; Ajayakumar, P V; Shanker, Karuna

    2014-01-01

    The genus Pluchea comprises about 80 species distributed worldwide, out of them, only Pluchea lanceolata (DC.) Oliv. & Hiern, is used extensively in the traditional system of India. No chromatographic method is available for its quality. To perform the energy audit for the extraction of biogenetic pentacyclic triterpene, its acetate and sterol from P. lanceolata utilising organic and four alternative solvents. Additionally to resolve the uncertainty of TLC determination, on-line/off-line coupling with a diode-array detector (DAD), and near-infrared (NIR) and electrospray ionisation (ESI) MS was introduced. The extraction of taraxasterol (Tx), taraxasterol acetate (TxAc) and stigmasterol (St) from P. lanceolata was performed using three energy modes. The effects of different operating parameters were studied for optimum extraction yield using the design of experiments, that is, the central composite design and Box-Behnken design. In addition to the retention factor (Rf ) and visible spectral matching, two additional optical spectroscopic techniques, that is, NIR and ESI-MS, were applied for extended specificity. The method was developed for Tx, TxAc and St determination using HPTLC at 645 nm. The optimum extraction yield of targeted compounds was found to be higher with organic solvents than eco-friendly surfactants. The pulse ultrasonic assisted extraction (PUAE) has resulted in optimum extraction of compounds comparable to hot extraction. Both NIR and ESI-MS provided extended specificity in determination. The 5/1-PUAE was determined to be effective, reproducible, simple and energy efficient for the determination of Tx, TxAc and St in P. lanceolata. The offline coupling of NIR and ESI-MS with HPTLC led to considerable improvement in specificity. Copyright © 2014 John Wiley & Sons, Ltd.

  19. Method of purifying phosphoric acid after solvent extraction

    International Nuclear Information System (INIS)

    Kouloheris, A.P.; Lefever, J.A.

    1979-01-01

    A method of purifying phosphoric acid after solvent extraction is described. The phosphoric acid is contacted with a sorbent which sorbs or takes up the residual amount of organic carrier and the phosphoric acid separated from the organic carrier-laden sorbent. The method is especially suitable for removing residual organic carrier from phosphoric acid after solvent extraction uranium recovery. (author)

  20. Long Life Moving-Bed Zinc Titanate Sorbent

    International Nuclear Information System (INIS)

    Copeland, Robert J.; Cesario, Mike; Feinberg, Daniel A.; Sibold, Jack; Windecker, Brian; Yang, Jing

    1997-01-01

    The objective of this work was to develop and test long-life sorbents for hot gas cleanup. Specifically, we measured the sulfur loading at space velocities typically used for absorption of H 2 S and regenerated the sorbent with diluted air for multiple cycles. Based on the experimental results, we prepared a conceptual design of the sorbent-fabrication system, and estimated the cost of sorbent production and of sulfur removal

  1. Alkaline sorbent injection for mercury control

    Science.gov (United States)

    Madden, Deborah A.; Holmes, Michael J.

    2002-01-01

    A mercury removal system for removing mercury from combustion flue gases is provided in which alkaline sorbents at generally extremely low stoichiometric molar ratios of alkaline earth or an alkali metal to sulfur of less than 1.0 are injected into a power plant system at one or more locations to remove at least between about 40% and 60% of the mercury content from combustion flue gases. Small amounts of alkaline sorbents are injected into the flue gas stream at a relatively low rate. A particulate filter is used to remove mercury-containing particles downstream of each injection point used in the power plant system.

  2. 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.

  3. Desulfurization Sorbents for Transport-Bed Applications

    International Nuclear Information System (INIS)

    Gupta, Raghubir P.; Turk, Brian S.; Vierheilig, Albert A.

    1997-01-01

    This project extends the prior work on the development of fluidizable zinc titanate particles using a spray-drying technique to impart high reactivity and attrition resistance. The specific objectives are: (1) To develop highly reactive and attrition-resistant zinc titanate sorbents in 40- to 150-(micro)m particle size range for transport reactor applications; (2) To transfer sorbent production technology to private sector; and (3) To provide technical support to Sierra Pacific Clean Coal Technology Demonstration plant and FETC's Hot-Gas Desulfurization Process Development Unit (PDU), both employing a transport reactor system

  4. Influence of lignin on properties of wood-inorganic sorbents

    International Nuclear Information System (INIS)

    Remez, V.P.; Charina, M.V.; Klass, S.M.; Shubin, A.S.; Tkachev, K.V.; Isaeva, O.F.

    1986-01-01

    Present article is devoted to influence of lignin on properties of wood-inorganic sorbents. The influence of component composition of matrix on sorption properties of sorbents and their stability in different mediums is studied. The dependence of sorption capacity of sorbent on component matrix composition and its porous structure is defined.

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

    Science.gov (United States)

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

    2015-07-01

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

  6. Non-carbon sorbents for mercury removal from flue gases

    Energy Technology Data Exchange (ETDEWEB)

    Alptekin, G.O.; Dubovik, M.; Cesario, M. [TDA Research Inc., Wheat Ridge, CO (United States)

    2005-07-01

    TDA Research Inc. is developing a new sorbent that can effectively remove mercury from flue gases. It is made of non-carbon based materials and will therefore not alter the properties of the fly ash. The sorbent can be produced as an injectable powder. The paper summarises the initial testing results of the new sorbent. The sorbent exhibited 7.5 to 11.0 mg/g mercury absorption capacity under representative flue gas streams depending on the operating temperature and gas hourly space velocity. The sorbent also showed resistance to sulfur poisoning by sulfur dioxide. 6 refs., 3 figs., 1 tab.

  7. Radon adsorption in fibrous carbon sorbents

    International Nuclear Information System (INIS)

    Anshakov, O.M.; Kish, A.O.; Chudakov, V.A.; Matvejchuk, S.V.; Sokolovskij, A.S.; Ugolev, I.I.

    2006-01-01

    Radon sorption in woven fibrous sorbents 'AUT-M' and 'Busofit' and nonwoven fiber in the temperature range 0-50 degrees centigrade was studied. Adsorption heat of radon from the ambient air in different types of carbon fiber was determined. (authors)

  8. Analysis of Ethane and Diethylbenzene Bridged Sorbents

    Science.gov (United States)

    2017-12-13

    Textiles modified in this manner have been shown to reduce or eliminate transport of chemical warfare agents and simulants across the fabric barrier...B.J. Johnson; B.J. Melde; M.H. Moore; A.P. Malanoski; J.R. Taft, "Improving sorbents for glycerol capture in biodiesel refinement," Materials 10

  9. 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. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. The antimicrobial efficiency of silver activated sorbents

    International Nuclear Information System (INIS)

    Đolić, Maja B.; Rajaković-Ognjanović, Vladana N.; Štrbac, Svetlana B.; Rakočević, Zlatko Lj.; Veljović, Đorđe N.; Dimitrijević, Suzana I.; Rajaković, Ljubinka V.

    2015-01-01

    Highlights: • Different sorbents were activated by Ag + -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 + -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 + -activated surface and Ag + -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 + -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 + -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 + -ions desorbed from the activated surface to the

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

    Science.gov (United States)

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

    2016-03-18

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

  12. EXTRACT

    DEFF Research Database (Denmark)

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

    2016-01-01

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

  13. Robust signal extraction for on-line monitoring data

    NARCIS (Netherlands)

    Davies, P.L.; Fried, R.; Gather, U.

    2004-01-01

    Data from the automatic monitoring of intensive care patients exhibits trends, outliers, and level changes as well as periods of relative constancy. All this is overlaid with a high level of noise and there are dependencies between the different items measured. Current monitoring systems tend to

  14. Double salts of ionic-liquid-based surfactants in microextraction: application of their mixed hemimicelles as novel sorbents in magnetic-assisted micro-dispersive solid-phase extraction for the determination of phenols.

    Science.gov (United States)

    Trujillo-Rodríguez, María J; Pino, Verónica; Anderson, Jared L; Ayala, Juan H; Afonso, Ana M

    2015-11-01

    The use of mixed hemimicelles of ionic liquid (IL)-based surfactants in a magnetic-based micro-dispersive solid-phase extraction (m-μdSPE) approach is described. Not only is the symmetric monocationic IL-based surfactant 1,3-didodecylimidazolium bromide (C12C12Im-Br) studied for first time in m-μdSPE, but double-salt (DS) IL (DSIL)-based surfactants are also examined. Nine DSIL-based surfactants were formed by combination of C12C12Im-Br with other IL-based surfactants, including nonsymmetric monocationic and dicationic ILs combined at three different molar fractions. The analytical application was focused on the determination of a group of eight phenols, including bisphenol A, in water samples. The best results were obtained with the DSIL formed by C12C12Im-Br (molar fraction 0.5) and 1-hexadecyl-3-methylimidazolium bromide (C16MIm-Br), after proper optimization of the overall method in combination with high-performance liquid chromatography (HPLC) and diode-array detection (DAD). The optimum conditions for 100 mL of water samples require a small amount (10 mg) of Fe3O4 magnetic nanoparticles, a low content (5.0 mg of C12C12Im-Br and 3.9 mg of C16MIm-Br) of the selected DSIL, pH 11, a sonication time of 2.5 min, and an equilibration time of 5 min with the aid of NdFeB magnets, followed by elution of phenols, evaporation, and reconstitution with 0.5 mL of acetonitrile. The overall m-μdSPE-HPLC-DAD method is characterized for limits of detection down to 1.3 μg · L(-1), intraday relative standard deviations lower than 13 % (n = 3), and interday relative standard deviations lower than 17 % (n = 9), with a spiking level of 15 μg · L(-1); with enrichment factors between 15.7 and 141, and average relative recoveries of 99.9 %.

  15. New polymer bounces into sorbent market

    International Nuclear Information System (INIS)

    Roy, K.A.

    1991-01-01

    Spectacular spills like the Exxon Valdez capture headlines and dominate conversation, but most releases involve quantities too small to attract media attention. For these spills, companies often rely on sorbents to collect the oil and dispose it. These devices come in a variety of shapes, sizes and absorbent materials, including a new generation of products that offers solid results-literally. This paper reports on the Solidifier which absorbs oil, as well as chlorinated solvents, hydrocarbons and PCBs, and, as the name implies, solidifies into a rubber-like material. A polymer used extensively in the rubber industry is the key to the sorbent's success. Oil and other contaminants, act like catalysts. They dissolve into the polymer, causing its molecules to bond together and form a rubber-like mass. No. 2 diesel fuel oil can be bounced on the floor after it solidifies

  16. 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.

  17. Sorbents based on carbonized rice peel

    International Nuclear Information System (INIS)

    Mansurova, R. M.; Taipova, R. A.; Zhylybaeva, N. K.; Mansurov, Z. A.; Bijsenbaev, M. A.

    2004-01-01

    The process receiving of sorbents based on carbonized rice peel (RP) was received and their sorption properties were investigated. Processing carbonization of samples leading on station, this was developed in laboratory of hybrid technology. Carbonization of samples was realized in nitric atmosphere on 400-8000 deg. C. On raising temperature of carbonization content of carbon in samples is rice, hydrogen and oxygen is reduce as a result isolation of volatility products is discover. The samples carbonized on 650 deg. C (910 m 2 /g) owners with maximum removed surface is discover. On carbonization temperature 600-800 deh. C the sorption of ions, which carbonized by sorbents based on rice peel is run to 95-100 %. Electron-microscopic investigation of samples leaded on EM-125 mechanism by accelerating pressure 100 kV. From electron-microscopic print of original samples of RP it is evident, that sample consists of carbonic fractions of different species: carbonic fiber of rounded fractions, fractions of ellipsoid form and of more thickly carbonic structure. Increasing sizes of pores and modification structure of synthesized sorbent is occur during carbonization process. The RP-samples, which carbonized by 650 deg. C has the higher specific surface. Samples consist of thin carbonic scum and reducing specific surface, by higher temperature

  18. CO2 Capacity Sorbent Analysis Using Volumetric Measurement Approach

    Science.gov (United States)

    Huang, Roger; Richardson, Tra-My Justine; Belancik, Grace; Jan, Darrell; Knox, Jim

    2017-01-01

    In support of air revitalization system sorbent selection for future space missions, Ames Research Center (ARC) has performed CO2 capacity tests on various solid sorbents to complement structural strength tests conducted at Marshall Space Flight Center (MSFC). The materials of interest are: Grace Davison Grade 544 13X, Honeywell UOP APG III, LiLSX VSA-10, BASF 13X, and Grace Davison Grade 522 5A. CO2 capacity was for all sorbent materials using a Micromeritics ASAP 2020 Physisorption Volumetric Analysis machine to produce 0C, 10C, 25C, 50C, and 75C isotherms. These data are to be used for modeling data and to provide a basis for continued sorbent research. The volumetric analysis method proved to be effective in generating consistent and repeatable data for the 13X sorbents, but the method needs to be refined to tailor to different sorbents.

  19. Poly(styrene-co-N-methacryloyl-l-phenylalanine methyl ester)-functionalized magnetic nanoparticles as sorbents for the analysis of sodium benzoate in beverages.

    Science.gov (United States)

    Ji, Shilei; Li, Nan; Qi, Li; Wang, Minglin

    2017-01-01

    In this study, poly(styrene-co-N-methacryloyl-l-phenylalanine methyl ester)-functionalized magnetic nanoparticles were constructed and used as magnetic solid-phase extraction sorbents for analysis of food preservatives in beverages. To prepare the poly(amino acid)-based sorbents, N-methacryloyl-l-phenylalanine methyl ester, and styrene served as the functional monomers and modified onto the magnetic nanoparticles via free radical polymerization. Interestingly, compared with propylparaben and potassium sorbate, the proposed poly(amino acid)-based sorbents showed a good selectivity to sodium benzoate. The adsorption capacity of the sorbents to sodium benzoate was 6.08 ± 0.31 mg/g. Moreover, the fast adsorption equilibrium could be reached within 5 min. Further, the resultant poly(amino acid)-based sorbents were applied in the analysis of sodium benzoate in real beverage samples. The results proved that the proposed magnetic solid-phase extraction sorbents have a great potential for the analysis of preservatives in food samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Advanced sorbent development progam; development of sorbents for moving-bed and fluidized-bed applications

    International Nuclear Information System (INIS)

    Ayala, R.E.; Venkataramani, V.S.

    1998-01-01

    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 (900-1000F) 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 assessment and

  1. Enhanced durability and reactivity for zinc ferrite desulfurization sorbent

    Energy Technology Data Exchange (ETDEWEB)

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

    1989-05-02

    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.

  2. Properties and reactivity of reactivated calcium-based sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Davini, P. [Pisa University, Pisa (Italy). Dept. of Chemical Engineering

    2002-04-01

    Calcium-based sorbents used in the process of high temperature desulfurisation of flue gases are partly regenerable by hydration with steam; the best results are obtained for treatment temperatures of approximately 300{degree}C. The regeneration process, and the consequent increase in the sorbent consumption can be correlated to the surface characteristics (BET surface area, porosity and pore size distribution) of the sorbents themselves. In particular, the presence of suitable pore structure, also having pores large enough to let molecules easily penetrate the inner part of the sorbent particles, is very important. 27 refs., 9 figs., 2 tabs.

  3. Simple test guidelines for screening oilspill sorbents for toxicity

    International Nuclear Information System (INIS)

    Blenkinsopp, S.A.; Sergy, G.; Doe, K.; Jackman, P.; Huybers, A.

    1998-01-01

    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

  4. Sorbent selection and design considerations for uranium trapping

    International Nuclear Information System (INIS)

    Schultz, R.M.; Hobbs, W.E.; Norton, J.L.; Stephenson, M.J.

    1981-07-01

    The efficient removal of UF 6 from effluent streams can be accomplished through the selection of the best solid sorbent and the implementation of good design principles. Pressure losses, sorbent capacity, reaction kinetics, sorbent regeneration/uranium recovery requirements and the effects of other system components are the performance factors which are summarized. The commonly used uranium trapping materials highlighted are sodium fluoride, H-151 alumina, XF-100 alumina, and F-1 alumina. Sorbent selection and trap design have to be made on a case-by-case basis but the theoretical modeling studies and the evaluation of the performance factors presented can be used as a guide for other chemical trap applications

  5. Shawnee Mission's On-Line Cataloging System

    Directory of Open Access Journals (Sweden)

    Ellen Wasby Miller

    1971-03-01

    Full Text Available An on-line cataloging pilot project for two elementary schools is discussed. The system components are 2740 terminals, upper-lower-case input, IBM's FASTER generalized software package, and usual cards/labels output. Reasons for choosing FASTER, software and hardware features, operating procedures, system performance and costs are detailed. Future expansion to cataloging 100,000 annual K-12 acquisitions, on-line circulation, retrospective conversion, and union book catalogs is set forth.

  6. INIS retrieval service, towards on-line

    International Nuclear Information System (INIS)

    Ebinuma, Yukio; Komatsubara, Yasutoshi

    1983-01-01

    Japan Atomic Energy Research Institute executes the retrieval service of INIS atomic energy information by batch system in cooperation with Genshiryoku Kozaikai. This service is very popular to the users in whole Japan, but the demand of on-line service has increased recently. Therefore, it was decided to begin the INIS on-line service from January, 1984, through the on-line information retrieval system of the Japan Information Center of Science and Technology. It is expected that when the operation will be started, the utilization of INIS atomic energy information in Japan will drastically increase. Also Japan Atomic Energy Research Institute has carried out the retrieval service by on-line system for those in the institute besides the batch system, accordingly, at this opportunity, the state of utilization of both systems and their distinction to use effectively, and the operation and the method of utilization of the on-line information retrieval system of JICST are explained. In the on-line system, the users are accessible to the data base themselves, and immediate information retrieval is possible, while in the batch system, the related information can be retrieved without fail, and the troublesome operation of equipment is not necessary. (Kako, I.)

  7. 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...

  8. Zwitterion-functionalized polymer microspheres as a sorbent for solid phase extraction of trace levels of V(V), Cr(III), As(III), Sn(IV), Sb(III) and Hg(II) prior to their determination by ICP-MS.

    Science.gov (United States)

    Jia, Xiaoyu; Gong, Dirong; Zhao, Junyi; Ren, Hongyun; Wang, Jiani; Zhang, Xian

    2018-03-19

    This paper describes the preparation of zwitterion-functionalized polymer microspheres (ZPMs) and their application to simultaneous enrichment of V(V), Cr(III), As(III), Sn(IV), Sb(III) and Hg(II) from environmental water samples. The ZPMs were prepared by emulsion copolymerization of ethyl methacrylate, 2-diethylaminoethyl methacrylate and triethylene glycol dimethyl acrylate followed by modification with 1,3-propanesultone. The components were analyzed by elemental analyses as well as Fourier transform infrared spectroscopy, and the structures were characterized by scanning electron microscopy and transmission electron microscopy. The ZPMs were packed into a mini-column for on-line solid-phase extraction (SPE) of the above metal ions. Following extraction with 40 mM NH 4 NO 3 and 0.5 M HNO 3 solution, the ions were quantified by ICP-MS. Under the optimized conditions, the enrichment factors (from a 40 mL sample) are up to 60 for the ions V(V), As(III), Sb(III) and Hg(II), and 55 for Cr(III) and Sn(IV). The detection limits are 1.2, 3.4, 1.0, 3.7, 2.1 and 1.6 ng L -1 for V(V), Cr(III), As(III), Sn(IV), Sb(III) and Hg(II), respectively, and the relative standard deviations (RSDs) are below 5.2%. The feasibility and accuracy of the method were validated by successfully analyzing six certified reference materials as well as lake, well and river waters. Graphical abstract Zwitterion-functionalized polymer microspheres (ZPMs) were prepared and packed into a mini-column for on-line solid-phase extraction (SPE) via pump 1. Then V(V), Cr(III), As(III), Sn(IV), Sb(III) and Hg(II) ions in environmental waters were eluted and submitted to ICP-MS via pump 2.

  9. 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)

  10. Development of Sorbents for Extraction and Stabilization of Nucleic Acids

    Science.gov (United States)

    2016-09-13

    on incorporating common sugars and bovine serum albumin (BSA) as stabilizing agents. Later work evaluated incorporating chemical functionalities...overnight [69]. Functionalized materials were recovered using vacuum filtration with Whatman #5 filter paper , rinsed with toluene, and dried at 110 °C...sugar, and dried at 60 °C for 24 h. For immobilization of bovine serum albumin (BSA), EDC (1-ethyl-3-[3-dimethylaminopropyl]carbodiimide) chemistry was

  11. Development of Sorbents for Extraction and Stabilization of Nucleic Acids

    Science.gov (United States)

    2016-09-13

    EXECUTIVE SUMMARY ...This page intentionally left blank E-1 EXECUTIVE SUMMARY October 2012, the Center for Bio/Molecular Science and...Unlimited 40 Brandy J. White 202-404-6100 Organosilicate RNA Capacity Transport DNA Stability Field sampling

  12. Anionic sorbents for arsenic and technetium species

    International Nuclear Information System (INIS)

    Lucero, Daniel A.; Moore, Robert Charles; Bontchev, Ranko Panayotov; Hasan, Ahmed Ali Mohamed; Zhao, Hongting; Salas, Fred Manuel; Holt, Kathleen Caroline

    2003-01-01

    Two sorbents, zirconium coated zeolite and magnesium hydroxide, were tested for their effectiveness in removing arsenic from Albuquerque municipal water. Results for the zirconium coated zeolite indicate that phosphate present in the water interfered with the sorption of arsenic. Additionally, there was a large quantity of iron and copper present in the water, corrosion products from the piping system, which may have interfered with the uptake of arsenic by the sorbent. Magnesium hydroxide has also been proven to be a strong sorbent for arsenic as well as other metals. Carbonate, present in water, has been shown to interfere with the sorption of arsenic by reacting with the magnesium hydroxide to form magnesium carbonate. The reaction mechanism was investigated by FT-IR and shows that hydrogen bonding between an oxygen on the arsenic species and a hydrogen on the Mg(OH)2 is most likely the mechanism of sorption. This was also confirmed by RAMAN spectroscopy and XRD. Technetium exists in multiple oxidation states (IV and VII) and is easily oxidized from the relatively insoluble Tc(IV) form to the highly water soluble and mobile Tc(VII) form. The two oxidation states exhibit different sorption characteristics. Tc(VII) does not sorb to most materials whereas Tc(IV) will strongly sorb to many materials. Therefore, it was determined that it is necessary to first reduce the Tc (using SnCl2) before sorption to stabilize Tc in the environment. Additionally, the effect of carbonate and phosphate on the sorption of technetium by hydroxyapatite was studied and indicated that both have a significant effect on reducing Tc sorption

  13. 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

  14. Method of making ionic liquid mediated sol-gel sorbents

    Science.gov (United States)

    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.

  15. TRUEX process solvent cleanup with solid sorbents

    International Nuclear Information System (INIS)

    Tse, Pui-Kwan; Reichley-Yinger, L.; Vandegrift, G.F.

    1989-01-01

    Solid sorbents, alumina, silica gel, and Amberlyst A-26 have been tested for the cleanup of degraded TRUEX-NPH solvent. A sodium carbonate scrub alone does not completely remove acidic degradation products from highly degraded solvent and cannot restore the stripping performance of the solvent. By following the carbonate scrub with either neutral alumina or Amberlyst A-26 anion exchange resin, the performance of the TRUEX-NPH is substantially restored. The degraded TRUEX-NPH was characterized before and after treatment by supercritical fluid chromatography. Its performance was evaluated by americium distribution ratios, phase-separation times, and lauric acid distribution coefficients. 17 refs., 2 figs., 5 tabs

  16. Assessment of spent mushroom substrate as sorbent of fungicides: influence of sorbent and sorbate properties.

    Science.gov (United States)

    Marín-Benito, Jesús M; Rodríguez-Cruz, M Sonia; Andrades, M Soledad; Sánchez-Martín, María J

    2012-01-01

    The capacity of spent mushroom substrate (SMS) as a sorbent of fungicides was evaluated for its possible use in regulating pesticide mobility in the environment. The sorption studies involved four different SMS types in terms of nature and treatment and eight fungicides selected as representative compounds from different chemical groups. Nonlinear sorption isotherms were observed for all SMS-fungicide combinations. The highest sorption was obtained by composted SMS from Agaricus bisporus cultivation. A significant negative and positive correlation was obtained between the K(OC) sorption constants and the polarity index values of sorbents and the K(OW) of fungicides, respectively. The statistic revealed that more than 77% of the variability in the K(OW) could be explained considering these properties jointly. The other properties of both the sorbent (total carbon, dissolved organic carbon, or pH) and the sorbate (water solubility) were nonsignificant. The hysteresis values for cyprodinil (log K(OW)= 4) were for all the sorbents much higher (>3) than for other fungicides. This was consistent with the remaining sorption after desorption considered as an indicator of the sorption efficiency of SMS for fungicides. Changes in the absorption bands of fungicides sorbed by SMS observed by FTIR permitted establishing the interaction mechanism of fungicides with SMS. The findings of this work provide evidence for the potential capacity of SMS as a sorbent of fungicides and the low desorption observed especially for some fungicides, although they suggest that more stabilized or humified organic substrates should be produced to enhance their efficiency in environmental applications. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

  17. On-line monitoring for calibration reduction

    International Nuclear Information System (INIS)

    Hoffmann, M.

    2005-09-01

    On-Line Monitoring evaluates instrument channel performance by assessing its consistency with other plant indications. Elimination or reduction of unnecessary field calibrations can reduce associated labour costs, reduce personnel radiation exposure, and reduce the potential for calibration errors. On-line calibration monitoring is an important technique to implement a state-based maintenance approach and reduce unnecessary field calibrations. In this report we will look at how the concept is currently applied in the industry and what the arising needs are as it becomes more commonplace. We will also look at the PEANO System, a tool developed by the Halden Project to perform signal validation and on-line calibration monitoring. Some issues will be identified that are being addressed in the further development of these tools to better serve the future needs of the industry in this area. An outline for how to improve these points and which aspects should be taken into account is described in detail. (Author)

  18. On-line signal trend identification

    International Nuclear Information System (INIS)

    Tambouratzis, T.; Antonopoulos-Domis, M.

    2004-01-01

    An artificial neural network, based on the self-organizing map, is proposed for on-line signal trend identification. Trends are categorized at each incoming signal as steady-state, increasing and decreasing, while they are further classified according to characteristics such signal shape and rate of change. Tests with model-generated signals illustrate the ability of the self-organizing map to accurately and reliably perform on-line trend identification in terms of both detection and classification. The proposed methodology has been found robust to the presence of white noise

  19. 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....... 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...

  20. On-line atomic data access

    Energy Technology Data Exchange (ETDEWEB)

    Schultz, D.R. [Oak Ridge National Lab., TN (United States); Nash, J.K. [Lawrence Livermore National Lab., CA (United States)

    1996-04-01

    The need for atomic data is one which continues to expand in a wide variety of applications including fusion energy, astrophysics, laser- produced plasma research, and plasma processing. Modern computer database and communications technology nables this data to be placed on-line and obtained by users of the Internet. Presented here is a summary of the observations and conclusions regarding such on-line atomic data access derived from a forum held at the Tenth APS Topical Conference on Atomic Processes in Plasmas.

  1. Post-combustion carbon capture - solid sorbents and membranes

    Energy Technology Data Exchange (ETDEWEB)

    Davidson, R.M.

    2009-01-15

    This report follows on from that on solvent scrubbing for post-combustion carbon capture from coal-fired power plants by considering the use of solid sorbents and membranes instead of solvents. First, mesoporous and microporous adsorbents are discussed: carbon-based adsorbents, zeolites, hydrotalcites and porous crystals. Attempts have been made to improve the performance of the porous adsorbent by functionalising them with nitrogen groups and specifically, amine groups to react with CO{sub 2} and thus enhance the physical adsorption properties. Dry, regenerable solid sorbents have attracted a good deal of research. Most of the work has been on the carbonation/calcination cycle of natural limestone but there have also been studies of other calcium-based sorbents and alkali metal-based sorbents. Membranes have also been studied as potential post-combustion capture devices. Finally, techno-economic studies predicting the economic performance of solid sorbents and membranes are discussed. 340 refs., 21 figs., 8 tabs.

  2. Detoxication and recycling of radioactive waters using selective mineral sorbents

    International Nuclear Information System (INIS)

    Berak, L.

    1980-01-01

    Activated BaSO 4 (designated AB 70) was proposed for use in decontaminating concentrated calcium salt solutions containing a small amount of 226 Ra. The AB 70 concentration factor amounts to 2x1a 3 . A sorption contactor for applying the powder sorbent was proposed and will be tested. The AB 70 sorbent liberates small amounts of sulphates into the decontaminated solution, and thus another suitable mineral sorbent was sought. A new sorbent could be synthetized and tested, called RAS-1 whose Ra/Ca selectivity is comparable to that of AB 70 while its Ra/Ba selectivity is considerably higher. The RAS-1 sorbent is also suitable for radiochemical separation in the analysis and concentration of Ra. (Ha)

  3. The development of an on-line gold analyser

    International Nuclear Information System (INIS)

    Robert, R.V.D.; Ormrod, G.T.W.

    1982-01-01

    An on-line analyser to monitor the gold in solutions from the carbon-in-pulp process is described. The automatic system is based on the delivery of filtered samples of the solutions to a distribution valve for measurement by flameless atomic-absorption spectrophotometry. The samples is introduced by the aerosol-deposition method. Operation of the analyser on a pilot plant and on a full-scale carbon-in-pulp plant has shown that the system is economically feasible and capable of providing a continuous indication of the efficiency of the extraction process

  4. The cleaning of the soils polluted by oil and radionuclides by natural sorbents

    International Nuclear Information System (INIS)

    Farajov, M.F.; Shamilov, E.N.; Abdullayev, A.S.; Huseynov, V.I.

    2005-01-01

    Full text : Problem of environmental pollution in oil extracting areas of Absheron peninsula became the very important discussion object lately. It this areas for many years oil and well waters were flowed to environmental areas caused a lot of pools in that areas and at the result the soil and plants were polluted with oil and radionuclides. By last years researches it was revealed that amount of radium 226 oil well water contains 10 - 500 Bq/l. Sometimes amount of radium 226 in polluted soils is increasing to 2000--5000 Bq/l and at the result it is raising probability of entering radionuclides by the way of migration from ground to plants into the nutrition chain cycle. Thus the polluted areas with oil and radionuclides and also when oil spills from oil-pipes by an accident the deactivation of soils is one of the main and most actual problems. In researches for cleaning of polluted soils with radionuclides for the first time were used the phyto sorbent modified breccias forms taken from Chaildag, Gobu, and Lokbatan mud volcano areas. The mineral contain of volcano mud generally consists of clay rocks -(kaolinit, montmorillonit, zeolite, chlorite, biotit) pyrite, and i.e.[2]. The polluted soil samples were taken in Surakhani region from area with the 150 mikroroentgen per hour radiation background. The contain and amount of radionuclides were determined with the radio spectrometer P rogress - Beta - Gamma . Polluted soil samples firstly are washed by hot water and HCl solution by mixing for 3-5 hours. At the next level by adding pieced sorbent into the solution is intensively mixing by mixer and putting for sedimentation for 24 hours. After sedimentation the stiring process is repeated by adding HCl on the sediment again. The soil is stirred by water for last time. Decomposed solutions from soil are adhering and are maked with sorbent again. Thus the soil is quite cleaned from oil and radionuclides by the sorbents we offer. At the same time this sorbents may be

  5. On-line monitoring for calibration reduction

    International Nuclear Information System (INIS)

    Hoffmann, Mario; Gran, Frauke Schmitt; Thunem, Harald P-J.

    2004-04-01

    On-Line Monitoring (OLM) of a channel's calibration state evaluates instrument channel performance by assessing its consistency with other plant indications. Industry and experience at several plants has shown this overall approach to be very effective in identifying instrument channels that are exhibiting degrading or inconsistent performance characteristics. The Halden Reactor Project has developed the signal validation system PEANO, which can be used to assist with the tasks of OLM. To further enhance the PEANO System for use as a calibration reduction tool, the following two additional modules have been developed; HRP Prox, which performs pre-processing and statistical analysis of signal data, Batch Monitoring Module (BMM), which is an off-line batch monitoring and reporting suite. The purpose and functionality of the HRP Prox and BMM modules are discussed in this report, as well as the improvements made to the PEANO Server to support these new modules. The Halden Reactor Project has established a Halden On-Line Monitoring User Group (HOLMUG), devoted to the discussion and implementation of on-line monitoring techniques in power plants. It is formed by utilities, vendors, regulatory bodies and research institutes that meet regularly to discuss implementation aspects of on-line monitoring, technical specification changes, cost-benefit analysis and regulatory issues. (Author)

  6. SPIRES I: on-line search guide

    International Nuclear Information System (INIS)

    Addis, L.

    1975-06-01

    SPIRES I is the first generation of the on-line Stanford Public Information Retrieval System. Designed as a prototype system, SPIRES I was later moved to the SLAC computing facility where it has been routinely available to SLAC users in the field of high-energy physics. The scope and use of the SPIRES I system are described in this manual

  7. HOPI: on-line injection optimization program

    International Nuclear Information System (INIS)

    LeMaire, J.L.

    1977-01-01

    A method of matching the beam from the 200 MeV linac to the AGS without the necessity of making emittance measurements is presented. An on-line computer program written on the PDP10 computer performs the matching by modifying independently the horizontal and vertical emittance. Experimental results show success with this method, which can be applied to any matching section

  8. Polymeric supported sorbents for decreasing hazardous metal ions content in wet process phosphoric acid

    International Nuclear Information System (INIS)

    El-Zahhar, A.A.; El-Naggar, H.A.; Ahmed, M.

    2005-01-01

    Procedure for preparation of polymeric supported silica, and their usage for decreasing hazardous metal ion content in wet process phosphoric acid was developed. The procedure is based firstly on extraction silica from rice straw by alkaline treatment , secondly supporting the produced silica on binding polyacrylonitrile (PAN). The produced polymer based sorbent was used for decreasing hazardous metal ions (especially iron) present as inorganic impurities in crud Egyptian phosphoric acid (green acid). Different factors affecting the sorption equilibrium ( contact time, temperature , sorbent mass and batch factor ) were studied. Studying the sorption isotherm revealed that the adsorption data could favorably fit the Langmuir adsorption isotherm. In the dynamic study , the sorption capacity at (Cξ/Cο = 50%) was found to be 28.5 mg/g and the loaded column could be regenerated using 50ml of 0.15 M HNO 3 . The regenerated column could undergo sorption regeneration cycles up to four cycles without significant decrease in the sorption capacity , weight loss or change in the physical properties of the sorbent

  9. A generalized theory of chromatography and multistep liquid extraction

    Science.gov (United States)

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

    2017-03-01

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

  10. 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.

  11. 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. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. 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.

  13. NIFSIL - a composite sorbent for caesium - properties and application

    International Nuclear Information System (INIS)

    Rajec, P.; Orechovska, J.

    1998-01-01

    Samples of the potassium-nickel ferrocyanides K 2 NiFe(CN) 6 , KNi 1,5 Fe(CN) 6 and Ni 2 Fe(CN) 6 were prepared and their properties studied with respect to their use as sorbents for caesium. Caesium is fixed on mixed alkaline-nickel ferrocyanide without structural change. The capacity of Cs retention never reached the theoretic value corresponding to a total release of the monovalent ions of the solid. High distribution coefficients (K D in the order of 10 4 cm 3 /g) determined in batch experiments show that these sorbents have a very high affinity for caesium ions, even in the presence of competing K + , Na + and Ca 2+ ions. The sorbents have a good chemical stability in a wide pH-range (2-12). The irradiation of some sorbent samples with high energy gamma-rays ( 60 Co) of a total dose of 1.10 5 Gy caused no remarkable changes in the sorbent properties (K D , sorption capacity and kinetics, mechanical stability). The sorbents were also tested for 85 Sr and 239 Pu and the results carried out under dynamic and batch experiments have shown that sorbents are not suitable for removal of these radionuclides. Potassium nickel hexacyanoferrate incorporated in silica-gel matrix could compete with others sorbents based on insoluble hexacyanoferrates, has the advantage of good radiation stability and suitable granulometry. The sorbent was prepared on a pilot scale with a capacity about 1000 kg per year with the prospect that it could be easily upgraded to an industrial scale

  14. 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....

  15. Efficient separations and processing crosscutting program: Develop and test sorbents

    International Nuclear Information System (INIS)

    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 ampersand M University, College Station, Texas. 3M and IBC are responsible for ligand and membrane technology development; AlliedSignal and Texas A ampersand 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

  16. Octahedral molecular sieve sorbents and catalysts

    Science.gov (United States)

    Li, Liyu [Richland, WA; King, David L [Richland, WA

    2010-04-20

    Octahedral molecular sieve sorbents and catalysts are disclosed, including silver hollandite and cryptomelane. These materials can be used, for example, to catalyze the oxidation of CO.sub.x (e.g., CO), NO.sub.x (e.g., NO), hydrocarbons (e.g., C.sub.3H.sub.6) and/or sulfur-containing compounds. The disclosed materials also may be used to catalyze other reactions, such as the reduction of NO.sub.2. In some cases, the disclosed materials are capable of sorbing certain products from the reactions they catalyze. Silver hollandite, in particular, can be used to remove a substantial portion of certain sulfur-containing compounds from a gas or liquid by catalysis and/or sorption. The gas or liquid can be, for example, natural gas or a liquid hydrocarbon.

  17. Potential of Cogon Grass as an Oil Sorbent

    OpenAIRE

    Wiloso, Edi Iswanto; Barlianti, Vera; Anggraini, Irni Fitria; Hendarsyah, Hendris

    2012-01-01

    Experiments on the potential of Cogon grass (lmperata cylindrica), a weed harmful to other plants, for use as a low-cost and biodegradable oil sorbent were carried out under various spill conditions. Flowers of Cogon grass adsorbed much larger amount of high-viscosity lubricating oil (57.9 g-oil/g-sorbent) than that adsorbed by Peat Sorb (7.7 g-oil/g-sorbent), a commercial oilsorbent based on peat. However, the flowers adsorbed only 27.9 g of low-viscosity crude oillgsorbent. In an oil-water ...

  18. Trends in on-line data processing

    International Nuclear Information System (INIS)

    Masetti, M.

    1981-01-01

    The developement of integrated circuits has been characterized by an exponential growth of gates on a single chip that will still continue in the coming years. In parallel the price per bit is dropping down with more or less the same law. As a consequence of this a few statements can be made: The present 16-bit minicomputer in a small configuration is going to be substituted by a 16-bit microcomputer, and the 16-bit microcomputer in a powerful configuration by a 32-bit midi having also a virtual memory facility. Fully programmable or microcoded powerful devices like the LASS hardware processor or MICE, will allow an efficient on-line filter. Higher computing speed can be achieved by a multiprocessor configuration which can be insensitive to hardware failures. Therefore we are moving towards an integrated on-line computing system with much higher computing power than now and the present distinction between on-line and off-line will no longer be so sharp. As more processing can be performed on-line, fast high quality feed-back can be provided for the experiment. In the years to come the trend towards more processing power, at a lower price, and assembled in the same hardware volume will continue for at least five years; at the same time the future large high-energy physics experiments at LEP will be carried out within a wide international collaboration. In this environment methods must be found for a large fraction of the work to be distributed amongst the collaborators. To accomplish this aim it is necessary to introduce common standard practices concerning both hardware and software, in such a way that the seperate parts, developed by the collaborators, will be plug-compatible. (orig.)

  19. 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...

  20. On-Line Maintenance Methodology Development

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hyo Won; Kim, Jae Ho; Jae, Moo Sung [Hanyang University, Seoul (Korea, Republic of)

    2012-05-15

    Most of domestic maintenance activities for nuclear power plants are performed while overhaul. Therefore, On-Line Maintenance (OLM) is one of the proper risks informed application techniques for diffusing maintenance burden during overhaul with safety of the plant is secured. The NUMARC 93-01 (Rev.3) presents the OLM state of the art and it provides methodology. This study adopts NUMARC 93-01 (Rev.3) and present OLM. The reference component is Emergency Diesel Generator (EDG) of Ulchin 3, 4

  1. Importance Role of Low-Cost Sorbent Produced from rice husk in Separation of zirconium from yttrium

    International Nuclear Information System (INIS)

    Kandil, S.A.

    2013-01-01

    The agricultural waste, rice husk, was used as a precursor for the production of low-cost sorbent. Rice husk, a by-product of the rice milling industry, accounts for about 20 % of the whole rice. The argro-residue sorbent extracted from rice husk was employed in separation of zirconium from yttrium. The separation of Zr from the binary systems (Zr-Y) was achieved in batch and column modes. In a batch mode, the adsorption behavior was studied in deferent media, namely, hydrochloric acid, 0.1 M citrate buffer and 0.1 M acetate buffer. In addition, other factors affecting the sorption process of each metal e.g. ph-value of the medium and metal ion concentration were also studied. The breakthrough experiments were carried in the form of mini-column with different bed depths of sorbent at flow rates of 20 ml/min and 40 ml/min. These studies were performed to elucidate the valuable of use of locally, available, agro-residue for separation of Zr from Y target as a promising sorbent for purification of 88 Zr, 89 Zr from Y.

  2. Evaluation of 137Cs sorbents for fixation in concrete

    International Nuclear Information System (INIS)

    Plodinec, M.J.

    1976-01-01

    As part of the long-term waste management program at the Savannah River Laboratory, several 137 Cs sorbents were evaluated for incorporation into concrete. The sorbents studied were: Linde AW-300, AW-500, 13-X, and SK-40; Norton Zeolon 200, 500, and 900; clinoptilolite; and vermiculite. The parameters studied were sorption kinetics, leachability, and compressive strength of the concrete. The best sorbents identified were Linde AW-500 and Norton Zeolon 900. In all tests, these two sorbents performed almost identically; sorption kinetics were acceptable; both strengthened the concrete, and both gave relatively leach-resistant concrete. Vermiculite that had been heated to collapse its lattice around 137 Cs gave the most leach-resistant concrete. However, it sorbed cesium slowly, and the resulting concrete was very weak. When silica gel was added to concrete to react with free calcium, the addition had no effect on cesium leachability

  3. 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.

  4. Dual layer hollow fiber sorbents: Concept, fabrication and characterization

    KAUST Repository

    Bhandari, Dhaval; Olanrewaju, Kayode O.; Bessho, Naoki; Breedveld, Victor; Koros, William J.

    2013-01-01

    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

  5. Development of magnetic micro-solid phase extraction for analysis of phthalate esters in packaged food.

    Science.gov (United States)

    Makkliang, Fonthip; Kanatharana, Proespichaya; Thavarungkul, Panote; Thammakhet, Chongdee

    2015-01-01

    A novel, simple and low cost magnetic multi-walled carbon nanotubes-poly (vinyl alcohol) cryogel-micro-solid phase extraction (magnetic-MWCNTs-PVA cryogel-μ-SPE) sorbent was synthesized by incorporating magnetic particles and MWCNTs into a PVA cryogel. The magnetic-MWCNTs-PVA cryogel-μ-SPE sorbent developed, with a large surface area and macro-porous structure, provided good sorbent-to-sorbent reproducibility (%RSDclear chicken soup samples in the range 0.02-0.07 μg mL(-1). Copyright © 2014 Elsevier Ltd. All rights reserved.

  6. Water purification from radionuclides with using fibroid sorbents

    International Nuclear Information System (INIS)

    Khaydarov, R. A.; Gapurova, O.U.; Khaydarov, R.R.

    2005-01-01

    Full text: Purification waste water and drinking water from radionuclides, heavy metal ions, organic contamination is one of the important problems today. For solving this problem we have created three types of fibroid sorbents on the base of Polyester: cationic and anionic exchange and carbonic. Main properties of these sorbents are described in this article. For example characteristics of the sorbents for removing radionuclides Co-60,57, Zn-65, Sr-89,90, Cs-134,137, etc., radionuclides containing organic molecules M-P-32, M-I-131, M-Mo-99+Tc-99m, M-C-14, etc., heavy metal ions Zn, Ni, Cu, Sb, Pb, Cd, Cr, U, etc., organic molecules (pesticides, phenols, dioxin, benzene, toluene, etc.) were investigated. Influence of pH on percent removal, influence of K, Na and another ions concentrations in the liquid on the percent removal, decreasing of the saturation capacity from number of regeneration and another characteristics are described. Static exchange capacity of the cationic sorbents is 1-2 mg-equ/g and anionic - 0.5-1 mg-equ/g. Capacity of the carbonic sorbents for benzene is 100 mg/g. Time of chemical balance setting is 1-2 s. The sorbents are effective in removing the low concentrations of contamination from the water (lower than 100-200 mg/l) and the air (lower than 100 mg/m 3 ). The use of sorbents in drinking water filters and mini-systems is described. The industrial water purification system consists of coagulating unit, sorbent unit and disinfectant unit. The systems are used in atomic power stations, electroplating plants, matches plants, leather and skin treating plants, car-washing stations, etc

  7. 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.

  8. REMOVAL OF ANIONIC SURFACTANTS FROM WASTEWATER BY MAGNETIC MINERAL SORBENTS

    Directory of Open Access Journals (Sweden)

    Oksana Vladimirova Makarchuk

    2016-07-01

    Full Text Available The simplest and most effective method of removing low concentrations of anionic surfactants such as sodium dodecyl benzenesulfonate (SDBS and sodium lauryl sulfate (SLS is adsorption. Among adsorbents the natural clays are cheap and promising for these purposes. However, there are significant difficulties in removal of spent sorbent after the adsorption process. So, the creation of magnetic sorbents that can be effectively removed from water after sorption by magnetic separation will be a successful decision. The aim of this investigation is the creation of cheap and efficient magnetic sorbents based on natural clays and magnetite for anionic surfactant removal from wastewater. We have synthesized a series of magnetic sorbents from different natural clays with a content of magnetite from 2 to 10 wt%. The ability of magnetic sorbents to remove SDBS and SLS from aqueous solutions has been studied for different adsorbate concentrations by varying the amount of adsorbent, temperature and shaking time. Thermodynamic parameters were calculated from the slope and intercept of the linear plots of ln K against 1/T. Analysis of adsorption results obtained at different temperatures showed that the adsorption pattern on magnetic sorbents correspond to the Langmuir isotherm. It is shown that with increasing the content of magnetite in the magnetic sorbents improves not only their separation from water by magnetic separation, but adsorption capacity to SDBS and SLS. Thus, we obtained of cheap magnetic sorbents based on natural clays and magnetite by the easy way, which not only quickly separated from the solution by magnetic separation, but effectively remove anionic surfactants.

  9. Effectiveness of liquid radioactive waste purification by inorganic granulated sorbents

    International Nuclear Information System (INIS)

    Komarevskij, V.M.; Stepanets, O.V.; Sharygin, L.M.; Matveev, S.A.

    1995-01-01

    Study results on purification of simulative and real liquid radioactive wastes from fission products radionuclides and by inorganic corrosion-nature sorbents 'Thermoxide' are presented. Properties by sorption of cesium, strontium and cobalt are studied; results of experiments on purification of weakly-salted water solutions (waste waters, ships drainage tanks, showers and laundries) of the Beloyarsk NPP are presented. Sorbents source characteristics are determined. 4 refs., 2 figs., 3 tabs

  10. Engineered sorbent barriers for low-level waste disposal

    International Nuclear Information System (INIS)

    Mitchell, S.J.; Freeman, H.D.; Buelt, J.L.

    1987-01-01

    The Engineered Sorbent Barriers Program at Pacific Northwest Laboratory is developing sorbent materials to prevent the migration of radionuclides from low-level waste sites. These materials would allow water to pass, preventing the bathtub effect at humid sites. Screening studies identified promising sorbent materials for three key radionuclides: for cesium, greensand; for cobalt, activated charcoal; and for strontium, synthetic zeolite of clinoptilolite. Mixtures of these sorbent materials were tested in 0.6-m-diameter columns using radioactive leachates. To simulate expected worst-case conditions, the leachate solution contained the radionuclides, competing cations, and a chelating agent, adjusted to a pH of 5. A sorbent barrier comprised of greensand (1 wt%), activated charcoal (6 wt%), synthetic zeolite (20 wt%), and soil (73 wt%) achieved the decontamination factors necessary to meet the regulatory performance requirements established for this study. Sorbent barriers can be applied to shallow land burial, as backfill around the waste or engineered structures, or as backup to other liner systems. 2 references, 6 figures, 3 tables

  11. Characterization of calcium carbonate sorbent particle in furnace environment

    International Nuclear Information System (INIS)

    Lee, Kang Soo; Jung, Jae Hee; Keel, Sang In; Yun, Jin Han; Min, Tai Jin; Kim, Sang Soo

    2012-01-01

    The oxy-fuel combustion system is a promising technology to control CO 2 and NO X emissions. Furthermore, sulfation reaction mechanism under CO 2 -rich atmospheric condition in a furnace may lead to in-furnace desulfurization. In the present study, we evaluated characteristics of calcium carbonate (CaCO 3 ) sorbent particles under different atmospheric conditions. To examine the physical/chemical characteristics of CaCO 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 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 2 atmosphere due to the higher CO 2 partial pressure. Instead, the sintering effect was dominant in the CO 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 2 atmospheres.

  12. Engineered sorbent barriers for low-level waste disposal.

    Energy Technology Data Exchange (ETDEWEB)

    Freeman, H.D.; Mitchell, S.J.; Buelt, J.L.

    1986-12-01

    The Engineered Sorbent Barriers Program at Pacific Northwest Laboratory is investigating sorbent materials to prevent the migration of soluble radio nuclides from low-level waste sites. These materials would allow water to pass, preventing the bathtub effect at humid sites. Laboratory studies identifield promising sorbent materials for three key radionuclides: for cesium, greensand; for cobalt, activated charcoal; and for strontium, synthetic zeolite or clinoptilolite. Mixtures of these sorbent materials were tested in 0.6-m-diameter columns using radioactive leachates. To simulate expected worst-case conditions, the leachate solution contained the radionuclides, competing cations, and a chelating agent and was adjusted to a pH of 5. A sorbent barrier comprised of greensand (1 wt%), activated charcoal (6 wt%), synthetic zeolite (20 wt%), and local soil (73 wt%) achieved the decontamination factors necessary to meet the regulatory performance requirements established for this study. Sorbent barriers can be applied to shallow-land burial, as backfill around the waste or engineered structures, or as backup to other liner systems. 7 refs., 14 figs., 12 tabs.

  13. Engineered sorbent barriers for low-level waste disposal

    International Nuclear Information System (INIS)

    Freeman, H.D.; Mitchell, S.J.; Buelt, J.L.

    1986-12-01

    The Engineered Sorbent Barriers Program at Pacific Northwest Laboratory is investigating sorbent materials to prevent the migration of soluble radio nuclides from low-level waste sites. These materials would allow water to pass, preventing the bathtub effect at humid sites. Laboratory studies identifield promising sorbent materials for three key radionuclides: for cesium, greensand; for cobalt, activated charcoal; and for strontium, synthetic zeolite or clinoptilolite. Mixtures of these sorbent materials were tested in 0.6-m-diameter columns using radioactive leachates. To simulate expected worst-case conditions, the leachate solution contained the radionuclides, competing cations, and a chelating agent and was adjusted to a pH of 5. A sorbent barrier comprised of greensand (1 wt%), activated charcoal (6 wt%), synthetic zeolite (20 wt%), and local soil (73 wt%) achieved the decontamination factors necessary to meet the regulatory performance requirements established for this study. Sorbent barriers can be applied to shallow-land burial, as backfill around the waste or engineered structures, or as backup to other liner systems. 7 refs., 14 figs., 12 tabs

  14. 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

  15. On-line neutron activation analyzers

    International Nuclear Information System (INIS)

    Flahaut, V.; Colmon, A.

    1999-01-01

    A neutronic analyser has been designed to determine the composition of the flow of raw materials entering a cement factory on the conveyor belt. This new system gives a reliable analysis of the whole cargo that outdates the sampling or the usual surface analysis based on fluorescence spectrometry. The accuracy is about 1%.The neutrons interact with the materials on an average depth of 25 cm and are absorbed by nuclei, these nuclei produce photons whose energy is characteristic of the chemical element itself. The composition can be deduced by measuring the number of photons emitted and their energy. The analysis is made on-line and can concern the search for about 10 compounds. In the case of cement the list of compounds is: SiO 2 , CaO, Al 2 O 3 , Fe 2 O 3 , MgO, Na 2 O, TiO 2 , S, Mn 2 O 3 , K 2 O, and H 2 O. The neutron generator involves a deuterium ion source whose deuterium ions are accelerated by means of an electrical field and impinge on a tritiated target, the nuclear reactions between deuterium and tritium produce 14 MeV neutrons. This neutron analysing technique can be adapted to any need of on-line composition determination. (A.C.)

  16. Modified mesoporous silica materials for on-line separation and preconcentration of hexavalent chromium using a microcolumn coupled with flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Wang Zheng, E-mail: wangzheng@mail.sic.ac.cn [Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); Fang Dongmei; Li Qing [Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); East China University of Science and Technology, Shanghai 200237 (China); Zhang Lingxia; Qian Rong; Zhu Yan; Qu Haiyun [Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); Du Yiping [East China University of Science and Technology, Shanghai 200237 (China)

    2012-05-06

    Highlights: Black-Right-Pointing-Pointer A modified SBA-15 mesoporous silica material (NH{sub 2}-SBA-15) was synthesized as sorbent. Black-Right-Pointing-Pointer The material was used for the first time in a flow injection on-line solid phase extraction (SPE) coupled with flame atomic absorption spectrometry (FAAS) to detect trace Cr (VI). Black-Right-Pointing-Pointer The NH{sub 2}-SBA-15 enables retain Cr (VI) with an enrichment factor of 44. Black-Right-Pointing-Pointer The micro-column of NH{sub 2}-SBA-15 underwent more than 100 adsorption/desorption cycles. - Abstract: A modified SBA-15 mesoporous silica material NH{sub 2}-SBA-15 was synthesized successfully by grafting {gamma}-aminopropyl-triethoxysilane. The material was characterized using transmission electron microscopy (TEM) and Fourier transform infrared/Raman (FT-IR/Raman) spectroscopy, and used for the first time in a flow injection on-line solid phase extraction (SPE) coupled with flame atomic absorption spectrometry (FAAS) to detect trace Cr (VI). Effective sorption of Cr (VI) was achieved at pH 2.0 with no interference from Cr (III) and other ions and 0.5 mol L{sup -1} NH{sub 3}{center_dot}H{sub 2}O solution was found optimal for the complete elution of Cr (VI). An enrichment factor of 44 and was achieved under optimized experimental conditions at a sample loading of 2.0 mL min{sup -1} sample loading (300 s) and an elution flow rate of 2.0 mL min{sup -1} (24 s). The precision of the 11 replicate Cr (VI) measurements was 2.1% at the 100 {mu}g L{sup -1} level with a detection limit of 0.2 {mu}g L{sup -1} (3 s, n = 10) using the FAAS. The developed method was successfully applied to trace chromium determination in waste water. The accuracy was validated using a certified reference material of riverine water (GBW08607).

  17. On-Line Core Thermal-Hydraulic Model Improvement

    International Nuclear Information System (INIS)

    In, Wang Kee; Chun, Tae Hyun; Oh, Dong Seok; Shin, Chang Hwan; Hwang, Dae Hyun; Seo, Kyung Won

    2007-02-01

    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

  18. 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.

  19. On line nuclear orientation: opportunity and challenge

    International Nuclear Information System (INIS)

    Stone, N.J.

    1985-01-01

    The development of the on-line nuclear orientation (OLNO) technique is reviewed. The present potential of the technique is discussed in the light of the attainable temperatures, the use of ion implantation and the required isotope flux. Limitations associated with spin-lattice relaxation are considered in some detail and a survey of accessible nuclei is presented. An outline comparison is given between OLNO and other methods for producing orientation of nuclei, for measuring nuclear spins and static moments and for the study of level structure and transition probabilities. The conclusion is drawn that the method in its present form has extensive potential over a wide range of nuclei. Future prospects for in-beam polarisation giving access to nuclei of shorter half lives are referred to briefly. (Auth.)

  20. An on-line diagnostic expert system

    International Nuclear Information System (INIS)

    Felkel, L.

    1987-01-01

    As experience with on-line information systems, experts systems and artificial intelligence tools grows, the authors retreat from the first euphoria that AI could help them solve the problem they were unable to solve with conventional programming. The major effort of the development time goes into building the knowledge-base. There is no such thing as a generic knowledge-base for nuclear power plants as there is, for example, for the diagnosis of a Boeing 747 aircraft. AI-methods, tools and hardware are still in a state which does not optimally lend itself to real-time application. The ability of developing prototype systems to investigate variants otherwise too costly to justify is one advantage that the authors gladly accept. Last, but no least the tools provide a flexible and adaptable user interface (desktop window systems) etc. The development of such tools in a project would be prohibitive and room for experimentation would be limited

  1. On-Line Algorithms and Reverse Mathematics

    Science.gov (United States)

    Harris, Seth

    In this thesis, we classify the reverse-mathematical strength of sequential problems. If we are given a problem P of the form ∀X(alpha(X) → ∃Zbeta(X,Z)) then the corresponding sequential problem, SeqP, asserts the existence of infinitely many solutions to P: ∀X(∀nalpha(Xn) → ∃Z∀nbeta(X n,Zn)). P is typically provable in RCA0 if all objects involved are finite. SeqP, however, is only guaranteed to be provable in ACA0. In this thesis we exactly characterize which sequential problems are equivalent to RCA0, WKL0, or ACA0.. We say that a problem P is solvable by an on-line algorithm if P can be solved according to a two-player game, played by Alice and Bob, in which Bob has a winning strategy. Bob wins the game if Alice's sequence of plays 〈a0, ..., ak〉 and Bob's sequence of responses 〈 b0, ..., bk〉 constitute a solution to P. Formally, an on-line algorithm A is a function that inputs an admissible sequence of plays 〈a 0, b0, ..., aj〉 and outputs a new play bj for Bob. (This differs from the typical definition of "algorithm", though quite often a concrete set of instructions can be easily deduced from A.). We show that SeqP is provable in RCA0 precisely when P is solvable by an on-line algorithm. Schmerl proved this result specifically for the graph coloring problem; we generalize Schmerl's result to any problem that is on-line solvable. To prove our separation, we introduce a principle called Predictk(r) that is equivalent to -WKL0 for standard k, r.. We show that WKL0 is sufficient to prove SeqP precisely when P has a solvable closed kernel. This means that a solution exists, and each initial segment of this solution is a solution to the corresponding initial segment of the problem. (Certain bounding conditions are necessary as well.) If no such solution exists, then SeqP is equivalent to ACA0 over RCA 0 + ISigma02; RCA0 alone suffices if only sequences of standard length are considered. We use different techniques from Schmerl to prove

  2. Software for on-line experiments

    International Nuclear Information System (INIS)

    Ivanchenko, I.M.

    1981-01-01

    A review of nowadays development state of software of on-line electron experiments is presented. The principles of organization of real time systems on second generation computer base are considered. The following methods for projections search are considered: combinator methods, global methods, methods of tracking, methods of a supporting band. The following methods for determining parameter estimates based on the Lorentz equation are analysed: analytical simulation of trajectories, determination of parameters by the iterative method using the technique of calculation of recycled integrals, multidimensional statistical analysis. For the purpose of successful usage and development of software the technique of selfdocumented programs is created and the computer is applied for preparing, revising and circulation of external descriptions which as program complexes are constructed according to the hierarchical principle [ru

  3. On line protection systems for induction motors

    International Nuclear Information System (INIS)

    Colak, I.; Celik, H.; Sefa, I.; Demirbas, S.

    2005-01-01

    Protection of induction motors is very important since they are widely used in industry for many applications due to their high robustness, reliability, low cost and maintenance, high efficiency and long service life. So, protecting these motors is crucial for operations. This paper presents a combined protection approach for induction motors. To achieve this, the electrical values of the induction motor were measured with sensitivity ±1% through a data acquisition card and processed with software developed in Visual C++. An on line protection system for induction motors was achieved easily and effectively. The experimental results have shown that the induction motor was protected against the possible problems faced during the operation. The software developed for this protection provides flexible and reliable media for operators and their motors. It is expected that the motor protection achieved in this study might be faster than the classical techniques and also may be applied to larger motors easily after small modifications of the software

  4. Tunable polymeric sorbent materials for fractionation of model naphthenates.

    Science.gov (United States)

    Mohamed, Mohamed H; Wilson, Lee D; Headley, John V

    2013-04-04

    The sorption properties are reported for several examples of single-component carboxylic acids representing naphthenic acids (NAs) with β-cyclodextrin (β-CD) based polyurethane sorbents. Seven single-component examples of NAs were chosen with variable z values, carbon number, and chemical structure as follows: 2-hexyldecanoic acid (z = 0 and C = 16; S1), n-caprylic acid (z = 0 and C = 8; S2), trans-4-pentylcyclohexanecarboxylic acid (z = -2 and C = 12; S3), 4-methylcyclohexanecarboxylic acid (z = -2 and C = 8; S4), dicyclohexylacetic acid (z = -4; C = 14; S5), 4-pentylbicyclo[2.2.2]octane-1-carboxylic acid (z = -4; C = 14; S6), and lithocholic acid (z = -6; C = 24; S7). The copolymer sorbents were synthesized at three relative β-CD:diisocyanate mole ratios (i.e., 1:1, 1:2, and 1:3) using 4,4'-dicyclohexylmethane diisocyanate (CDI) and 4,4'-diphenylmethane diisocyanate (MDI). The sorption properties of the copolymer sorbents were characterized using equilibrium sorption isotherms in aqueous solution at pH 9.00 with electrospray ionization mass spectrometry. The equilibrium fraction of the unbound carboxylate anions was monitored in the aqueous phase. The sorption properties of the copolymer sorbents (i.e., Qm) were obtained from the Sips isotherm model. The Qm values generally decrease as the number of accessible β-CD inclusion sites in the copolymer framework decreases. The chemical structure of the adsorbates played an important role in their relative uptake, as evidenced by the adsorbate lipophilic surface area (LSA) and the involvement of hydrophobic effects. The copolymers exhibit molecular selective sorption of the single-component carboxylates in mixtures which suggests their application as sorbents for fractionation of mixtures of NAs. By comparison, granular activated carbon (GAC) and chitosan sorbents did not exhibit any significant molecular selective sorption relative to the copolymer materials; however, evidence of variable sorption capacity was

  5. 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.

  6. Tributyl phosphate removal from reprocessing off-gas streams using a selected sorbent

    International Nuclear Information System (INIS)

    Parker, G.B.

    1980-01-01

    Laboratory experiments used small laboratory-scale columns packed with selected sorbent materials to remove tributyl phosphate (TBP) and iodine at conditions approaching those in actual reprocessing off-gas streams. The sorbent materials for TBP removal were placed upstream of iodine sorbent materials to protect the iodine sorbent from the deleterious effects of TBP. Methyl iodide in an airstream containing 30% TBP in normal paraffin hydrocarbons (NPH) and water vapor was metered to two packed columns of sorbents simultaneously (in parallel). One column contained a segment of 8-in. x 14-in. mesh alumina sorbent for TBP removal, the other did not. The measure of the effectiveness of TBP sorbent materials for TBP removal was determined by comparing the iodine retention of the iodine sorbent materials in the two parallel columns. Results from an 18 wt % Ag substituted mordenite iodine sorbent indicated that the iodine retention capacity of the sorbent was reduced 60% by the TBP and that the column containing iodine sorbent material protected by the alumina TBP sorbent retained 30 times more iodine than the column without TBP sorbent. TBP concentration was up to 500 mg/m 3 . Similar experiments using a 7 wt % Ag impregnated silica gel indicated that the TBP vapor had little effect on the iodine retention of the silica gel material. The stoichiometric maximum amount of iodine was retained by the silica gel material. Further experiments were conducted assessing the effects of NO 2 on iodine retention of this 7 wt % Ag sorbent. After the two columns were loaded with iodine in the presence of TBP (in NPH), one column was subjected to 2 vol % NO 2 in air. From visual comparison of the two columns, it appeared that the NO 2 regenerated the silica gel iodine sorbent and that iodine was washed off the silica gel iodine sorbent leaving the sorbent in the original state

  7. Respirometry-based on-line model parameter estimation at a full-scale WWTP

    NARCIS (Netherlands)

    Spanjers, H.; Patry, G.G.; Keesman, K.J.

    2002-01-01

    This paper describes part of a project to develop a systematic approach to knowledge extraction from on-line respirometric measurements in support of wastewater treatment plant control and operation. The paper deals with the following issues: (1) test of the implementation of an automatic set-up

  8. The isotope separator on-line at the INS-SF cyclotron

    International Nuclear Information System (INIS)

    Yonehara, H.; Kawakami, H.; Tanaka, J.; Omata, K.; Shida, Y.

    1981-02-01

    The Isotope Separator On-Line at the SF Cyclotron has been improved. Some details of improvements are described on the target-ion source, rapid extraction with aluminized tape, tape transport system and data aquisition. The performance of the improved SF-ISOL is discussed. (author)

  9. Post combustion carbon capture - solid sorbents and membranes

    Energy Technology Data Exchange (ETDEWEB)

    Davidson, R.M. [IEA Clean Coal Centre, London (United Kingdom)

    2009-04-15

    This report follows on from that on solvent scrubbing for post-combustion carbon capture from coal-fired power plants by considering the use of solid sorbents and membranes instead of solvents. First, mesoporous and microporous adsorbents are discussed: carbon-based adsorbents, zeolites, hydrotalcites and porous crystals. Attempts have been made to improve the performance of the porous adsorbent by functionalising them with nitrogen groups and specifically, amine groups to react with CO{sub 2} and thus enhance the physical adsorption properties. Dry, regenerable solid sorbents have attracted a good deal of research. Most of the work has been on the carbonation/calcination cycle of natural limestone but there have also been studies of other calcium-based sorbents and alkali metal-based sorbents. Membranes have also been studied as potential post-combustion capture devices. Finally, techno-economic studies predicting the economic performance of solid sorbents and membranes are discussed. The report is available from IEA Clean Coal Centre as report no. CCC/144. See Coal Abstracts entry April 2009 00406. 340 refs., 21 figs., 8 tabs.

  10. Oil spill sorbents: Testing protocol and certification listing program

    International Nuclear Information System (INIS)

    Cooper, D.; Gausemel, I.

    1993-01-01

    Environment Canada's Emergencies Engineering Division is spearheading a program in conjunction with the Canadian General Standards Board that would see the development of a certification and listing program in addition to a national standard for the testing of sorbent materials. Funding for this program is provided by Environment Canada (EC), Canadian Coast Guard (CCG), Marine Spill Response Corporation (MSRC), US Coast Guard (USCG), and US Minerals Management Service (MMS). The test methods are based upon those defined by the American Society for Testing and Materials and previous test methods developed by Environment Canada for our series of reports entitled Selection Criteria and Laboratory Evaluation of Oil Spill Sorbents. This series, which was started in 1975, encompasses a number of commercially available oil spill sorbents tested with different petroleum products and hydrocarbon solvents. The testing program will categorize the sorbents according to their operating characteristics. The main categories are oil spills on water, oil spills on land, and industrial use. The characteristics to be evaluated with the new test protocols include initial and maximum sorption capacities, water pickup, buoyancy, reuse potential, retention profile, disintegration (material integrity), and ease of application and retrieval. In the near future are plans to incorporate changes to the test that would involve increasing the list of test liquids to encompass spills in an industrial setting, in addition to testing sorbent booms and addressing the disposal problem

  11. Engineered sorbent barriers for low-level waste disposal

    International Nuclear Information System (INIS)

    Mitchell, S.J.; Freeman, H.D.; Buelt, J.L.

    1986-01-01

    Pacific Northwest Laboratory is developing sorbent materials to prevent the migration of radionuclides from low-level waste sites. These materials would allow water to pass, preventing the bathtub effect at humid sites. Screening studies identified promising sorbent materials for three key radionuclides: for cesium, greensand; for cobalt, activated charcoal; and for strontium, synthetic zeolite or clinoptilolite. Mixtures of these sorbent materials were tested in 0.6-m-diameter columns using radioactive leachates. To simulate expected worst-case conditions, the leachate solution contained the radionuclides, competing cations, and a chelating agent, adjusted to a pH of 5. A sorbent barrier comprised of greensand (1 wt %), activated charcoal (6 wt %), synthetic zeolite (20 wt %), and soil (73 wt %) achieved the decontamination factors necessary to meet the regulatory performance requirements established for this study. Sorbent barriers can be applied to shallow land burial, as backfill around the waste or engineered structures, or as backup to other liner systems. 2 refs., 6 figs., 3 tabs

  12. 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.

  13. Ecologically pure sorbents for power system of Myanmar

    Science.gov (United States)

    Nikitina, I. S.; Moryganova, Y. A.; Maung, Ko Ko; Arefeva, E. A.

    2017-11-01

    Currently, one of the most important problems of the thermal power plant, and many industrial enterprises in different countries is a wastewater treatment for oil products. When choosing the good sorbents is necessary to consider not only the properties and efficiency of the recommended materials, but also the cost, the possibility of environmentally friendly disposal of used sorbents and the possibility of using secondary resources. The purpose of this paper is to study the possibility of using agricultural waste in Myanmar as the sorbents in wastewater treatment containing oil products. The results of experiments have confirmed that rice hulls, and coconut fiber can be effectively used as the sorbents in wastewater treatment containing oil products at concentrations up to 10 mg/l. According to comparative analysis with the conventional sorbent-activated birch carbon (BAC-A) in the Russian power industry has shown that coconut fiber has very good sorption capacity and it is available to use as the raw materials for industries, which does not require to regenerate after using it and can be directly recycled in the factory.

  14. 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.

  15. Sorbent application on the base of chitosan for radionuclides separation

    International Nuclear Information System (INIS)

    Pivarciova, L.

    2016-01-01

    Radioactive waste contains enormous amounts of radionuclides, which pollute the environment and can cause serious chemical and radiological toxicity threats to lower and higher living organism. Alternative process for the removal of heavy metal ions and radionuclides is sorption, which utilizes various certain natural materials of biological origin. Amino-polysaccharide-based sorbents e.g. chitosan represent suitable materials for binding of metal oxo-anion species because of numerous functional groups -OH and -NH_2 because of their suitable H-bond donor and acceptor sites. The sorbents on the base chitosan prepared through chemical modification were used for removal and separation certain radionuclides from aqueous media. The aim of this work was the study of physicochemical properties of prepared sorbents. The specific surface of sorbents was characterized with BET methods. Point of zero charge was identified with potentiometric titration. The size of particles and shape of sorbents were determined by scanning electron microscope. The sorption experiments for selected radionuclides were conducted under static and dynamic conditions. The effect of various parameters on the sorption "9"9"mTc, "6"0Co and the effect of pH on the separation of radionuclide mixture in the solution were studied. (author)

  16. On-line maintenance at Cofrentes NPP

    International Nuclear Information System (INIS)

    Roldan Vilches, J.; Moreno Matarranz, M. A.; Hermana Mendioroz, I.

    1998-01-01

    Cofrentes NPP has begun in 1997 activities related to At Power Preventive Maintenance over trains or systems which lead to a voluntary entry in a Limitative Condition of Operation (LCO) of the Technical Specifications. From others benefits, this program ha improved the risk management and the staff's knowledge over the functions and safety implications of the different systems, the better exploit of the resources, the co-ordination of the different organisations involved (Maintenance an Operation) and the reductions of works during shutdowns. Previous to each work, a feasibility study analyzes qualitative and quantitative (PSA), using the Risk Monitor, the implications on safety of all the tasks, assuring that the global safety of the Plant is always maintained. Tech. Spec. are analyzed in detail and also are analyzed situations of simultaneous unavailabilities of systems which could lead to a high risk situation. Two different risk controls are defined (punctual and accumulated) to assure that high risk situations will not be given. Finally, historical risk profile is analyzed to assure that the accumulated risk increase is not significant. Risk Monitor helps staff in the schedule and follow-up of the activities of On-Line Maintenance. Each one of the tasks are deeply planned and harshly analyzed and are carried out by high qualified workers. By the moment, this program is running with fully satisfaction on the Plant. (Author)

  17. 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.

  18. Simplified automatic on-line document searching

    International Nuclear Information System (INIS)

    Ebinuma, Yukio

    1983-01-01

    The author proposed searching method for users who need not-comprehensive retrieval. That is to provide flexible number of related documents for the users automatically. A group of technical terms are used as search terms to express an inquiry. Logical sums of the terms in the ascending order of frequency of the usage are prepared sequentially and automatically, and then the search formulas, qsub(m) and qsub(m-1) which meet certain threshold values are selected automatically also. Users justify precision of the search output up to 20 items retrieved by the formula qsub(m). If a user wishes more than 30% of recall ratio, the serach result should be output by qsub(m), and if he wishes less than 30% of it, it should be output by qsub(m-1). The search by this method using one year volume of INIS Database (76,600 items) and five inquiries resulted in 32% of recall ratio and 36% of precision ratio on the average in the case of qsub(m). The connecting time of a terminal was within 15 minutes per an inquiry. It showed more efficiency than that of an inexperienced searcher. The method can be applied to on-line searching system for database in which natural language only or natural language and controlled vocabulary are used. (author)

  19. 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.

  20. Application of on-line analytical processing technique in accelerator

    International Nuclear Information System (INIS)

    Xie Dong; Li Weimin; He Duohui; Liu Gongfa; Xuan Ke

    2005-01-01

    A method of application of the on-line analytical processing technique in accelerator is described, which includes data pre-processing, the process of constructing of data warehouse and on-line analytical processing. (authors)

  1. Simultaneous Determination of Palladium and Platinum by On-line ...

    African Journals Online (AJOL)

    NJD

    using high performance liquid chromatography equipped with an on-line enrichment technique. Prior to ... The on-line enrichment system (Waters Corporation, USA) that was ... Using an appropriate volume (industrial plant effluents 20 mL,.

  2. 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...

  3. 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.

  4. 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…

  5. 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

  6. Itaconic acid based potential sorbent for uranium recovery

    International Nuclear Information System (INIS)

    Kalyan, Y.; Naidu, G.R.K.; Das, Sadananda; Pandey, A.K.; Reddy, A.V.R.

    2010-01-01

    Cross-linked hydrogels and adsorptive membranes containing Itaconic acid, Acrylamide, Penta erythritol tetra acrylate and α, α-dimethyl- α-phenyl aceto phenone were prepared by UV-initiated bulk polymerization. These hydrogels and adsorptive membranes were characterized for pH uptake, sorption and desorption kinetics and selectivity towards uranium. The sorption ability of the sorbents towards uranyl ion was thoroughly examined. The developed itaconic acid based sorbents were evaluated for the recovery of uranium from lean sources like sea water. (author)

  7. Bench-scale studies on capture of mercury on mineral non-carbon based sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Li, Yang [Huazhong Univ. of Science and Technology, Wuhan (China). State Key Lab. of Coal Combustion; Utah Univ., Salt Lake City, UT (United States). Dept. of Chemical Engineering; Wendt, Jost O.L. [Utah Univ., Salt Lake City, UT (United States). Dept. of Chemical Engineering; Zhang, Junying; Zheng, Chuguang [Huazhong Univ. of Science and Technology, Wuhan (China). State Key Lab. of Coal Combustion

    2013-07-01

    A new high-temperature, mineral non-carbon based dispersed sorbent derived from paper recycling products has been shown to capture mercury at high temperatures in excess of 600 C. The sorbent is consisted of kaolinite/calcite/lime mixtures. Experiments have been conducted on chemi-sorption of elemental mercury in air on a packed bed. The sorption occurs at temperatures between 600 and 1,100 C and requires activation of the minerals contained within the sorbents. Mercury capture is dominated by temperature and capture on sorbents over long time scales. The capture shows a maximum effectiveness at 1,000 C and increases monotonically with temperature. The presence of oxygen is also the required. Freshly activated sorbent is the most effective, and deactivation of sorbents occurs at high temperatures with long pre-exposure times. This activation is suspected to involve a solid-solid reaction between intimately mixed calcium oxide and silica that are both contained within the sorbent. Deactivation occurs at temperatures higher than 1,000 C, and this is due to melting of the substrate and pore closure. The situation in packed beds is complicated because the bed also shrinks, thus allowing channeling and by-passing, and consequent ambiguities in determining sorbent saturation. Sorbent A had significantly greater capacity for mercury sorption than did Sorbent B, for all temperatures and exposure time examined. The effect of SiO{sub 2} on poor Sorbent B is much larger than sorbent A.

  8. Preparation of Magnetic Sorbent with Surface Modified by C18for Removal of Selected Organic Pollutants from Aqueous Samples

    Science.gov (United States)

    Kuráň, Pavel; Pilnaj, Dominik; Ciencialová, Lucie; Pšenička, Martin

    2017-12-01

    Magnetic sorbents have great potential in environmental applications due to their simple synthesis and separation in magnetic field, usability in heterogeneous systems and low toxicity. Possible syntheses, surface modifications and characteristics were described by Li et al 2013. This type of solid-phase extraction is being successfully used in various fields as health care, microbiology, biotechnologies or sample preconcentration in analytical chemistry. In this preliminary study we report on the preparation and application of magnetically separable sorbent with surface modified by C18 alkyl chain for purification of water contaminated by environmentally hazardous organic compounds. Magnetic cores were co-precipitated from Fe2+ and Fe3+ chlorides in alkalic aqueous solution. Surface of synthetized Fe3O4 was modified with SiO2 by tetraethylorthosilicate to assure physico-chemical stability. Furthermore, Fe3O4/SiO2 complex has been treated by C18 functional group, which provides good affinity towards hydrophobic substances in water. Efficiency of sorption under various conditions has been examined on benzene, toluene, ethylbenzene and xylenes (BTEX), compounds found in petroleum products which contaminate air, soil and groundwater near of store tanks. Sorption kinetics was followed by gas chromatography with mass spectrometry. The preliminary sorption kinetics data and efficiency of BTEX removal point at the possible application of prepared magnetic sorbent for BTEX removal, especially for ethylbenzene and xylenes.

  9. 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.

  10. Sorption of europium (3) by polymer sorbents with grafted heterocyclic nitrogen-containing groupings

    International Nuclear Information System (INIS)

    Bel'tyukova, S.V.; Kravchenko, T.B.; Balamtsarashvili, G.M.; Roska, A.S.

    1990-01-01

    On polymer sorbents (copolymer of styrene-divinylbenzene) with grafted heterocyclic nitrogen-containing functional groupings of tetrazole, triazole and imidazole (sorbents 1,2,3, respectively). It is stated that europium sorption takes place from neutral solutions in presence of organic solvents. Luminescent properties of europium on sorbent are used to develope methods of its determination in high purity lanthanide and yttrium oxides. Europium determination limits consist 7.5·10 -5 μg/ml on 1 and 3 sorbents and 1.5·10 -4 μg/ml on sorbent 2, S p value is 0.089 and 0.075, respectivaly

  11. Flow-injection determination of total organic fluorine with off-line defluorination reaction on a solid sorbent bed.

    Science.gov (United States)

    Musijowski, Jacek; Trojanowicz, Marek; Szostek, Bogdan; da Costa Lima, José Luis Fontes; Lapa, Rui; Yamashita, Hiroki; Takayanagi, Toshio; Motomizu, Shoji

    2007-09-26

    Considering recent reports on widespread occurrence and concerns about perfluoroalkyl substances (PFAS) in environmental and biological systems, analysis of these compounds have gained much attention in recent years. Majority of analyte-specific methods are based on a LC/MS/MS or a GC/MS detection, however many environmental or biological studies would benefit from a total organic fluorine (TOF) determination. Presented work was aimed at developing a method for TOF determination. TOF is determined as an amount of inorganic fluoride obtained after defluorination reaction conducted off-line using sodium biphenyl reagent directly on the sorbent without elution of retained analytes. Recovered fluoride was analyzed using flow-injection system with either fluorimetric or potentiometric detection. The TOF method was tested using perfluorocarboxylic acids (PFCA), including perfluorooctanoic acid (PFOA), as model compounds. Considering low concentrations of PFAS in natural samples, solid-phase extraction as a preconcentration procedure was evaluated. Several carbon-based sorbents were tested, namely multi-wall carbon nanotubes, carbon nanofibres and activated carbon. Good sorption of all analytes was achieved and defluorination reaction was possible to carry out directly on a sorbent bed. Recoveries obtained for PFCAs, adsorbed on an activated carbon sorbent, and measured as TOF, were 99.5+/-1.7, 110+/-9.4, 95+/-26, 120+/-32, 110+/-12 for C4, C6, C8, C10 and C12-PFCA, respectively. Two flow systems that would enable the defluorination reaction and fluoride determination in a single system were designed and tested.

  12. Novel composite sorbent AAm/MA hydrogels containing starch and ...

    Indian Academy of Sciences (India)

    A novel polymer/clay composite sorbent based on acrylamide/maleic acid, starch and clay such as kaolin was synthesized with free radical solution polymerization by using ammonium persulfate/,,','-tetramethylethylenediamine as redox initiating pair in the presence of poly(ethylene glycol)diacrylate as a crosslinker.

  13. New Composite Sorbents for Caesium and Strontium Ions Sorption

    Directory of Open Access Journals (Sweden)

    Mykola Kartel

    2017-06-01

    Full Text Available Composite lignocellulose-inorganic sorbents derived from plant residues of agriculture and food industry, modified with ferrocyanides of d-metals and hydrated antimony pentoxide were prepared. Caesium and strontium ions removal from water was tested by radiotracer method. Sorption of heavy metal ions, methylene blue, gelatin, vitamin B12 was also studied.

  14. Evaluation of inorganic sorbent treatment for LWR coolant process streams

    International Nuclear Information System (INIS)

    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

  15. Comments on "Ceria-Zirconia High-Temperature Desulfurization Sorbents".

    Czech Academy of Sciences Publication Activity Database

    Hartman, Miloslav; Trnka, Otakar

    2006-01-01

    Roč. 45, č. 4 (2006), s. 1548-1549 ISSN 0888-5885 Institutional research plan: CEZ:AV0Z40720504 Keywords : hydrogen sulfide * desulfurization * cerium sorbent Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 1.518, year: 2006

  16. Natural sorbents for decontamination of objects of urban territories

    International Nuclear Information System (INIS)

    Movchan, N.; Fedorenko, Yu.; Zlobenko, B.; Spigoun, A.

    1996-01-01

    This paper gives an information about the use of film coverings, based on natural sorbents, in decontamination of buildings, contaminated after the Chernobyl accident. This method has incontrovertible advantages in the beginning period after the accident and can be used for cleaning considerable areas of urban territories

  17. Core-in-shell sorbent for hot coal gas desulfurization

    Science.gov (United States)

    Wheelock, Thomas D.; Akiti, Jr., Tetteh T.

    2004-02-10

    A core-in-shell sorbent is described herein. The core is reactive to the compounds of interest, and is preferably calcium-based, such as limestone for hot gas desulfurization. The shell is a porous protective layer, preferably inert, which allows the reactive core to remove the desired compounds while maintaining the desired physical characteristics to withstand the conditions of use.

  18. 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.

  19. 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

  20. Composite materials based on inorganic sorbents and extractants - new sorbents for several radionuclides removal from liquid radioactive wastes

    International Nuclear Information System (INIS)

    Kopyrin, A.A.

    1999-01-01

    A short review of recent investigation concerned with liquid radioactive waste treatment by means of composite materials. It is considered different aspects of technology of selective radionuclides removal and its direction connected with usage of composites. Results of research works in this line carried out under the direction of author are presented. (author)

  1. On-line packed magnetic in-tube solid phase microextraction of acidic drugs such as naproxen and indomethacin by using Fe3O4@SiO2@layered double hydroxide nanoparticles with high anion exchange capacity.

    Science.gov (United States)

    Shamsayei, Maryam; Yamini, Yadollah; Asiabi, Hamid; Safari, Meysam

    2018-02-22

    The authors describe a 3-component nanoparticle system composed of a silica-coated magnetite (Fe 3 O 4 ) core and a layered double (Cu-Cr) hydroxide nanoplatelet shell. The sorbent has a high anion exchange capacity for extraction anionic species. A simple online system, referred to as "on-line packed magnetic-in-tube solid phase microextraction" was designed. The nanoparticles were placed in a stainless steel cartridge via dry packing. The cartridge was then applied to the preconcentration acidic drugs including naproxen and indomethacin from urine and plasma. Extraction and desorption times, pH values of the sample solution and flow rates of sample solution and eluent were optimized. Analytes were then quantified by HPLC with UV detection. Under optimal conditions, the limits of detection range from 70 to 800 ng L -1 , with linear responses from 0.1-500 μg L -1 (water samples), 0.6-500 μg L -1 (spiked urine), and 0.9-500 μg L -1 (spiked plasma). The inter- and intra-assay precisions (RSDs, for n = 5) are in the range of 2.2-5.4%, 2.8-4.9%, and 2.0-5.2% at concentration levels of 5, 25 and 50 μg L -1 , respectively. The method was applied to the analysis of the drugs in spiked human urine and plasma, and good results were achieved. Graphical abstract Fe 3 O 4 @SiO 2 @CuCr-LDH magnetic nanoparticles were synthesized and packed in to a stainless steel column. The column was applied to solid phase microextraction of acidic drugs from biological samples.

  2. 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

  3. 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.

  4. 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-C 12 ) and phenethyl (PhE) ligands. Here, the ability of the PF-C 12 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-C 12 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

  5. DOE-EPRI On-Line Monitoring Implementation Guidelines

    International Nuclear Information System (INIS)

    E. Davis, R. Bickford

    2003-01-01

    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 feasibility of on-line monitoring at several participating nuclear plants. The results have been very encouraging, and substantial progress is anticipated in the coming years

  6. A critical review of microextraction by packed sorbent as a sample preparation approach in drug bioanalysis.

    Science.gov (United States)

    Alves, Gilberto; Rodrigues, Márcio; Fortuna, Ana; Falcão, Amílcar; Queiroz, João

    2013-06-01

    Sample preparation is widely accepted as the most labor-intensive and error-prone part of the bioanalytical process. The recent advances in this field have been focused on the miniaturization and integration of sample preparation online with analytical instrumentation, in order to reduce laboratory workload and increase analytical performance. From this perspective, microextraction by packed sorbent (MEPS) has emerged in the last few years as a powerful sample preparation approach suitable to be easily automated with liquid and gas chromatographic systems applied in a variety of bioanalytical areas (pharmaceutical, clinical, toxicological, environmental and food research). This paper aims to provide an overview and a critical discussion of recent bioanalytical methods reported in literature based on MEPS, with special emphasis on those developed for the quantification of therapeutic drugs and/or metabolites in biological samples. The advantages and some limitations of MEPS, as well as its comparison with other extraction techniques, are also addressed herein.

  7. 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.

  8. Comparing the Hierarchy of Keywords in On-Line News Portals.

    Directory of Open Access Journals (Sweden)

    Gergely Tibély

    Full Text Available 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.

  9. 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

  10. Comparison of extraction chromatography and a procedure based on the molecular recognition method as separation methods in the determination of neptunium and plutonium radionuclides

    International Nuclear Information System (INIS)

    Strisovska, Jana; Galanda, Dusan; Drabova, Veronika; Kuruc, Jozef

    2012-01-01

    The potential of various types of sorbents for separation of radionuclides of plutonium and neptunium were examined. Extraction chromatography and a procedure based on the molecular recognition method were used for the separation. The suitability of the various sorbent types and brands for this purpose was determined. (orig.)

  11. On-line determination of manganese in solid seafood samples by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Yebra, M.C.; Moreno-Cid, A.

    2003-01-01

    Manganese is extracted on-line from solid seafood samples by a simple continuous ultrasound-assisted extraction system (CUES). This system is connected to an on-line manifold, which permits the flow-injection flame atomic absorption spectrometric determination of manganese. Optimisation of the continuous leaching procedure is performed by an experimental design. The proposed method allows the determination of manganese with a relative standard deviation of 0.9% for a sample containing 23.4 μg g -1 manganese (dry mass). The detection limit is 0.4 μg g -1 (dry mass) for 30 mg of sample and the sample throughput is ca. 60 samples per hour. Accurate results are obtained by measuring TORT-1 certified reference material. The procedure is finally applied to mussel, tuna, sardine and clams samples

  12. 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.

  13. 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

  14. 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. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Graphene Quantum Dots/Eggshell Membrane Composite as a Nano-sorbent for Preconcentration and Determination of Organophosphorus Pesticides by High-Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Vahideh Abdollahi

    2017-10-01

    Full Text Available In this study graphene quantum dots/eggshell membrane nanocomposite (GQDS/ESM is prepared and used as an efficient solid-phase extraction (SPE sorbent for preconcentration of organophosphorus pesticides (OPPs from aqueous solutions. The retained analytes on the sorbent are stripped by acetonitrile and subsequently are determined by high-performance liquid chromatography. Various parameters affecting the extraction efficiency of OPPs on the GQDS/ESM, such as solution pH, amount of nano-sorbent, sample loading flow rate, elution conditions and sample volume are investigated. The results demonstrated that the proposed method has a wide dynamic linear range (0.05–100 ng mL-1, good linearity (R2>0.997 and low detection limits (0.006-0.32 ng mL-1. High enrichment factors are achieved ranging from 110 to 140. In the optimum experimental conditions, the established method is successfully applied for the determination of OPPs in spiked water samples (well, tap, shaft and canal and apple juice. Satisfactory recovery results show that the sample matrices under consideration do not significantly affect the extraction process.

  16. Algorithms for the on-line travelling salesman

    NARCIS (Netherlands)

    Ausiello, G.; Feuerstein, E.; Leonardi, S.; Stougie, L.; Talamo, M.

    1999-01-01

    In this paper the problem of efficiently serving a sequence of requests presented in an on-line fashion located at points of a metric space is considered. We call this problem the On-Line Travelling Salesman Problem (OLTSP). It has a variety of relevant applications in logistics and robotics. We

  17. An algorithm for on-line price discrimination

    NARCIS (Netherlands)

    D.D.B. van Bragt; D.J.A. Somefun (Koye); E. Kutschinski; J.A. La Poutré (Han)

    2002-01-01

    textabstractThe combination of on-line dynamic pricing with price discrimination can be very beneficial for firms operating on the Internet. We therefore develop an on-line dynamic pricing algorithm that can adjust the price schedule for a good or service on behalf of a firm. This algorithm (a

  18. On-Line Voltage Stability Assessment based on PMU Measurements

    DEFF Research Database (Denmark)

    Garcia-Valle, Rodrigo; P. Da Silva, Luiz C.; Nielsen, Arne Hejde

    2009-01-01

    This paper presents a method for on-line monitoring of risk voltage collapse based on synchronised phasor measurement. As there is no room for intensive computation and analysis in real-time, the method is based on the combination of off-line computation and on-line monitoring, which are correlat...

  19. 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

  20. On-line Learning of Prototypes and Principal Components

    NARCIS (Netherlands)

    Biehl, M.; Freking, A.; Hölzer, M.; Reents, G.; Schlösser, E.; Saad, David

    1998-01-01

    We review our recent investigation of on-line unsupervised learning from high-dimensional structured data. First, on-line competitive learning is studied as a method for the identification of prototype vectors from overlapping clusters of examples. Specifically, we analyse the dynamics of the

  1. On-line and bulk analysis for the resource industries

    International Nuclear Information System (INIS)

    Lim, C.S.; Sowerby, B.D.; Tickner, J.R.; Madsen, I.C.

    2001-01-01

    Nuclear techniques are the basis of many CSIRO on-line and bulk analysis systems that are now widely used in the mineral and energy industries. The continuous analysis and rapid response of these systems have led to improved control of mining, processing and blending operations. This paper reviews recent developments in neutron, gamma-ray and X-ray techniques for on-line and bulk analysis by CSIRO Minerals including neutron techniques for the on-conveyor belt determination of the composition of cement raw meal, the on-line analysis of composition in pyrometallurgical applications, the on-conveyor belt determination of ash in coal, and the rapid and accurate determination of gold in bulk laboratory samples. The paper also discusses a new gamma-ray technique for the on-line determination of ash in coal and the application of X-ray diffraction techniques for the on-line determination of mineralogy in the cement industry

  2. 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.

  3. 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.

  4. Sorbents for effective removal of radioactive antimony during chemical decontamination

    International Nuclear Information System (INIS)

    Nishad, Padala Abdul; Bhaskarapillai, Anupkumar; Velmurugan, Sankaralingam

    2014-01-01

    Removal of radioactive antimony is a challenging problem. Often, during decontamination, they get mobilized around the system and redeposit in different areas thus offsetting the reduction in the radiation field obtained by removing other activities such as 60 Co. Thus, there is a clear need for better antimony removing materials/strategies for effective reactor decontamination. In this regard, six commercially available sorbents namely, Tulsion A33 (strong base anion (-OH) resin), Amberlite IRC-718 (chelating resin), Radex ® Sb-1000, nano TiO 2 -special grade (Inorganic type IX), Chitosan (biosorbent) and Aeroxide p25 (nano TiO 2 , Inorganic type IX) were evaluated for their antimony sorption properties. Radex ® and TiO 2 based materials were found to be more effective in removing both Sb(V) and Sb(III). Solution pH was seen to significantly influence the antimony sorption and the effect was more prominent in anion resin, when tested under column conditions. Apart from the commercial sorbents, we have synthesised a robust high performing sorbent (TA-Chitosan beads) in the form of stable beads, using nano-TiO 2 and chitosan. The beads were found to retain the antimony sorption properties of the nano-TiO 2 , while adapting a physical format suitable for large scale operations. The sorbent exhibited almost complete sorption of antimony both in low (ppb level) as well as high concentrations of antimony. The suitability of the beads for use in column mode has been established and its radiation stability was probed in detail. The beads were found to be stable to irradiations as ascertained from the TOC values and unchanged sorption properties. The sorption properties of the CHITA beads in typical decontamination formulation containing mixture of complexing agents have been investigated in detail. (author)

  5. 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.

  6. CARBON DIOXIDE CAPTURE FROM FLUE GAS USING DRY REGENERABLE SORBENTS

    International Nuclear Information System (INIS)

    David A. Green; Brian S. Turk; Raghubir P. Gupta; William J. McMichael; Douglas P. Harrison; Ya Liang

    2002-01-01

    The objective of this project is to develop a simple, inexpensive process to separate CO(sub 2) as an essentially pure stream from a fossil fuel combustion system using a regenerable, sodium-based sorbent. The sorbents being investigated in this project are primarily alkali carbonates, and particularly sodium carbonate and potassium carbonate, which are converted to bicarbonates, through reaction with carbon dioxide and water vapor. Bicarbonates are regenerated to carbonates when heated, producing a nearly pure CO(sub 2) stream after condensation of water vapor. This quarter, electrobalance tests conducted at LSU indicated that exposure of sorbent to water vapor prior to contact with carbonation gas does not significantly increase the reaction rate. Calcined fine mesh trona has a greater initial carbonation rate than calcined sodium bicarbonate, but appears to be more susceptible to loss of reactivity under severe calcination conditions. The Davison attrition indices for Grade 5 sodium bicarbonate, commercial grade sodium carbonate and extra fine granular potassium carbonate were, as tested, outside of the range suitable for entrained bed reactor testing. Fluidized bed testing at RTI indicated that in the initial stages of reaction potassium carbonate removed 35% of the carbon dioxide in simulated flue gas, and is reactive at higher temperatures than sodium carbonate. Removals declined to 6% when 54% of the capacity of the sorbent was exhausted. Carbonation data from electrobalance testing was correlated using a shrinking core reaction model. The activation energy of the reaction of sodium carbonate with carbon dioxide and water vapor was determined from nonisothermal thermogravimetry

  7. Stir Bar Sorptive Extraction (SBSE), a novel extraction technique for aqueous samples: theory and principles

    NARCIS (Netherlands)

    Baltussen, H.A.; Sandra, P.J.F.; David, F.; Cramers, C.A.M.G.

    1999-01-01

    The theory and practice of a novel approach for sample enrichment, namely the application of stir bars coated with the sorbent polydimethylsiloxane (PDMS) and referred to as stir bar sorptive extraction (SBSE) are presented. Stir bars with a length of 10 and 40 mm coated with 55 and 219 L of PDMS

  8. 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.

  9. CARBON DIOXIDE CAPTURE FROM FLUE GAS USING DRY REGENERABLE SORBENTS

    Energy Technology Data Exchange (ETDEWEB)

    David A. Green; Brian S. Turk; Raghubir P. Gupta; Alejandro Lopez-Ortiz; Douglas P. Harrison; Ya Liang

    2001-07-01

    Sodium based sorbents including sodium carbonate may be used to capture carbon dioxide from flue gas. A relatively concentrated carbon dioxide stream may be recoverable for sequestration when the sorbent is regenerated. Electrobalance tests indicated that sodium carbonate monohydrate was formed in a mixture of helium and water vapor at temperatures below 65 C. Additional compounds may also form, but this could not be confirmed. In the presence of carbon dioxide and water vapor, both the initial reaction rate of sodium carbonate with carbon dioxide and water and the sorbent capacity decreased with increasing temperature, consistent with the results from the previous quarter. Increasing the carbon dioxide concentration at constant temperature and water vapor concentration produced a measurable increase in rate, as did increasing the water vapor concentration at constant carbon dioxide concentration and temperature. Runs conducted with a flatter TGA pan resulted in a higher initial reaction rate, presumably due to improved gas-solid contact, but after a short time, there was no significant difference in the rates measured with the different pans. Analyses of kinetic data suggest that the surface of the sodium carbonate particles may be much hotter than the bulk gas due to the highly exothermic reaction with carbon dioxide and water, and that the rate of heat removal from the particle may control the reaction rate. A material and energy balance was developed for a cyclic carbonation/calcination process which captures about 26 percent of the carbon dioxide present in flue gas available at 250 C.

  10. Cleanup of Savannah River Plant solvent using solid sorbents

    International Nuclear Information System (INIS)

    Mailen, J.C.; Tallent, O.K.

    1985-04-01

    The degradation products produced in Purex solvent by exposure to nitric acid and radiation can be divided into two groups: those which are removed by scrubbing with sodium carbonate solutions and those which are not; these latter materials are called secondary degradation products. This study investigated the use of solid sorbents for removal of the secondary degradation products from first-cycle Savannah River Plant solvent that had been previously washed with sodium carbonate solution. Silica gel, activated charcoal, macroreticular resin, attapulgite clay and activated alumina were the sorbents investigated in preliminary testing. Activated alumina was found to be most effective for improving phase separation of the solvent from sodium carbonate solutions and for increasing the interfacial tension. The activated alumina was also the sorbent most useful for removing complexants which retain plutonium at low acidity, but it was less effective in removing anionic surfactants and ruthenium. We found that the capacity of the activated alumina was greatly improved by drying the solvent before treatment

  11. Investigation of solid phase sorbents for the pre- concentration of pads from aqueous medium and their quantitation by high performance liquid chromatography-UV detection

    International Nuclear Information System (INIS)

    Waqar, F.; Jan, S.; Muhammad, B.; Ahmad, S.; Riaz, M.; Akram, N.

    2005-01-01

    A solid phase extraction method was optimized for the pre-concentration of polyaromatic hydrocarbons (PAHs) in water samples. Graphite powder and Lab scale locally synthesized styrene divinylbenzene (SDVB) Copolymer were used as sorbents for the extraction of PAHs and compared with commercially used C18 solid phase extraction cartridge (SPE). Various parameters were optimized to evaluate the extraction efficiencies, the best results were obtained by proper conditioning of extraction cartridges and desorption with suitable solvent. Percentage recoveries were enhanced by rinsing the sample bottles with acetonitrile and combining the rinse with the sample extract. Quantitative analysis was performed by High performance Liquid chromatography (HPLC) with UV detection. Many other parameters, including optimization of mobile phase, selection of HPLC Columns, sample-loading flow rate on extraction cartridge and weight of sorbent were performed to get optimal results. Percent recoveries obtained with synthesized copolymer were comparable with commercial cartridge, while graphite powder showed excellent retention but very poor recoveries. Obtained recoveries of selected PAHs were ranged from 80-87% with relative standard deviation <6%. Developed method was applied for the analysis of drinking water samples(author)

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

    KAUST Repository

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

    2013-01-01

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

  13. Different sorbents in calcium looping cycle for CO{sub 2} capture

    Energy Technology Data Exchange (ETDEWEB)

    Luo, Cong; Zheng, Ying; Ding, Ning [Huazhong Univ. of Science and Technology, Wuhan (China). State Key Lab. of Coal Combustion

    2013-07-01

    Cyclic CO{sub 2} capture using commercial pure micro CaCO{sub 3} and nano CaCO{sub 3} is investigated in this paper which focuses on the different characteristics two different sorbents during high temperature reactions. The results indicate that the nano CaCO{sub 3} sorbent has higher carbonation conversions and carbonation rates than the micro CaCO{sub 3} sorbent in the cyclic reactions. Furthermore, nano sorbent can retain its fast carbonation rates at the beginning dozens of seconds during each cycle. In contrast, the carbonation rates of micro sorbent diminish with the increase of cycle number. But, unfortunately, CaO derived from nano CaCO3 sorbent sinter much easily. Its grains, which are composed of numerous spherical nanocrystallites, experience dramatic morphological changes during high temperature reactions.

  14. 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.

  15. Off-Gas Treatment: Evaluation of Nano-structured Sorbents for Selective Removal of Contaminants

    Energy Technology Data Exchange (ETDEWEB)

    Utgikar, Vivek; Aston, D. Eric; Sabharwall, Piyush

    2018-03-30

    Reprocessing of used nuclear fuel (UNF) is expected to play an important role for sustainable development of nuclear energy by increasing the energy extracted from the fuel and reducing the generation of the high level waste (HLW). However, aqueous reprocessing of UNF is accompanied by emission of off-gas streams containing radioactive nuclides including iodine, krypton, xenon, carbon, and tritium. Volatile iodine (129I), and krypton (85Kr) are long lived isotopes which have adverse effects on the environment as well as human health. Development of methods for the capture and long-term storage of radioactive gases is of crucial importance in order to manage their emissions that are anticipated to increase significantly with the growth of nuclear energy. For more than 70 years, porous solid sorbents have been in the forefront of radioactive contaminant removal due to promising results and their advantages such as high removal efficiency, low maintenance cost, simple equipment design and operation over other techniques. The research conducted in this project has focused on development of a novel nanostructured sorbent and its application for the capture of the above two contaminants of interest. Nanostructured carbon polyhedrons supported on Engelhard Titanosilicate-10 sorbent was synthesized using hydrothermal methods and subjected to structural and compositional characterization using various techniques including electron microscopy, Raman, x-ray diffraction and BET surface area analysis. Dynamic sorption experiments conducted using a flow-through column setup yielded information on the thermodynamics and kinetics of sorption in single-contaminant and multi-contaminant streams. Parameters varied in the study included carbon loading, temperature, contact time, contaminant concentration and humidity. The behavior of the system was modeled using models available in literature as well as development of a mass-transfer model from fundamental principles. Experimental

  16. Human interface for personal information systems. On-line handwriting recognition; Pasonaru joho kiki ni okeru human interface. On-line tegaki ninshiki

    Energy Technology Data Exchange (ETDEWEB)

    Morita, T. [Sharp Corp., Osaka (Japan)

    1996-01-05

    Most of information devices used in the business field use keyboards for the inputting measure, but keyboards are rather awkward for personal use. In contrast to this, the pen input method which everybody can use easily is a product of the latest development. In this articles, on-line handwritten letter recognition is roughly explained which is the basic technique of pen input. Pen input has a demerit that its letter inputting speed is slow, but has much more merits that Chinese ideographs can be directly input, figures, handwritten memoranda, etc. are treated likewise, the device itself can be made compact and no noise is made. The on-line letter recognition methods now used practically can be roughly divided into the pattern matching method and the basic stroke method. Each of them has its own merits and demerits. For the current on-line handwritten letter recognition, the condition is necessary to handwritten a letter in the square style (kaisho) and carefully within the framework for letter entry upon writing, and for this arrangement, input is performed through the work processes of pretreatment/feature extraction, stroke recognition, letter comparison, detail discrimination, and after-treatment. 3 refs., 7 figs.

  17. 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

  18. 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

  19. Understanding on-line community: the affordances of virtual space

    Directory of Open Access Journals (Sweden)

    Karen Ruhleder

    2002-01-01

    Full Text Available Increasing numbers of on-line venues for learning are emerging as virtual communities become more accessible and commonplace. This paper looks at one particular virtual community, an on-line degree programme at the University of Illinois, Urbana-Champaign, which offers an M.S. in Library and Information Science (called LEEP. It draws on a framework presented by Mynatt, et al. (1998, which provides a lens for talking about on-line community as a set of affordances. This framework is applied to illustrate the interactions, artefacts, and expectations that shape this community.

  20. An Approach to On-line Risk Assessment in NPP

    International Nuclear Information System (INIS)

    Simic, Z.; Mikulicic, V.; O'Brien, J.

    1996-01-01

    Probabilistic Risk Assessment (PRA) can provide safety status information for a plant during different configurations; additional effort is needed to do this in real time for on-line operation. This paper describes an approach to use PRA to achieve these goals. A Risk Assessment On-Line (RAOL) application was developed to monitor maintenance (on-line and planned) activities. RAOL is based on the results from a full-scope PRA, engineering/operational judgment and incorporates a user friendly program interface approach. Results from RAOL can be used by planners or operations to effectively manage the level of risk by controlling the actual plant configuration. (author)

  1. On-line spectroscopy with thermal atomic beams

    International Nuclear Information System (INIS)

    Thibault, C.; Guimbal, P.; Klapisch, R.; Saint Simon, M. de; Serre, J.M.; Touchard, F.; Duong, H.T.; Jacquinot, P.; Juncar, P.

    1981-01-01

    On-line high resolution laser spectroscopy experiments have been performed in which the light from a cw tunable dye laser interacts at right angles with a thermal atomic beam. sup(76-98)Rb, sup(118-145)Cs and sup(208-213)Fr have been studied using the ionic beam delivered by the ISOLDE on-line mass separator at CERN while sup(20-31)Na and sup(38-47)K have been studied by setting the apparaturs directly on-line with the PS 20 GeV proton beam. The principle of the method is briefly explained and some results concerning nuclear structure are given. (orig.)

  2. Comparison of On-Line Maintenance Support Tools

    International Nuclear Information System (INIS)

    Simic, Z.; Follen, S. M.; Mikulicic, V.

    1998-01-01

    Modeling approach to on-line risk monitoring is today in a rapid developing phase. For that reason number of different solutions are available. This paper will attempt to present existing approaches to address on-line risk modeling problem Starting with description of on-line risk monitoring issues in general, then following by presentation of existing software tools (EPRI's Safety Monitor, Equipment Out of Service Monitor, and ORAM-SENTINEL) the current state of the art in this area will be demonstrated. Finally, conclusions and ideas will be outlined. (author)

  3. CARBON DIOXIDE CAPTURE FROM FLUE GAS USING DRY REGENERABLE SORBENTS

    Energy Technology Data Exchange (ETDEWEB)

    David A. Green; Brian S. Turk; Raghubir P. Gupta; William J. McMichael; Douglas P. Harrison; Ya Liang

    2002-01-01

    The objective of this project is to develop a simple, inexpensive process to separate CO{sub 2} as an essentially pure stream from a fossil fuel combustion system using a regenerable, sodium-based sorbent. The sorbent being used in this project is sodium carbonate which is converted to sodium bicarbonate, or ''baking soda,'' through reaction with carbon dioxide and water vapor. Sodium bicarbonate is regenerated to sodium carbonate when heated, producing a nearly pure CO{sub 2} stream after condensation of water vapor. This quarter, five cycle thermogravimetric tests were conducted at the Louisiana State University (LSU) with sodium bicarbonate Grade 3 (SBC{number_sign}3) which showed that carbonation activity declined slightly over 5 cycles following severe calcination conditions of 200 C in pure CO{sub 2}. Three different sets of calcination conditions were tested. Initial carbonation activity (as measured by extent of reaction in the first 25 minutes) was greatest subsequent to calcination at 120 C in He, slightly less subsequent to calcination in 80% CO{sub 2}/20% H{sub 2}O, and lowest subsequent to calcination in pure CO{sub 2} at 200 C. Differences in the extent of reaction after 150 minutes of carbonation, subsequent to calcination under the same conditions followed the same trend but were less significant. The differences between fractional carbonation under the three calcination conditions declined with increasing cycles. A preliminary fixed bed reactor test was also conducted at LSU. Following calcination, the sorbent removed approximately 19% of the CO{sub 2} in the simulated flue gas. CO{sub 2} evolved during subsequent calcination was consistent with an extent of carbonation of approximately 49%. Following successful testing of SBC{number_sign}3 sorbent at RTI reported in the last quarter, a two cycle fluidized bed reactor test was conducted with trona as the sorbent precursor, which was calcined to sodium carbonate. In the first

  4. CARBON DIOXIDE CAPTURE FROM FLUE GAS USING DRY REGENERABLE SORBENTS

    International Nuclear Information System (INIS)

    David A. Green; Brian S. Turk; Raghubir P. Gupta; William J. McMichael; Douglas P. Harrison; Ya Liang

    2002-01-01

    The objective of this project is to develop a simple, inexpensive process to separate CO(sub 2) as an essentially pure stream from a fossil fuel combustion system using a regenerable, sodium-based sorbent. The sorbent being used in this project is sodium carbonate which is converted to sodium bicarbonate, or ''baking soda,'' through reaction with carbon dioxide and water vapor. Sodium bicarbonate is regenerated to sodium carbonate when heated, producing a nearly pure CO(sub 2) stream after condensation of water vapor. This quarter, five cycle thermogravimetric tests were conducted at the Louisiana State University (LSU) with sodium bicarbonate Grade 3 (SBC(number s ign)3) which showed that carbonation activity declined slightly over 5 cycles following severe calcination conditions of 200 C in pure CO(sub 2). Three different sets of calcination conditions were tested. Initial carbonation activity (as measured by extent of reaction in the first 25 minutes) was greatest subsequent to calcination at 120 C in He, slightly less subsequent to calcination in 80% CO(sub 2)/20% H(sub 2)O, and lowest subsequent to calcination in pure CO(sub 2) at 200 C. Differences in the extent of reaction after 150 minutes of carbonation, subsequent to calcination under the same conditions followed the same trend but were less significant. The differences between fractional carbonation under the three calcination conditions declined with increasing cycles. A preliminary fixed bed reactor test was also conducted at LSU. Following calcination, the sorbent removed approximately 19% of the CO(sub 2) in the simulated flue gas. CO(sub 2) evolved during subsequent calcination was consistent with an extent of carbonation of approximately 49%. Following successful testing of SBC(number s ign)3 sorbent at RTI reported in the last quarter, a two cycle fluidized bed reactor test was conducted with trona as the sorbent precursor, which was calcined to sodium carbonate. In the first carbonation cycle, CO

  5. 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. copyright 2004 Elsevier Ltd.

  6. 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.

  7. IMMOBILIZATION OF MICROALGAE ON THE SURFACE OF NEW CROSS-LINKED POLYETHYLENIMINE-BASED SORBENTS.

    Science.gov (United States)

    Vasilieva, Svetlana; Shibzukhova, Karina; Morozov, Alexey; Solovchenko, Alexei; Bessonov, Ivan; Kopitsyna, Maria; Lukyanov, Alexander; Chekanov, Konstantin; Lobakova, Elena

    2018-04-11

    We report on the use of the polyethylenimine-based (PEI) sorbents for immobilization and harvesting of microalgae (MA) cells. Specific materials assessed were porous solid polymers from highly-branched PEI synthesized by cross-linking with epichlorohydrin (ECH) or diethylene glycol diglycidyl ether (DGDE). We estimated the effect of PEI/cross-linker ratio on the MA attachment and biocompatibility of the sorbents with the MA cells. A decrease in the cross-linker percentage resulted in the enhancement of the immobilization efficiency but impaired the cell viability as was manifested by inhibition of the photosynthetic activity of the MA cells. The rate of Chlorella vulgaris cell attachment to the sorbents with ECH was faster as compared to that of the PEI-DGDE-based polymers. The cells immobilized on the PEI-ECH sorbents showed a more profound decline in their viability (assessed via photosynthetic activity). The sorbents with 60% of DGDE were characterized by high immobilization efficiency. These sorbents supported a prolonged cultivation of the immobilized MA without impairing their viability and metabolic activity. We conclude that the sorbents with a lower percentage of DGDE (<30%) and sorbents with ECH are suitable for harvesting of the MA cells intended for immediate downstream processing, potentially without the cell desorption. To the best of our knowledge, this is the first report on successful application of PEI-based sorbents in microalgal biotechnology. Copyright © 2018 Elsevier B.V. All rights reserved.

  8. 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

    2018-02-01

    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.

  9. Noble metal extraction and sorption concentrating

    International Nuclear Information System (INIS)

    Petrukhin, O.M.; Malofeeva, G.I.

    1985-01-01

    Works performed in the USSR Academy of Sciences GEOCHI laboratory of extraction methods and devoted to selectivity problems of extraction and sorption methods of platinum metal, cadmium and indium concentrating in analytical chemistry are discussed. On choosing complexino. reagent main attention is paid to the selectivity variation based on different stability of metal complexes. Platinum metals are extracted in the form of ion associates when usinq hard, mainly oxyqen-containing, extractants. Coordination-solvated metal complexes are extracted white usinq extractants containing sulfur, trivalent phosphorus and aromatic nitroqen as donor anions. Selectivity is maximum for sulfur- and nitroren-containinq extractants and sorbents. In case of the group extraction of platinum metals sorption is preferable and in case of selective extraction of individual metals, especially, in case of need of relative concentratinq extraction is preferable

  10. On-line methanol sensor system development for recombinant ...

    African Journals Online (AJOL)

    On-line methanol sensor system development for recombinant human serum ... of the methanol sensor system was done in a medium environment with yeast cells ... induction at a low temperature and a pH where protease does not function.

  11. On-line control systems in power plants

    International Nuclear Information System (INIS)

    Freymeyer, P.

    1981-01-01

    This report is a review of on-line control systems as a complex system connected with all problems like, development, planning, degree of automation, economics, service, quality and documentation. (orig.) [de

  12. Why do People Stop Playing On-Line Games?

    DEFF Research Database (Denmark)

    Sudzina, Frantisek; Razmerita, Liana

    2012-01-01

    The recent initial public offering of shares of Zynga, probably the most important on-line game provider, drew interest of potential investors but also of general public to their business model. What the most interested people learned so far is that if Zynga had not changed their accounting...... practice, they would be in red numbers for several months already. This is most likely caused by people stopping to play their games. This paper provides an estimate of what proportion of people, who played on-line games, already stopped playing them. Additionally, it analyzed the reasons why people...... stopped playing on-line games. It also compares Facebook and other on-line games....

  13. The Daresbury On-Line Isotope Separator (DOLIS)

    International Nuclear Information System (INIS)

    Grant, I.S.; Eastham, D.A.; Groves, J.; Tolfree, D.W.L.; Walker, P.M.; Green, V.R.; Rikovska, J.; Stone, N.J.; Hamilton, W.D.

    1987-01-01

    The isotope separator DOLIS, which is on-line to the Daresbury Laboratory's 20-MV tandem accelerator, is used to measure nuclear moments and decay schemes. Separated beams may be collected on a tape and transported to a counting station, implanted directly into a host lattice at on-line temperatures down to less than 10 mK, or allowed to interact with a collinear laser beam. The present status of DOLIS and its ancillary equipment is described

  14. The Daresbury on-line isotope separator (DOLIS)

    International Nuclear Information System (INIS)

    Grant, I.S.; Eastham, D.A.; Groves, J.; Tolfree, D.W.L.; Walker, P.M.; Green, V.R.; Rikovska, J.; Stone, N.J.; Hamilton, W.D.

    1987-01-01

    The isotope separator DOLIS, which is on-line to the Daresbury Laboratory's 20-MV tandem accelerator, is used to measure nuclear moments and decay schemes. Separated beams may be collected on a tape and transported to a counting station, implanted directly into a host lattice at on-line temperatures down to less than 10 mK, or allowed to interact with a collinear laser beam. The present status of DOLIS and its ancillary equipment is described. (orig.)

  15. Considerations in applying on-line IC techniques to BWR's

    International Nuclear Information System (INIS)

    Kaleda, R.J.

    1992-01-01

    Ion-Chromatography (IC) has moved from its traditional role as a laboratory analytical tool to a real time, dynamic, on-line measurement device to follow ppb and sub-ppb concentrations of deleterious impurities in nuclear power plants. Electric Power Research Institute (EPRI), individual utilities, and industry all have played significant roles in effecting the transition. This paper highlights considerations and the evolution in current on-line Ion Chromatography systems. The first applications of on-line techniques were demonstrated by General Electric (GE) under EPRI sponsorship at Rancho Seco (1980), Calvert Cliffs, and McGuire nuclear units. The primary use was for diagnostic purposes. Today the on-line IC applications have been expanded to include process control and routine plant monitoring. Current on-line IC's are innovative in design, promote operational simplicity, are modular for simplified maintenance and repair, and use field-proven components which enhance reliability. Conductivity detection with electronic or chemical suppression and spectrometric detection techniques are intermixed in applications. Remote multi-point sample systems have addressed memory effects. Early applications measured ionic species in the part per billion range. Today reliable part per trillion measurements are common for on-line systems. Current systems are meeting the challenge of EPRI guideline requirements. Today's on-line IC's, with programmed sampling systems, monitor fluid streams throughout a power plant, supplying data that can be trended, stored and retrieved easily. The on-line IC has come of age. Many technical challenges were overcome to achieve today's IC

  16. On-line mixture-based alternative to logistic regression

    Czech Academy of Sciences Publication Activity Database

    Nagy, Ivan; Suzdaleva, Evgenia

    2016-01-01

    Roč. 26, č. 5 (2016), s. 417-437 ISSN 1210-0552 R&D Projects: GA ČR GA15-03564S Institutional support: RVO:67985556 Keywords : on-line modeling * on-line logistic regression * recursive mixture estimation * data dependent pointer Subject RIV: BB - Applied Statistics, Operational Research Impact factor: 0.394, year: 2016 http://library.utia.cas.cz/separaty/2016/ZS/suzdaleva-0464463.pdf

  17. Unattended reaction monitoring using an automated microfluidic sampler and on-line liquid chromatography.

    Science.gov (United States)

    Patel, Darshan C; Lyu, Yaqi Fara; Gandarilla, Jorge; Doherty, Steve

    2018-04-03

    In-process sampling and analysis is an important aspect of monitoring kinetic profiles and impurity formation or rejection, both in development and during commercial manufacturing. In pharmaceutical process development, the technology of choice for a substantial portion of this analysis is high-performance liquid chromatography (HPLC). Traditionally, the sample extraction and preparation for reaction characterization have been performed manually. This can be time consuming, laborious, and impractical for long processes. Depending on the complexity of the sample preparation, there can be variability introduced by different analysts, and in some cases, the integrity of the sample can be compromised during handling. While there are commercial instruments available for on-line monitoring with HPLC, they lack capabilities in many key areas. Some do not provide integration of the sampling and analysis, while others afford limited flexibility in sample preparation. The current offerings provide a limited number of unit operations available for sample processing and no option for workflow customizability. This work describes development of a microfluidic automated program (MAP) which fully automates the sample extraction, manipulation, and on-line LC analysis. The flexible system is controlled using an intuitive Microsoft Excel based user interface. The autonomous system is capable of unattended reaction monitoring that allows flexible unit operations and workflow customization to enable complex operations and on-line sample preparation. The automated system is shown to offer advantages over manual approaches in key areas while providing consistent and reproducible in-process data. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Determination of antibiotic compounds in water by on-line SPE-LC/MSD.

    Science.gov (United States)

    Choi, Keun-Joo; Kim, Sang-Goo; Kim, Chang-won; Kim, Seung-Hyun

    2007-01-01

    This study attempts to provide an improved approach for the analysis of antibiotics, which normally exist at low concentration in complex matrices such as receiving streams of wastewater treatment plant discharge. The analytical method developed in this study combines an existing pretreatment technique of solid-phase extraction (SPE) with liquid chromatography mass spectrometry (LC/MSD) through on-line connection. The on-line connection suppressed the target loss by keeping the cartridge from drying, which resulted in improvement of the recovery and saving of the analytical time. For the on-line solid-phase extraction of 10 ml water samples, recoveries were between 74.3% and 116.5% and average LOQ was 0.11 microg l(-1) for the sulfonamide antibiotics (SA) and 0.09 microg l(-1) for the tetracycline antibiotics (TA). Application of the developed method for the analysis of fourteen antibiotics revealed that several antibiotics were detected at concentrations above the LOQ in ARW. Treated and untreated sewage and agricultural wastewater were mostly responsible for the antibiotics contamination of the river. Antibiotics were detected at much higher concentrations in the agricultural wastewater sample than in the sewage sample, implying substantial use of antibiotics in the agricultural industry. Wastewater treatment was generally effective in separation of the antibiotics tested in this study. The extent of the treatment depended on the type of antibiotics. Hydrophobic antibiotics were more effectively separated from the solution than hydrophilic antibiotics.

  19. Development of composite calcium hydroxide sorbent in mechanical operations and evaluation of its basic sorption properties

    Directory of Open Access Journals (Sweden)

    Gara Paweł

    2017-01-01

    Full Text Available This article presents the results of research carried out on the possibility of obtaining composite calcium hydroxide sorbent in the process of two-step granulation, containing additional compounds of Al, Mg and Fe, and their textural and sorption studies. For this purpose, attempts were undertaken to compact commercial calcium hydroxide powder with six additives in the laboratory roll press. The resulting compacts were crushed and sieved in order to achieve the assumed sieve fraction. Based on the obtained results, basic parameters of the process of formation of composite sorbent have been determined. Both, the selected composite sorbents fractions and additives were subsequently subjected to textural studies (determination of the specific surface area and porosity and sorption capacity performance. In addition, for the better interpretation of the results, thermogravimetric studies were carried out both for the additives and composite sorbents, as well as the grain size distribution of the additives. The results of the physicochemical tests of the obtained composite sorbents were compared with analogic results from the study on fine-grained hydroxide sorbent without additives and carbonate sorbent. The presented results showed that in a two-step granulation process it is possible to obtain the granular Ca(OH2 sorbent, as well as composite sorbents possessing better SO2 sorption capacity in comparison to the powder Ca(OH2 and/or to the calcium carbonate sorbent. This can be attributed to the combination of capability of the sorbent to appropriate thermal decomposition and the formation of a group of pores in the range of 0.07-0.3 microns.

  20. Volume overload cleanup: An approach for on-line SPE-GC, GPC-GC, and GPC-SPE-GC

    NARCIS (Netherlands)

    Kerkdijk, H.; Mol, H.G.J.; Nagel, B. van der

    2007-01-01

    A new concept for cleanup, based on volume overloading of the cleanup column, has been developed for on-line coupling of gel permeation chromatography (GPC), solid-phase extraction (SPE), or both, to gas chromatography (GC). The principle is outlined and the applicability demonstrated by the

  1. On-Line/At-Line Technetium Monitor Using Scintillating Ion Exchange Resins for the Savannah River Site

    International Nuclear Information System (INIS)

    Wach, S.T.

    2000-01-01

    The results of this study indicate that the combination of extraction chromatography and on-line flow-cell scintillation counting can exceed a 99Tc detection limit of 0.005 Ci/mL in the presence of 90Sr, 137Cs, and 239Pu in less than an 18 minute analysis time

  2. 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 nano-molar quantification in few seconds, in addition to an accelerated extraction-free GC-MS method that through automation can deliver results much faster than other similar methods. The implementation of these high tech methods will provide the meat industry with a leading edge not only with product...... 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...

  3. On-line monitoring of fluid bed granulation by photometric imaging.

    Science.gov (United States)

    Soppela, Ira; Antikainen, Osmo; Sandler, Niklas; Yliruusi, Jouko

    2014-11-01

    This paper introduces and discusses a photometric surface imaging approach for on-line monitoring of fluid bed granulation. Five granule batches consisting of paracetamol and varying amounts of lactose and microcrystalline cellulose were manufactured with an instrumented fluid bed granulator. Photometric images and NIR spectra were continuously captured on-line and particle size information was extracted from them. Also key process parameters were recorded. The images provided direct real-time information on the growth, attrition and packing behaviour of the batches. Moreover, decreasing image brightness in the drying phase was found to indicate granule drying. The changes observed in the image data were also linked to the moisture and temperature profiles of the processes. Combined with complementary process analytical tools, photometric imaging opens up possibilities for improved real-time evaluation fluid bed granulation. Furthermore, images can give valuable insight into the behaviour of excipients or formulations during product development. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. FURNACE INJECTION OF ALKALINE SORBENTS FOR SULFURIC ACID REMOVAL

    Energy Technology Data Exchange (ETDEWEB)

    Gary M. Blythe

    2004-01-01

    The objective of this project has been to demonstrate the use of alkaline reagents injected into the furnace of coal-fired boilers as a means of controlling sulfuric acid emissions. The project was co-funded by the U.S. DOE National Energy Technology Laboratory under Cooperative Agreement DE-FC26-99FT40718, along with EPRI, the American Electric Power Company (AEP), FirstEnergy Corporation, the Tennessee Valley Authority, and Carmeuse North America. Sulfuric acid controls are becoming of increased interest for coal-fired power generating units for a number of reasons. In particular, sulfuric acid can cause plant operation problems such as air heater plugging and fouling, back-end corrosion, and plume opacity. These issues will likely be exacerbated with the retrofit of selective catalytic reduction (SCR) for NOX control, as SCR catalysts are known to further oxidize a portion of the flue gas SO{sub 2} to SO{sub 3}. The project tested the effectiveness of furnace injection of four different magnesium-based or dolomitic alkaline sorbents on full-scale utility boilers. These reagents were tested during one- to two-week tests conducted on two FirstEnergy Bruce Mansfield Plant (BMP) units. One of the sorbents tested was a magnesium hydroxide slurry byproduct from a modified Thiosorbic{reg_sign} Lime wet flue gas desulfurization process. The other three sorbents are available commercially and include dolomite, pressure-hydrated dolomitic lime, and commercially available magnesium hydroxide. The dolomite reagent was injected as a dry powder through out-of-service burners. The other three reagents were injected as slurries through air-atomizing nozzles inserted through the front wall of the upper furnace. After completing the four one- to two-week tests, the most promising sorbents were selected for longer-term (approximately 25-day) full-scale tests on two different units. The longer-term tests were conducted to confirm sorbent effectiveness over extended operation on two

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

    Science.gov (United States)

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

    2013-05-01

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

  6. The spectroscopic study of building composites containing natural sorbents.

    Science.gov (United States)

    Król, M; Mozgawa, W

    2011-08-15

    This work presents the results of FT-IR spectroscopic studies of heavy metal cations (Ag(+), Pb(2+), Zn(2+), Cd(2+) and Cr(3+)) immobilization from aqueous solutions on natural sorbents. The sorption has been conducted on sodium forms of zeolite (clinoptilolite) and clay minerals (mixtures containing mainly montmorillonite and kaolinite) which have been separated from natural Polish deposit. In the next part of the work both sorbents were used to obtain new building composites. It was proven those heavy metal cations' sorption causes changes in IR spectra of the zeolite and clay minerals. These alterations are dependent on the way the cations were sorbed. In the case of zeolite, variations of the bands corresponding to the characteristic ring vibrations have been observed. These rings occur in pseudomolecular complexes 4-4-1 (built of alumino- and silicooxygen tetrahedra) which constitute the secondary building units (SBU) and form spatial framework of the zeolite. The most significant changes have been determined in the region of pseudolattice vibrations (650-700 cm(-1)). In the instance of clay minerals, changes in the spectra occur at two ranges: 1200-800 cm(-1)--the range of the bands assigned to asymmetric Si-O(Si,Al) and bending Al-OH vibrations and 3800-3000 cm(-1)--the range of the bands originating from OH(-) groups stretching vibrations. Next results indicate possibilities of applying the used natural sorbents for the obtainment of new building materials having favourable composition and valuable properties. The zeolite was used for obtaining autoclaved materials with an addition of CaO, and the clay minerals for ceramic sintered materials with an addition of quartz and clinoptilolite were produced. FT-IR studies were also conducted on the obtained materials. Copyright © 2010 Elsevier B.V. All rights reserved.

  7. The Efficient Extraction of Phenolic Compounds from Oak Gall Using a Miniaturized Matrix Solid-Phase Dispersion Method before their HPLC Determination

    Directory of Open Access Journals (Sweden)

    Ahmad Daneshfar

    2017-06-01

    Conclusion: The proposed technique is simple and fast. It substantially reduced the amounts of sample, sorbent and organic solvents required for the extraction. The maximum amounts of the phenolic compounds were found in Qalqaf and Bramazu galls.

  8. Microwave synthesis of nanostructured oxide sorbents doped with lanthanides

    Energy Technology Data Exchange (ETDEWEB)

    Mitrofanov, Andrey A., E-mail: mitrofanov-a@icloud.com; Silyavka, Elena S.; Shilovskikh, Vladimir V.; Kolonitckii, Petr D.; Sukhodolov, Nikolai G.; Selyutin, Artem A., E-mail: selutin@inbox.ru [Saint Petersburg State University, 7/9, Universitetskaya nab., St. Petersburg, 199034 (Russian Federation)

    2016-06-17

    A number of nanostructured mesoporous oxide systems based on aluminum oxide, doped with lanthanide ions have been obtained in this study. Structure and morphology of oxides obtained have been examined by X-ray diffraction analysis, thermogravimetric analysis, scanning electron microscopy. The surface area of the samples was determined by the BET method. The dependence of the adsorption of insulin on synthesized oxides from the concentration was investigated. The containing of insulin in solutions after adsorption was determined by the Bradford method. The isotherms of adsorption of insulin on resulting oxide sorbents were plotted, the dependence capacity of the sorption of insulin from the lanthanide dopant was determined.

  9. Durable zinc oxide-containing sorbents for coal gas desulfurization

    Science.gov (United States)

    Siriwardane, Ranjani V.

    1996-01-01

    Durable zinc-oxide containing sorbent pellets for removing hydrogen sulfide from a gas stream at an elevated temperature are made up to contain titania as a diluent, high-surface-area silica gel, and a binder. These materials are mixed, moistened, and formed into pellets, which are then dried and calcined. The resulting pellets undergo repeated cycles of sulfidation and regeneration without loss of reactivity and without mechanical degradation. Regeneration of the pellets is carried out by contacting the bed with an oxidizing gas mixture.

  10. The use of clays as sorbents and catalysts

    International Nuclear Information System (INIS)

    McCabe, R.W.

    1998-01-01

    The paper attempts to show the structural, physical and chemical properties of clay minerals relate to their laboratory, industrial and environmental uses as sorbents and catalysts. A brief review of the formulae and structures of clays and their relationship to their chemical and physical properties follows. Clay minerals are also useful in environmental protection as they can adsorb crude oils from spills and they are used, sometimes mixed into concrete, as containment barriers for radionuclides caesium 137 and strontium 90. Clay soils can also act as natural barriers to the migration of radionuclides in the environment

  11. SORBENT/UREA SLURRY INJECTION FOR SIMULTANEOUS SO2/NOX REMOVAL

    Science.gov (United States)

    The combination of sorbent injection and selective noncatalytic reduction (SNCR) technologies has been investigated for simulataneous SO2/NOx removal. A slurry composed of a urea-based solution and various Ca-based sorbents was injected at a range of tempera...

  12. Adsorption of H2O and CO2 on supported amine sorbents

    NARCIS (Netherlands)

    Veneman, Rens; Frigka, Natalia; Zhao, Wenying; Li, Zhenshan; Kersten, Sascha R.A.; Brilman, Derk Willem Frederik

    2015-01-01

    In this work the adsorption of H2O and CO2 on Lewatit VP OC 1065 was studied in view of the potential application of this sorbent in post combustion CO2 capture. Both CO2 and H2O were found to adsorb on the amine active sites present on the pore surface of the sorbent material. However, where the

  13. Synthesis of hydroxide type sorbents from industry high-iron wastes

    International Nuclear Information System (INIS)

    Stepanenko, E.K.; Smirnov, A.L.

    1986-01-01

    Article presents the results of studies on possibility of using of technological iron containing wastes for the obtaining of hydroxide type sorbents in granular form. The scheme of technology of synthesis of hydroxide type sorbents from high-iron wastes is elaborated.

  14. Evaluation of hydrous ferric oxide loaded activated carbon as a granular composite sorbent for radiostrontium

    International Nuclear Information System (INIS)

    Samanta, S.K.

    1997-01-01

    A composite sorbent was prepared in granular form by depositing hydrous ferric oxide inside the pores of activated carbon. The composite sorbent was found to show excellent sorption of radiostrontium in the presence of high sodium concentration under alkaline conditions. (author). 3 refs., 2 figs., 1 tab

  15. Coating membranes for a sorbent-based artificial liver: adsorption characteristics

    NARCIS (Netherlands)

    de Koning, H. W.; Chamuleau, R. A.; Bantjes, A.

    1982-01-01

    Techniques are described for the coating of sorbents to be used in an artificial liver support system based on mixed sorbent bed hemoperfusion. Activated charcoal has been coated with cellulose acetate (CA) by solvent evaporation. With Amberlite XAD-4, the Wurster technique was used for coating with

  16. Cross-linked poly(tetrahydrofuran) as promising sorbent for organic solvent/oil spill

    Energy Technology Data Exchange (ETDEWEB)

    Yati, Ilker; Ozan Aydin, Gulsah; Bulbul Sonmez, Hayal, E-mail: hayalsonmez@gtu.edu.tr

    2016-05-15

    Highlights: • Poly(tetrahydrofuran) based sorbents were prepared. • PTHF sorbents demonstrate reusability at least for ten times. • PTHF based sorbents show fast and quick absorption-desorption process. • 19 g of oil can be absorbed by 1 g of PTHF based sorbent. - Abstract: In this study, a series of different molecular weights of poly(tetrahydrofuran) (PTHF), which is one of the most important commercial polymers around the world, was condensed with tris[3-(trimethoxysilyl)propyl]isocyanurate (ICS) to generate a cross-linked 3-dimensional network in order to obtain organic solvent/oil sorbents having high swelling capacity. The prepared sorbents show high and fast swelling capacity in oils such as dichloromethane (DCM), tetrahydrofuran (THF), acetone, t-butyl methyl ether (MTBE), gasoline, euro diesel, and crude oil. The recovery of the absorbed oils from contaminated surfaces, especially from water, and the regeneration of the sorbents after several applications are effective. The characterization and thermal properties of the sorbents are identified by Fourier transform infrared spectroscopy (FTIR), solid-state {sup 13}C and {sup 29}Si cross-polarization magic angle spinning (CPMAS) nuclear magnetic resonance (NMR), differential scanning calorimetry (DSC) and thermal gravimetric analyses (TGA), respectively. The new usage area of PTHF is emerged by the preparation of PTHF-based network structure with high oil absorption capacity and having excellent reusability as an oil absorbent for the removal of organic liquids from the spill site.

  17. Synthesis and test of sorbents based on calcium aluminates for SE-SR

    International Nuclear Information System (INIS)

    Barelli, L.; Bidini, G.; Di Michele, A.; Gallorini, F.; Petrillo, C.; Sacchetti, F.

    2014-01-01

    Highlights: • Synthesis strategy of CaO incorporation into calcium aluminates was approached. • Three innovative sorbents (M1, M2, M3) were synthesized and characterized. • Sorption capacity of developed sorbents was evaluated in multi-cycle processes. • M3 sorbent showed best performance, much higher than conventional CaO ones. • M3 sorbent functionality in SE-SR process was verified. - Abstract: Greenhouse gases emission of power generation plants will be continuously tightened to achieve European targets in terms of CO 2 emissions. In particular, the switching to a sustainable power generation using fossil fuels will be strongly encouraged in the future. In this context, sorption-enhanced steam reforming (SE-SR) is a promising process because it can be implemented as a CCS pre-combustion methodology. The purpose of this study is to develop and test innovative materials in order to overcome main limitations of standard CaO sorbent, usually used in the SE-SR process. The investigated innovative sorbents are based on incorporation of CaO particles into inert materials which significantly reduce the performance degradation. In particular, sorbent materials based on calcium aluminates were considered, investigating different techniques of synthesis. All synthesized materials were packed, together with the catalyst, in a fixed bed reactor and tested in sorption/regeneration cycles. Significant improvements were obtained respect to standard CaO regarding sorption capacity stability exhibited by the sorbent

  18. Development of New Potassium Carbonate Sorbent for CO2 Capture under Real Flue Gas Conditions

    Directory of Open Access Journals (Sweden)

    Javad Esmaili

    2014-07-01

    Full Text Available In this paper, the development of a new potassium carbonateon alumina support sorbent prepared by impregnating K2CO3 with an industrial grade of Al2O3 support was investigated. The CO2 capture capacity was measured using real flue gas with 8% CO2 and 12% H2O in a fixed-bed reactor at a temperature of 65 °C using breakthrough curves. The developed sorbent showed an adsorption capacity of 66.2 mgCO2/(gr sorbent. The stability of sorbent capture capacity was higher than the reference sorbent. The SO2 impurity decreased sorbent capacity about 10%. The free carbon had a small effect on sorbent capacity after 5 cycles. After 5 cycles of adsorption and regeneration, the changes in the pore volume and surface area were 0.020 cm3/gr and 5.5 m2/gr respectively. Small changes occurred in the pore size distribution and surface area of sorbent after 5 cycles.

  19. Molecularly imprinted polymer cartridges coupled on-line with high performance liquid chromatography for simple and rapid analysis of dextromethorphan in human plasma samples.

    Science.gov (United States)

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

    2011-04-01

    In this paper, a novel method is described for automated determination of dextromethorphan in biological fluids using molecularly imprinted solid-phase extraction (MISPE) 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 functional monomer, ethylene glycol dimethacrylate as cross-linker, chloroform as porogen and dextromethorphan as template molecule. These imprinted polymers were used as solid-phase extraction sorbent for the extraction of dextromethorphan from human plasma samples. Various parameters affecting the extraction efficiency of the MIP cartridges were evaluated. The high selectivity of the sorbent coupled to the high performance liquid chromatographic system permitted a simple and rapid analysis of this drug in plasma samples with limits of detection (LOD) and quantification (LOQ) of 0.12 ng/mL and 0.35 ng/mL, respectively. The MIP selectivity was evaluated by analyzing of the dextromethorphan in presence of several substances with similar molecular structures and properties. Results from the HPLC analyses showed that the recoveries of dextromethorphan using MIP cartridges from human plasma samples in the range of 1-50 ng/mL were higher than 87%. Copyright © 2011 Elsevier B.V. All rights reserved.

  20. On-line maintenance PSA support at NPP Krsko

    International Nuclear Information System (INIS)

    Prosen, R.; Vrbanic, I.; Kastelan, M.

    2000-01-01

    In 1997 Krsko NPP initiated the on-line maintenance (OLM) practice. On-line maintenance constitutes of corrective activities, preventive activities, surveillance activities, tests and inspections, as well as calibrations and modifications, taking place during the normal power operations. The on-line maintenance is a multidisciplinary process consisting of activity specification, planning, and preparation and performing of the OLM activity of interest. The primary role of the PSA group is to assess from the r isk perspective , using the plant-specific NEK PSA model, system unavailability and the impact to the plant operational risk. The intent is to support planning of the on-line maintenance activities from the risk perspective. The risk evaluation of the OLM activities is based on the probability of core damage evaluation for the defined discrete plant configuration states, determined by the OLM activities. Within this application, the optimized, plant-specific PSA model is used on Risk Spectrum platform. To perform the risk assessment of the on-line maintenance activities, first the systems to be affected are defined based on the planned OLM activities. The next important step is the assessment of the planned work schedule. To define the final schedule, the co-ordination and optimizing the planned OLM activities needs activation of all participating departments, supported also from PSA group. The P3 (i.e. Primavera) planning tool system windows are defined for different systems and groups of systems, and the activities are sorted in particular weeks according to these windows. (author)

  1. OLDASS: On-line data acquisition system at SF cyclotron

    International Nuclear Information System (INIS)

    Omata, Kazuo; Yasue, Masaharu; Hamagaki, Hideki

    1982-01-01

    The on-line data acquisition system in the Institute for Nuclear Study, the University of Tokyo, is composed of 2 systems of Fujitsu mini-computer PFU-400 for data processing at the high energy synchrotron and one system of that computer for low energy cyclotron as terminals, the host computer being M 180 II AD of the same company. This system has been developed to have the features of being the on-line system capable of following the improvement of host computer performance, being capable of developing the on-line programmes of other experimenting groups in parallel with batch jobs or the operation of the on-line system, and capable of developing programmes using FORTRAN. The result of about 220 KB/s was obtained for the data transfer rate between the programmes of the host computer and terminals, and this fulfilled the aimed performance. The terminal system on the low energy side is provided with an ADC interface and a display interface specified particularly in addition to the miniature computer PFU400 and standard I/O devices of the manufacture. The accumulating type graphic display of the I/O devices can be switched to be connected to the host computer, and immediately displays the results transferred to the host computer and analyzed. Hard copy is also available. The above hardware and software are explained. The on-line system insures 80 K bytes of the total memory of 224 K bytes for data area. (Wakatsuki, Y.)

  2. Sport Management Taught On-Line: A Discussion

    Directory of Open Access Journals (Sweden)

    William F. Stier Jr

    2009-01-01

    Full Text Available An introduction to the world of on-line courses (distance education/learning is presented. In addition, the world of on-line learning, as it pertains to sport management, is examined within the framework of (a pedagogy, (b finances,(c assessment, and (d choosing to transition from the traditional classroom to on-line learning. Pertinent points relative to each of the four categories are presented from the literature. In an effort to stimulate thought and discussion to the subject of on-line learning for sport management programs/courses the authors provide their reactions to the literature points by presenting their comments/reactions from a sport management perspective. Sport management professors and administrators are encouraged to critically examine the feasibility of such on-line courses (distance education/learning within their own curricula while maintaining an appropriate framework revolving around sound theoretical instructional strategies, methods as well as appropriate use of instructional tools, including but not limited to, computersand the WWW.

  3. Effect of characteristic of sorbents on their sulfur capture capability at a fluidized bed condition

    Energy Technology Data Exchange (ETDEWEB)

    Leming Cheng; Bo Chen; Ni Liu; Zhongyang Luo; Kefa Cen [Zhejiang University, Hangzhou (China). Clean Energy and Environment Engineering Key Lab of Ministry of Education, Institute for Thermal Power Engineering

    2004-05-01

    This research was intent for finding relationships among physical and/or chemical properties of sorbents and their sulfur capture capability at a fluidized bed condition. Three limestones and two seashells were chosen as a SO{sub 2} sorbent. Characteristics of sorbents were evaluated based on atomic absorption spectrophotometer, scanning electron microscope and mercury-penetration porosimeter analyses. Their sulfur capture capabilities were measured on a fluidized bed test system at 800, 850, 900 and 950{sup o}C. Conversion of the sobents was computed and analyzed depending on the sorbents' morphology and microstructure analysis. Results showed pore size and specific surface might have large influence on sorbents' desulfurization ability in the range of 800 950{sup o}C. 14 refs., 6 figs., 4 tabs.

  4. Experimental research on combustion fluorine retention using calcium-based sorbents during coal combustion (II)

    Energy Technology Data Exchange (ETDEWEB)

    Qi, Q.; Ma, X.; Liu, J.; Wu, X.; Zhou, J.; Cen, K. [Liaoning Technical University, Fuxin (China). College of Resource and Environment Engineering

    2008-12-15

    Fluoride pollution produced by coal burning can be controlled with the calcium-based sorbent combustion fluorine technique in which calcium-based sorbents are mixed with the coal or sprayed into the combustion chamber. In a fixed bed tube furnace combustion experiment using one calcium-based natural mineral, limestone and one calcium-based building material, it was shown that the calcium-based sorbent particle grain size and pore structure have a big influence on the combustion fluorine retention effect. Reducing the calcium-based sorbent particle grain size and improving the calcium sorbent structure characteristics at very high temperature to enhance the fluorine retention effect is the important approach to the fluorine retention agent development. 8 refs., 1 fig., 5 tabs.

  5. Preparation and characterisation of a sorbent suitable for technetium separation from environmental matrices

    International Nuclear Information System (INIS)

    Bartosova, A.; Rajec, P.; Reich, M.

    2003-01-01

    A sorbent based on Aliquat 336 anchored on hydrophobised silica gel support as an ion exchanger was prepared. Prepared sorbent was suitable for separation of technetium-99 from environmental matrices. The sorbent properties, sorption characteristic and distribution coefficient of 99 mTcO 4 - in various medium was studied. The chemical yield of Tc during separation process was determined using 99m Tc tracer and gamma measurement. Typical sorption recoveries of Tc for this sorbent from 0.1 M HNO 3 were more than 98 %. Typical desorption recoveries using 8 M HNO 3 were in the range 92 - 96 %. The commercial TEVA Spec resin from Eichrom Industries for comparison purpose was used as well. It was found that the prepared sorbent is suitable for separation of technetium from environmental matrices. (authors)

  6. [Applications and prospects of on-line near infrared spectroscopy technology in manufacturing of Chinese materia medica].

    Science.gov (United States)

    Li, Yang; Wu, Zhi-Sheng; Pan, Xiao-Ning; Shi, Xin-Yuan; Guo, Ming-Ye; Xu, Bing; Qiao, Yan-Jiang

    2014-10-01

    The quality of Chinese materia medica (CMM) is affected by every process in CMM manufacturing. According to multi-unit complex features in the production of CMM, on-line near infrared spectroscopy (NIR) is used as an evaluating technology with its rapid, non-destructive and non-pollution etc. advantages. With the research in institutions, the on-line NIR applied in process analysis and control of CMM was described systematically, and the on-line NIR platform building was used as an example to clarify the feasibility of on-line NIR technology in CMM manufacturing process. Then, from the point of application by pharmaceutical companies, the current on-line NIR research on CMM and its production in pharmaceutical companies was relatively comprehensively summarized. Meanwhile, the types of CMM productions were classified in accordance with two formulations (liquid and solid dosage formulations). The different production processes (extraction, concentration and alcohol precipitation, etc. ) were used as liquid formulation diacritical points; the different types (tablets, capsules and plasters, etc.) were used as solid dosage formulation diacritical points, and the reliability of on-line NIR used in the whole process in CMM production was proved in according to the summary of literatures in recent 10 years, which could support the modernization of CMM production.

  7. Initiating Events Modeling for On-Line Risk Monitoring Application

    International Nuclear Information System (INIS)

    Simic, Z.; Mikulicic, V.

    1998-01-01

    In order to make on-line risk monitoring application of Probabilistic Risk Assessment more complete and realistic, a special attention need to be dedicated to initiating events modeling. Two different issues are of special importance: one is how to model initiating events frequency according to current plant configuration (equipment alignment and out of service status) and operating condition (weather and various activities), and the second is how to preserve dependencies between initiating events model and rest of PRA model. First, the paper will discuss how initiating events can be treated in on-line risk monitoring application. Second, practical example of ini