Determination of scandium in acid mine drainage by ICP-OES with flow injection on-line preconcentration using oxidized multiwalled carbon nanotubes.

Science.gov (United States)

Jerez, Javier; Isaguirre, Andrea C; Bazán, Cristian; Martinez, Luis D; Cerutti, Soledad

2014-06-01

An on-line scandium preconcentration and determination system implemented with inductively coupled plasma optical emission spectrometry associated with flow injection was studied. Trace amounts of scandium were preconcentrated by sorption on a minicolumn packed with oxidized multiwalled carbon nanotubes, at pH 1.5. The retained analyte was removed from the minicolumn with 30% (v/v) nitric acid. A total enrichment factor of 225-fold was obtained within a preconcentration time of 300 s (for a 25 mL sample volume). The overall time required for preconcentration and elution of 25 mL of sample was about 6 min; the throughput was about 10 samples per hour. The value of the detection limit was 4 ng L(-1) and the precision for 10 replicate determinations at 100 ng L(-1) Sc level was 5% relative standard deviation, calculated from the peak heights obtained. The calibration graph using the preconcentration system was linear with a correlation coefficient of 0.9996 at levels near the detection limits up to at least 10 mg L(-1). After optimization, the method was successfully applied to the determination of Sc in an acid drainage from an abandoned mine located in the province of San Luis, Argentina. Copyright © 2014 Elsevier B.V. All rights reserved.

Progress in metal ion separation and preconcentration: an overview

International Nuclear Information System (INIS)

Bond, A. H.

1998-01-01

A brief historical perspective covering the most mature chemically-based metal ion separation methods is presented, as is a summary of the recommendations made in the 1987 National Research Council (NRC) report entitled ''Separation and Purification: Critical Needs and Opportunities''. A review of Progress in Metal Ion Separation and Preconcentration shows that advances are occurring in each area of need cited by the NRC. Following an explanation of the objectives and general organization of this book, the contents of each chapter are briefly summarized and some future research opportunities in metal ion separations are presented

Development and application of an on-line sequential injection system for the separation of artificial and natural radionuclides in environmental samples

International Nuclear Information System (INIS)

Kim, C.-K.; Sansone, U.; Martin, P.; Kim, C.-S.

2007-02-01

The Chemistry Unit of the Physics, Chemistry and Instrumentation Laboratory in the IAEA's Seibersdorf Laboratory in Austria, has the programmatic responsibility to provide assistance to Member State laboratories in maintaining and improving the reliability of analytical measurement results, both in trace element and radionuclide determinations. This is accomplished through the provision of reference materials of terrestrial origin, validated analytical procedures, training in the implementation of internal quality control, and through the evaluation of measurement performance by organization of worldwide and regional interlaboratory comparison exercises. In this framework an on-line sequential injection (SI) system was developed, which can be widely used for the separation and preconcentration of target analytes from diverse environmental samples. The system enables the separation time to be shortened by maintaining a constant flow rate of solution and by avoiding clogging or bubbling in a chromatographic column. The SI system was successfully applied to the separation of Pu in IAEA reference material (IAEA Soil-6) and to the sequential separation of 210 Po and 210 Pb in phosphogypsum candidate reference material. The replicate analysis results of Pu in IAEA reference material (Soil-6) obtained with the SI system are in good agreement with the recommended value within 5% of standard deviation. The SI system enabled a halving in the separation time required for of radionuclides

On-line preconcentration and determination of chromium in parenteral solutions by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Gil, R.A.; Cerutti, S.; Gasquez, J.A.; Olsina, R.A.; Martinez, L.D.

2005-01-01

A method for the preconcentration and speciation of chromium was developed. On-line preconcentration and determination were obtained using inductively coupled plasma optical emission spectrometry (ICP-OES) coupled with flow injection. To determinate the chromium (III) present in parenteral solutions, chromium was retained on activated carbon at pH 5.0. On the other hand, a step of reduction was necessary in order to determine total chromium content. The Cr(VI) concentration was then determined by difference between the total chromium concentration and that of Cr(III). A sensitivity enrichment factor of 70-fold was obtained with respect to the chromium determination by ICP-OES without preconcentration. The detection limit for the preconcentration of 25 ml of sample was 29 ng l -1 . The precision for the 10 replicate determinations at the 5 μg l -1 Cr level was 2.3% relative standard deviation, calculated with the peak heights. The calibration graph using the preconcentration method for chromium species was linear with a correlation coefficient of 0.9995 at levels near the detection limits up to at least 60 μg l -1 . The method can be applied to the determination and speciation of chromium in parenteral solutions

Flow injection on-line preconcentration of low levels of Cr(VI) with detection by ETAAS

DEFF Research Database (Denmark)

Som-aum, Waraporn; Liawruangrath, Saisunee; Hansen, Elo Harald

2002-01-01

A flow injection (FI) on-line sorption preconcentration procedure utilizing a packed column reactor and combined with electrothermal atomic absorption spectrometry (ETAAS) is proposed for the determination of low levels of Cr(VI) in water samples. Polytetrafluoroethylene (PTFE) beads packed in a ...

Progress in metal ion separation and preconcentration : an overview.

Energy Technology Data Exchange (ETDEWEB)

Bond, A. H.

1998-05-19

A brief historical perspective covering the most mature chemically-based metal ion separation methods is presented, as is a summary of the recommendations made in the 1987 National Research Council (NRC) report entitled ''Separation and Purification: Critical Needs and Opportunities''. A review of Progress in Metal Ion Separation and Preconcentration shows that advances are occurring in each area of need cited by the NRC. Following an explanation of the objectives and general organization of this book, the contents of each chapter are briefly summarized and some future research opportunities in metal ion separations are presented.

An off-line automated preconcentration system with ethylenediaminetriacetate chelating resin for the determination of trace metals in seawater by high-resolution inductively coupled plasma mass spectrometry.

Science.gov (United States)

Minami, Tomoharu; Konagaya, Wataru; Zheng, Linjie; Takano, Shotaro; Sasaki, Masanobu; Murata, Rena; Nakaguchi, Yuzuru; Sohrin, Yoshiki

2015-01-07

A novel automated off-line preconcentration system for trace metals (Al, Mn, Fe, Co, Ni, Cu, Zn, Cd, and Pb) in seawater was developed by improving a commercially available solid-phase extraction system SPE-100 (Hiranuma Sangyo). The utilized chelating resin was NOBIAS Chelate-PA1 (Hitachi High-Technologies) with ethylenediaminetriacetic acid and iminodiacetic acid functional groups. Parts of the 8-way valve made of alumina and zirconia in the original SPE-100 system were replaced with parts made of polychlorotrifluoroethylene in order to reduce contamination of trace metals. The eluent pass was altered for the back flush elution of trace metals. We optimized the cleaning procedures for the chelating resin column and flow lines of the preconcentration system, and developed a preconcentration procedure, which required less labor and led to a superior performance compared to manual preconcentration (Sohrin et al.). The nine trace metals were simultaneously and quantitatively preconcentrated from ∼120 g of seawater, eluted with ∼15 g of 1M HNO3, and determined by HR-ICP-MS using the calibration curve method. The single-step preconcentration removed more than 99.998% of Na, K, Mg, Ca, and Sr from seawater. The procedural blanks and detection limits were lower than the lowest concentrations in seawater for Mn, Ni, Cu, and Pb, while they were as low as the lowest concentrations in seawater for Al, Fe, Co, Zn, and Cd. The accuracy and precision of this method were confirmed by the analysis of reference seawater samples (CASS-5, NASS-5, GEOTRACES GS, and GD) and seawater samples for vertical distribution in the western North Pacific Ocean. Copyright © 2014 Elsevier B.V. All rights reserved.

Preconcentration and Separation of Mixed-Species Samples Near a Nano-Junction in a Convergent Microchannel

Directory of Open Access Journals (Sweden)

Ping-Hsien Chiu

2015-12-01

Full Text Available A fluidic microchip incorporating a convergent microchannel and a Nafion-nanoporous membrane is proposed for the preconcentration and separation of multi-species samples on a single platform. In the device, sample preconcentration is achieved by means of the ion concentration polarization effect induced at the micro/nano interface under the application of an external electric field, while species separation is achieved by exploiting the different electrophoretic mobilities of the sample components. The experimental results show that the device is capable of detecting C-reactive protein (CRP with an initial concentration as low as 9.50 × 10−6 mg/L given a sufficient preconcentration time and driving voltage. In addition, it is shown that a mixed-species sample consisting of three negatively-charged components (bovine serum albumin (BSA, tetramethylrhodamine(TAMRA isothiocyanate-Dextran and fluorescent polymer beads can be separated and preconcentrated within 20 min given a driving voltage of 100 V across 1 cm microchannel in length. In general, the present results confirm the feasibility of the device for the immunoassay or detection of various multi-species samples under low concentration in the biochemical and biomedical fields. The novel device can therefore improve the detection limit of traditional medical facilities.

Flow injection on-line spectrophotometric determination of thorium(IV) after preconcentration on XAD-4 resin impregnated with oxytetracycline

Energy Technology Data Exchange (ETDEWEB)

Shahida, Shabnam; Khan, Muhammad Haleem [Univ. of Azad Jammu and Kashmir, Muzaffarabad (Pakistan). Dept. of Chemistry; Ali, Akbar [Pakistan Institute of Nuclear Science and Technology, Islamabad (Pakistan). Chemistry Div.

2014-02-15

A very sensitive, selective and simple flow injection time-based method was developed for on-line preconcentration and determination of thorium(IV) at micro g L{sup -1} levels in environmental samples. The system operation was based on thorium(IV) ion retention at pH 4.0 in the minicolumn at a flow rate of 15.2 mL min{sup -1}. The trapped complex was then eluted with 3.6 mol L{sup -1} HCl at a flow rate of 4.9 mL min{sup -1}. The amount of thorium(IV) in the eluate was measured spectrophotometrically at 651 nm using arsenazo-III solution (0.05 % in 3.6 mol L{sup -1} HCl stabilized with 1 % triton X-100, 4.9 mL min{sup -1}) as colorimetric reagent. All chemical, and flow injection variables were optimized for the quantitative preconcentration of metal and a study of interference level of various ions was also carried out. The system offered low backpressure and improved sensitivity and selectivity. At a preconcentration time of 60 s and a sample frequency of 40 h{sup -1}, the enhancement factor was 97, the detection limit was 0.25 μg L{sup -1}, and the precision expressed as relative standard deviation was 1.08 % (at 50 μg L{sup -1}), whereas for 300 s of the preconcentration time and a sample frequency of 10 h{sup -1}, the enhancement factor of 357, the detection limit (3s) of 0.069 μg L{sup -1} and the precision of 1.32 % (at 10 μg L{sup -1}) was reported. The accuracy of the developed method was sufficient and evaluated by the analysis of certified reference material IAEA-SL-1 (Lake Sediment) and spiked water samples.

Flow injection on-line spectrophotometric determination of thorium(IV) after preconcentration on XAD-4 resin impregnated with oxytetracycline

International Nuclear Information System (INIS)

Shahida, Shabnam; Khan, Muhammad Haleem; Ali, Akbar

2014-01-01

A very sensitive, selective and simple flow injection time-based method was developed for on-line preconcentration and determination of thorium(IV) at micro g L"-"1 levels in environmental samples. The system operation was based on thorium(IV) ion retention at pH 4.0 in the minicolumn at a flow rate of 15.2 mL min"-"1. The trapped complex was then eluted with 3.6 mol L"-"1 HCl at a flow rate of 4.9 mL min"-"1. The amount of thorium(IV) in the eluate was measured spectrophotometrically at 651 nm using arsenazo-III solution (0.05 % in 3.6 mol L"-"1 HCl stabilized with 1 % triton X-100, 4.9 mL min"-"1) as colorimetric reagent. All chemical, and flow injection variables were optimized for the quantitative preconcentration of metal and a study of interference level of various ions was also carried out. The system offered low backpressure and improved sensitivity and selectivity. At a preconcentration time of 60 s and a sample frequency of 40 h"-"1, the enhancement factor was 97, the detection limit was 0.25 μg L"-"1, and the precision expressed as relative standard deviation was 1.08 % (at 50 μg L"-"1), whereas for 300 s of the preconcentration time and a sample frequency of 10 h"-"1, the enhancement factor of 357, the detection limit (3s) of 0.069 μg L"-"1 and the precision of 1.32 % (at 10 μg L"-"1) was reported. The accuracy of the developed method was sufficient and evaluated by the analysis of certified reference material IAEA-SL-1 (Lake Sediment) and spiked water samples.

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.

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)

On-line preconcentration and determination of mercury in biological and environmental samples by cold vapor-atomic absorption spectrometry

International Nuclear Information System (INIS)

Ferrua, N.; Cerutti, S.; Salonia, J.A.; Olsina, R.A.; Martinez, L.D.

2007-01-01

An on-line procedure for the determination of traces of total mercury in environmental and biological samples is described. The present methodology combines cold vapor generation associated to atomic absorption spectrometry (CV-AAS) with preconcentration of the analyte on a minicolumn packed with activated carbon. The retained analyte was quantitatively eluted from the minicolumn with nitric acid. After that, volatile specie of mercury was generated by merging the acidified sample and sodium tetrahydroborate(III) in a continuous flow system. The gaseous analyte was subsequently introduced via a stream of Ar carrier into the atomizer device. Optimizations of both, preconcentration and mercury volatile specie generation variables were carried out using two level full factorial design (2 3 ) with 3 replicates of the central point. Considering a sample consumption of 25 mL, an enrichment factor of 13-fold was obtained. The detection limit (3σ) was 10 ng L -1 and the precision (relative standard deviation) was 3.1% (n = 10) at the 5 μg L -1 level. The calibration curve using the preconcentration system for mercury was linear with a correlation coefficient of 0.9995 at levels near the detection limit up to at least 1000 μg L -1 . Satisfactory results were obtained for the analysis of mercury in tap water and hair samples

Analysis of biogenic carbonates by inductively coupled plasma-mass spectrometry (ICP-MS). Flow injection on-line solid-phase preconcentration for trace element determination in fish otoliths.

Science.gov (United States)

Arslan, Z; Paulson, A J

2002-04-01

The aragonite deposits within the ear bones (otoliths) of teleost fish retain a chemical signal reflecting the life history of fish (similar to rings of trees) and the nature of fish habitats. Otoliths dissolved in acid solutions contain high concentrations of calcium and a variety of proteins. Elimination of matrix salts and organic interferences during preconcentration is essential for accurate determination of trace elements in otolith solutions by inductively coupled plasma-quadrupole mass spectrometry. An iminodiacetate-based chelating resin (Toyopearl AF-Chelate 650 M) has been used for on-line preconcentration and matrix separation for the determination of 31 transition and rare elements. Successful preconcentration of the elements was achieved at pH 5 by on-line buffering, except Mn which required pH 8.8. Sample solutions were loaded on to the column for 1 min at 3.2 mL min(-1), and then eluted directly into the mass spectrometer with 4% v/v nitric acid. This procedure enabled up to 25-fold preconcentration with successful removal of the calcium matrix. The effect of heat-assisted oxidation with concentrated nitric acid was investigated to eliminate the organic matrix. It was found that heating to dryness after dissolution and further mineralization with the acid significantly improved the retention of the transition elements. The method was validated by analysis of a certified reference material produced from saggittal otoliths of emperor snapper ( Lutjanus sebae), and then applied to the determination of trace metal concentrations in juvenile bluefin tuna ( Thunnus thynnus) from the Western Pacific Ocean.

An on-line system using ion-imprinted polymer for preconcentration and determination of bismuth in seawater employing atomic fluorescence spectrometry.

Science.gov (United States)

Felix, Caio S A; Silva, Darllen G; Andrade, Heloysa M C; Riatto, Valeria B; Victor, Mauricio M; Ferreira, Sergio L C

2018-07-01

This work proposes an on-line preconcentration system using ion-imprinted polymer (IIP) for determination of bismuth in seawater employing atomic fluorescence spectrometry (AFS). The polymer was synthesized using 2- (5-bromo-2-pyridylazo) -5-diethylaminophenol (Br-PADAP) for complex formation, ethylene glycol dimethacrylate (EGDMA), cross-linking reagent and methacrylic acid (AMA) reagents, used as the functional monomer, 2,2-azobisisobutyronitrile was used as the radical initiator. The polymer was characterized employing the Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The determination of bismuth was performed employing hydride generation atomic fluorescence spectrometry (HG AFS) and the experimental conditions were optimized using a Box Behnken design involving the factors sample pH, eluent concentration and sodium tetrahydroborate concentration. So, using the optimized conditions the system allows the determination of bismuth with limits of detection and quantification of 26 and 88 ng L -1 , a preconcentration factor of 19.8. All these parameters were determined using a sample volume of 25 mL. The precision expressed as relative standard deviation (RSD%) was 3.7% for a bismuth(III) solution of concentration 0.25 µg L -1 . The system proposed was applied for the determination of bismuth in four seawater samples collected in Salvador City, Bahia State, Brazil. The concentrations obtained varied from 0.38 to 0.45 μg L -1 . The accuracy was evaluated by addition/recovery test, and the recoveries found varied from 92% to 101%. Copyright © 2018 Elsevier B.V. All rights reserved.

Evaluation of a novel PTFE material for separation and preconcentration of trace levels of metal ions in sequential injection (SI) and sequential injection lab-on-valve (SI-LOV) systems interfaced with detection by ETAAS

DEFF Research Database (Denmark)

Long, Xiangbao; Chomchoei, Roongrat; Gała, Piotr

The operational characteristics of a novel PTFE bead material, granular Algoflon®, used for separation and preconcentration of metal ions via adsorption of on-line generated non-charged metal complexes, were evaluated in a sequential injection (SI) system furnished with an external packed column...... and in a sequential injection lab-on-valve (SI-LOV) system. Employed for the determination of cadmium(II), complexed with diethyldithiophosphate (DDPA), and detection by electrothermal atomic absorption spectrometry (ETAAS), its performance was compared to that of a previously used material, Aldrich PTFE, which had...... demonstrated that PTFE was the most promising for solid-state pretreatments. By comparing the two materials, the Algoflon® beads exhibited much higher sensitivity (1.6107 versus 0.2956 μg l-1 per integrated absorbance (s)), and better retention efficiency (82% versus 74%) and enrichment factor (20.8 versus 17...

Automatic on-line pre-concentration system using a knotted reactor for the FAAS determination of lead in drinking water

International Nuclear Information System (INIS)

Souza, Anderson S.; Brandao, Geovani C.; Santos, Walter N.L. dos; Lemos, Valfredo A.; Ganzarolli, Edgard M.; Bruns, Roy E.; Ferreira, Sergio L.C.

2007-01-01

An automatic on-line pre-concentration system is proposed for lead determination in drinking water using flame atomic absorption spectrometry (FAAS). Lead(II) ions are retained as the 1-(2-pyridylazo)-2-naphthol (PAN) complex in the walls of a knotted reactor, followed by an elution step using 0.50 mol L -1 hydrochloric acid solution. Optimisation involving the sampling flow rate, pH and buffer concentration factors was performed using a Box-Behnken design. Other factors were established considering results of previous experiments. The procedure allows the determination of lead with a 0.43 μg L -1 detection limit (3σ/S) and precisions (expressed as relative standard deviation) of 4.84% (N = 7) and 2.9% (N = 7) for lead concentrations of 5 and 25 μg L -1 , respectively. The accuracy was confirmed by the determination of lead in the NIST SRM 1643d trace elements in natural water standard reference material. The pre-concentration factor obtained is 26.5 and the sampling frequency is 48 h -1 . The recovery achieved for lead determination in the presence of several ions demonstrated that this procedure could be applied to the analysis of drinking water samples. The method was applied for lead determination in drinking water samples collected in Jequie City, Brazil. The lead concentration found in 25 samples were always lower than the permissible maximum levels stipulated by World Health Organization

Separation and Preconcentration of Trace Amounts of Nickel from Aqueous Samples

Directory of Open Access Journals (Sweden)

Reyhaneh Rahnama

2018-05-01

Full Text Available In this paper, a new method for preconcentration and measurement of trace amounts of nickel in aqueous samples by magnetic solid phase extraction (MSPE via magnetic carbon nanotubes (Mag-CNTs was developed. In order to increase selectivity, α-Furildioxime was used as chelating agent. In order to do extraction, optimum amount of ligand was added to the nickel sample and pH was set on 9, then 7 ml. of adsorbent was added and stirred for 15 minutes. After that, aqueous phase and adsorbent were separated by a strong magnet. Finally, the absorption was measured via flame atomic absorption spectrometry by analyte elution from the absorbent with an appropriate solution. Parameters affecting the extraction and preconcentration of nickel were investigated and optimized. Under optimum conditions, the calibration curve was linear in concentration range from 2.5 to 375 µg L-1 and the detection limit was 0.8 µg L-1 of nickel. The method was applied for determination of nickel in aqueous samples. The relative efficiency values of nickel measurement in aqueous samples were from 98.7% to 102.1%.  Results indicated that Mag-CNTs can be used as an effective and inexpensive absorbent for preconcentration and extraction of nickel from actual samples.

Determination of low cadmium concentrations in wine by on-line preconcentration in a knotted reactor coupled to an inductively coupled plasma optical emission spectrometer with ultrasonic nebulization

Energy Technology Data Exchange (ETDEWEB)

Lara, R.F. [Inst. de Investigaciones Mineras, Universidad Nacional de San Juan (Argentina); Wuilloud, R.G.; Salonia, J.A. [Dept. of Analytical Chemistry, National University of San Luis (Argentina); Olsina, R.A.; Martinez, L.D. [Dept. of Analytical Chemistry, National University of San Luis (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina)

2001-12-01

An on-line cadmium preconcentration and determination system implemented with inductively coupled plasma optical emission spectrometry (ICP-OES) associated to flow injection (FI) with ultrasonic nebulization system (USN) was studied. The cadmium was retained as the cadmium-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol, Cd-(5-Br-PADAP), complex, at pH 9.5. The cadmium complex was removed from the knotted reactor (KR) with 3.0 mol/L nitric acid. A total enhancement factor of 216 was obtained with respect to ICP-OES using pneumatic nebulization (12 for USN and 18 for KR) with a preconcentration time of 60 s. The value of the detection limit for the preconcentration of 5 mL of sample solution was 5 ng/L. The precision for 10 replicate determinations at the 5 {mu}g/L Cd level was 2.9% relative standard deviation (RSD), calculated from the peak heights obtained. The calibration graph using the preconcentration system for cadmium was linear with a correlation coefficient of 0.9998 at levels near the detection limits up to at least 1000 {mu}g/L. The method was successfully applied to the determination of cadmium in wine samples. (orig.)

Flow analysis by using solenoid valves for As(III determination in natural waters by an on-line separation and pre-concentration system coupled to a tungsten coil atomizer

Directory of Open Access Journals (Sweden)

José Y. Neira

2005-03-01

Full Text Available A flow system coupled to a tungsten coil atomizer in an atomic absorption spectrometer (TCA-AAS was developed for As(III determination in waters, by extraction with sodium diethyldithiocarbamate (NaDDTC as complexing agent, and by sorption of the As(III-DDTC complex in a micro-column filled with 5 mg C18 reversed phase (10 µL dry sorbent, followed by elution with ethanol. A complete pre-concentration/elution cycle took 208 s, with 30 s sample load time (1.7 mL and 4 s elution time (71 µL. The interface and software for the synchronous control of two peristaltic pumps (RUN/ STOP, an autosampler arm, seven solenoid valves, one injection valve, the electrothermal atomizer and the spectrometer Read function were constructed. The system was characterized and validated by analytical recovery studies performed both in synthetic solutions and in natural waters. Using a 30 s pre-concentration period, the working curve was linear between 0.25 and 6.0 µg L-1 (r = 0.9976, the retention efficiency was 94±1% (6.0 µg L-1, and the pre-concentration coefficient was 28.9. The characteristic mass was 58 pg, the mean repeatability (expressed as the variation coefficient was 3.4% (n=5, the detection limit was 0.058 µg L-1 (4.1 pg in 71 µL of eluate injected into the coil, and the mean analytical recovery in natural waters was 92.6 ± 9.5 % (n=15. The procedure is simple, economic, less prone to sample loss and contamination and the useful lifetime of the micro-column was between 200-300 pre-concentration cycles.

Force fields of charged particles in micro-nanofluidic preconcentration systems

Science.gov (United States)

Gong, Lingyan; Ouyang, Wei; Li, Zirui; Han, Jongyoon

2017-12-01

Electrokinetic concentration devices based on the ion concentration polarization (ICP) phenomenon have drawn much attention due to their simple setup, high enrichment factor, and easy integration with many subsequent processes, such as separation, reaction, and extraction etc. Despite significant progress in the experimental research, fundamental understanding and detailed modeling of the preconcentration systems is still lacking. The mechanism of the electrokinetic trapping of charged particles is currently limited to the force balance analysis between the electric force and fluid drag force in an over-simplified one-dimensional (1D) model, which misses many signatures of the actual system. This letter studies the particle trapping phenomena that are not explainable in the 1D model through the calculation of the two-dimensional (2D) force fields. The trapping of charged particles is shown to significantly distort the electric field and fluid flow pattern, which in turn leads to the different trapping behaviors of particles of different sizes. The mechanisms behind the protrusions and instability of the focused band, which are important factors determining overall preconcentration efficiency, are revealed through analyzing the rotating fluxes of particles in the vicinity of the ion-selective membrane. The differences in the enrichment factors of differently sized particles are understood through the interplay between the electric force and convective fluid flow. These results provide insights into the electrokinetic concentration effect, which could facilitate the design and optimization of ICP-based preconcentration systems.

Preconcentration of traces of radionuclides with sorbents based on spherical polyurethane membrane systems in the analysis of environmental samples

International Nuclear Information System (INIS)

Palagyi, S.; Braun, T.

1986-01-01

In the paper the importance of preconcentration and a permanent need for efficient preconcentrating agents in environmental analysis are pointed out. The increased attention is devoted to the foamed polyurethane sorbents as a novel advance in the separation chemistry. The paper has two main aims. The first is to present a survey of recent applications of unloaded and reagent loaded open-cell type resilient polyurethane foams to the separation and preconcentration of radionuclides from environmental samples. The second is to show the newest results in the use of these foams for the preconcentration and determination of traces of some mainly inorganic species in environmental samples by radioanalytical techniques. Some future possibilities of the use of polyurethane foams in trace elemental determinations in environmental analysis are also outlined. (author)

An on-line pre-concentration system for determination of cadmium in drinking water using FAAS

International Nuclear Information System (INIS)

Santos, Walter N.L. dos; Costa, Jorge L.O.; Araujo, Rennan G.O.; Jesus, Djane S. de; Costa, Antonio C.S.

2006-01-01

In the present paper, a minicolumn of polyurethane foam loaded with 4-(2-pyridylazo)-resorcinol (PAR) is proposed as pre-concentration system for cadmium determination in drinking water samples by flame atomic absorption spectrometry. The optimization step was performed using two-level full factorial design and Doehlert matrix, involving the variables: sampling flow rate, elution concentration, buffer concentration and pH. Using the established experimental conditions in the optimization step of: pH 8.2, sampling flow rate 8.5 mL min -1 , buffer concentration 0.05 mol L -1 and elution concentration of 1.0 mol L -1 , this system allows the determination of cadmium with detection limit (LD) (3σ/S) of 20.0 ng L -1 and quantification limit (LQ) (10σ/S) of 64 ng L -1 , precision expressed as relative standard deviation (R.S.D.) of 5.0 and 4.7% for cadmium concentration of 5.0 and 40.0 μg L -1 , respectively, and a pre-concentration factor of 158 for a sample volume of 20.0 mL. The accuracy was confirmed by cadmium determination in the standard reference material, NIST SRM 1643d trace elements in natural water. This procedure was applied for cadmium determination in drinking water samples collected from Salvador City, Bahia, Brazil. For five samples analyzed, the achieved concentrations varied from 0.31 to 0.86 μg L -1

Determination of trace amounts of lead by chelating ion exchange and on-line preconcentration in flow-injection atomic absorption spectrometry

International Nuclear Information System (INIS)

Purohit, Rajesh; Devi, Surekha

1992-01-01

Resins synthesized from quinolin-8-ol and resorcinol or hydro-quinone, with furfuraldehyde, formaldehyde or benzaldehyde as cross-linking agent, were used for the preconcentration of nanogram amounts of lead. The rate of exchange and activation energy of lead exchange were calculated. Column separations of lead-copper and lead-zinc did not show any cross-contamination. A continuous flow manifold using resin microcolumns was developed for the preconcentration and determination of lead. (author). 24 refs.; 5 figs.; 3 tabs

Lead ultra-trace on-line preconcentration and determination using selective solid phase extraction and electrothermal atomic absorption spectrometry: applications in seawaters and biological samples

Energy Technology Data Exchange (ETDEWEB)

Vereda Alonso, E.; Siles Cordero, M.T.; Garcia de Torres, A.; Cano Pavon, J.M. [University of Malaga, Department of Analytical Chemistry Faculty of Sciences, Malaga (Spain)

2006-08-15

In this work, a new chelating resin [1,5-bis (2-pyridyl)-3-sulphophenyl methylene] thiocarbonohydrazide immobilised on aminopropyl-controlled pore glass (550 Aa; PSTH-cpg) was synthesised and packed in a microcolumn which replaced the sample tip of the autosampler arm. The system was applied to the preconcentration of lead. When microliters of 10% HNO{sub 3}, which acts as elution agent, pass through the microcolumn, the preconcentrated Pb(II) is eluted and directly deposited in a tungsten-rhodium coated graphite tube. With the use of the separation and preconcentration step and the permanent modifiers, the analytical characteristics of the technique were improved. The proposed method has a linear calibration range from 0.012 to 10 ng ml{sup -1} of lead. At a sample frequency of 36 h{sup -1} with a 90 s preconcentration time, the enrichment factor was 20.5, the detection and determination limits were 0.012 and 0.14 ng ml{sup -1}, respectively and the precision, expressed as relative standard deviation, was 3.2% (at 1 ng ml{sup -1}). Results from the determination of Pb in biological certified reference materials were in agreement with the certified values. Seawaters and other biological samples were analysed too. (orig.)

Microfluidic paper-based biomolecule preconcentrator based on ion concentration polarization.

Science.gov (United States)

Han, Sung Il; Hwang, Kyo Seon; Kwak, Rhokyun; Lee, Jeong Hoon

2016-06-21

Microfluidic paper-based analytical devices (μPADs) for molecular detection have great potential in the field of point-of-care diagnostics. Currently, a critical problem being faced by μPADs is improving their detection sensitivity. Various preconcentration processes have been developed, but they still have complicated structures and fabrication processes to integrate into μPADs. To address this issue, we have developed a novel paper-based preconcentrator utilizing ion concentration polarization (ICP) with minimal addition on lateral-flow paper. The cation selective membrane (i.e., Nafion) is patterned on adhesive tape, and this tape is then attached to paper-based channels. When an electric field is applied across the Nafion, ICP is initiated to preconcentrate the biomolecules in the paper channel. Departing from previous paper-based preconcentrators, we maintain steady lateral fluid flow with the separated Nafion layer; as a result, fluorescent dyes and proteins (FITC-albumin and bovine serum albumin) are continuously delivered to the preconcentration zone, achieving high preconcentration performance up to 1000-fold. In addition, we demonstrate that the Nafion-patterned tape can be integrated with various geometries (multiplexed preconcentrator) and platforms (string and polymer microfluidic channel). This work would facilitate integration of various ICP devices, including preconcentrators, pH/concentration modulators, and micro mixers, with steady lateral flows in paper-based platforms.

Separation and preconcentration of uranium from different matrices by extraction chromatography on U-TEVA resin

International Nuclear Information System (INIS)

Becquart, Elena T.; Bianco, Gladis N.; Chiacchio, Hugo A.; Palestrini, Leonardo J.; Servant, Roberto E.

1999-01-01

The objectives of this work were the determination of uranium in effluents and spring waters, in high and low U 3 O 8 containing minerals and in Zircaloy. The separations were done by extraction chromatography, using U-TEVA Spec (uranium tetravalent actinide specific, ElChroM, Illinois, USA), a commercial resin consisting of Amberlite XAD-7 (Rohm and Haas), an inert support of a non ionic polymeric adsorbent, soaked by diamylamylphosphonate, a selective extractant. Disposable plastic columns, 7.9 mm internal diameter, 10 cm total length, with a bed 4.5 cm high and 2 ml volume were used. Quantification was done by spectrophotometric determination of uranium with the chromogenic reagent 2-(5-bromo-2-pyridylazo)-5-diethyl aminophenol (Br-PADAP). The following working conditions were optimized: uranium sorption and preconcentration, elution, separation of others cations as Zr (IV), Gd (III), Th (IV) and uranium elution, using different solutions of nitric or hydrochloric acids as convenient. Break through was 30 mg of uranium and capacity at total saturation was between 35 and 40 mg U/ml of bed. Programs were developed for previous leaching of minerals and Zircaloy in a microwave oven. Procedures operations were satisfactory with recoveries higher than 95% and a percent relative standard deviation better than 1% for 100 μg of uranium, on five replicates. Quantification limit was 4 ppb (0.1 μg of U in the 25 ml volumetric flask where color was developed with chromogenic reagent), but if uranium is concentrated 5 times in the column and a 5 ml volume is used for elution, a sample containing 0.4 ppb of uranium can be analysed. Absorbance was measured at λ = 578 nm using 5 cm cells. The extraction system is profitable because it allows to work at room temperature, with gravity flow, high specificity and minimum waste generation. The objectives have been satisfactorily accomplished, so an easy, in small columns, uranium sorbing system is available to be used in the

High-throughput liquid-absorption preconcentrator sampling methods

Science.gov (United States)

Zaromb, Solomon

1994-01-01

A system for detecting trace concentrations of an analyte in air includes a preconcentrator for the analyte and an analyte detector. The preconcentrator includes an elongated tubular container comprising a wettable material. The wettable material is continuously wetted with an analyte-sorbing liquid which flows from one part of the container to a lower end. Sampled air flows through the container in contact with the wetted material with a swirling motion which results in efficient transfer of analyte vapors or aerosol particles to the sorbing liquid and preconcentration of traces of analyte in the liquid. The preconcentrated traces of analyte may be either detected within the container or removed therefrom for injection into a separate detection means or for subsequent analysis.

Coupling sequential injection on-line preconcentration using a PTFE beads packed column to direct injection nebulization inductively coupled plasma mass spectrometry

DEFF Research Database (Denmark)

Wang, Jianhua; Hansen, Elo Harald

2002-01-01

An automated sequential injection on-line preconcentration procedure for trace metals by using a PTFE bead-packed microcolumn coupled to ICP-MS is described, and used for simultaneous analyses of cadmium and lead. In dilute nitric acid (0.5%, v/v), neutral complexes between the analytes...

A novel fiber-packed column for on-line preconcentration and speciation analysis of chromium in drinking water with flame atomic absorption spectrometry.

Science.gov (United States)

Monasterio, Romina P; Altamirano, Jorgelina C; Martínez, Luis D; Wuilloud, Rodolfo G

2009-02-15

A novel on-line preconcentration and determination system based on a fiber-packed column was developed for speciation analysis of Cr in drinking water samples prior to its determination by flame atomic absorption spectrometry (FAAS). All variables involved in the development of the preconcentration method including, pH, eluent type, sample and eluent flow rates, interfering effects, etc., were studied in order to achieve the best analytical performance. A preconcentration factor of 32 was obtained for Cr(VI) and Cr(III). The levels of Cr(III) species were calculated by difference of total Cr and Cr(VI) levels. Total Cr was determined after oxidation of Cr(III) to Cr(VI) with hydrogen peroxide. The calibration graph was linear with a correlation coefficient of 0.999 at levels near the detection limit and up to at least 50 microg L(-1). The relative standard deviation (R.S.D.) was 4.3% (C=5 microg L(-1) Cr(VI), n=10, sample volume=25 mL). The limit of detection (LOD) for both Cr(III) and Cr(VI) species was 0.3 microg L(-1). Verification of the accuracy was carried out by the analysis of a standard reference material (NIST SRM 1643e "Trace elements in natural water"). The method was successfully applied to the determination of Cr(III) and Cr(VI) species in drinking water samples.

Separation and preconcentration of lead(II), cobalt(II), and nickel(II) on EDTA immobilized activated carbon cloth prior to flame atomic absorption spectrometric determination in environmental samples

OpenAIRE

ALOTHMAN, ZEID ABDULLAH; YILMAZ, ERKAN; HABİLA, MOHAMED; SOYLAK, MUSTAFA

2015-01-01

The synthesis and characterization of ethylenediaminetetraacetic acid immobilized activated carbon cloth was performed in the present work. It was used for preconcentration-separation of lead(II), cobalt(II), and nickel(II) at trace levels as an adsorbent. Factors including pH, concentration and volume of eluent, sample and eluent flow rates, sample volume, and effect of coexisting ions on the solid phase extraction of analytes were examined. The preconcentration factor was 50. The detection ...

Determination of arsenic in water samples by Total Reflection X-Ray Fluorescence using pre-concentration with alumina

Energy Technology Data Exchange (ETDEWEB)

Barros, Haydn [Laboratorio de Fisica Nuclear, Dpto. De Fisica, Universidad Simon Bolivar, Sartenejas, Baruta (Venezuela, Bolivarian Republic of); Marco Parra, Lue-Meru, E-mail: luemerumarco@yahoo.e [Universidad Centroccidental Lisandro Alvarado, Dpto. Quimica y Suelos, Decanato de Agronomia, Tarabana, Cabudare, Edo.Lara (Venezuela, Bolivarian Republic of); Bennun, Leonardo [Universidad de Concepcion, Concepcion (Chile); Greaves, Eduardo D. [Laboratorio de Fisica Nuclear, Dpto. De Fisica, Universidad Simon Bolivar, Sartenejas, Baruta (Venezuela, Bolivarian Republic of)

2010-06-15

The determination of arsenic in water samples requires techniques of high sensitivity. Total Reflection X-Ray Fluorescence (TXRF) allows the determination but a prior separation and pre-concentration procedure is necessary. Alumina is a suitable substrate for the selective separation of the analytes. A method for separation and pre-concentration in alumina, followed by direct analysis of the alumina is evaluated. Quantification was performed using the Al-K{alpha} and Co-K{alpha} lines as internal standard in samples prepared on an alumina matrix, and compared to a calibration with aqueous standards. Artificial water samples of As (III) and As (V) were analyzed after the treatment. Fifty milliliters of the sample at ppb concentration levels were mixed with 10 mg of alumina. The pH, time and temperature were controlled. The alumina was separated from the slurry by centrifugation, washed with de-ionized water and analyzed directly on the sample holder. A pre-concentration factor of 100 was found, with detection limit of 0.7 {mu}gL{sup -1}. The percentage of recovery was 98% for As (III) and 95% for As (V) demonstrating the suitability of the procedure.

Determination of arsenic in water samples by Total Reflection X-Ray Fluorescence using pre-concentration with alumina

International Nuclear Information System (INIS)

Barros, Haydn; Marco Parra, Lue-Meru; Bennun, Leonardo; Greaves, Eduardo D.

2010-01-01

The determination of arsenic in water samples requires techniques of high sensitivity. Total Reflection X-Ray Fluorescence (TXRF) allows the determination but a prior separation and pre-concentration procedure is necessary. Alumina is a suitable substrate for the selective separation of the analytes. A method for separation and pre-concentration in alumina, followed by direct analysis of the alumina is evaluated. Quantification was performed using the Al-Kα and Co-Kα lines as internal standard in samples prepared on an alumina matrix, and compared to a calibration with aqueous standards. Artificial water samples of As (III) and As (V) were analyzed after the treatment. Fifty milliliters of the sample at ppb concentration levels were mixed with 10 mg of alumina. The pH, time and temperature were controlled. The alumina was separated from the slurry by centrifugation, washed with de-ionized water and analyzed directly on the sample holder. A pre-concentration factor of 100 was found, with detection limit of 0.7 μgL -1 . The percentage of recovery was 98% for As (III) and 95% for As (V) demonstrating the suitability of the procedure.

Electrolytic preconcentration in instrumental analysis.

Science.gov (United States)

Sioda, R E; Batley, G E; Lund, W; Wang, J; Leach, S C

1986-05-01

The use of electrolytic deposition as a separation and preconcentration step in trace metal analysis is reviewed. Both the principles and applications of the technique are dealt with in some detail. Electrolytic preconcentration can be combined with a variety of instrumental techniques. Special attention is given to stripping voltammetry, potentiometric stripping analysis, different combinations with atomic-absorption spectrometry, and the use of flow-through porous electrodes. It is pointed out that the electrolytic preconcentration technique deserves more extensive use as well as fundamental investigation.

On-line preconcentration using a resin functionalized with 3,4-dihydroxybenzoic acid for the determination of trace elements in biological samples by thermospray flame furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Lemos, Valfredo A.; Bezerra, Marcos A.; Amorim, Fabio A.C.

2008-01-01

In the present paper, an on-line preconcentration procedure for determination of cadmium, copper and zinc by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) is proposed. Amberlite XAD-4 functionalized with 3,4-dihydroxybenzoic acid (XAD4-DHB) packed in a minicolumn was used as sorbent material. The metals were retained on the XAD-DHB resin, from which it could be eluted directly to the thermospray flame furnace system. The detection limits were 28 (Cd), 100 (Cu) and 77 ng L -1 (Zn) for 60 s preconcentration time, at a sample flow rate of 7.0 mL min -1 . Enrichment factors were 102, 91 and 62, for cadmium, copper and zinc, respectively. The procedure has been applied successfully to metal determination in biological standard reference materials

Non-chromatographic speciation analysis of mercury by flow injection on-line preconcentration in combination with chemical vapor generation atomic fluorescence spectrometry

International Nuclear Information System (INIS)

Wu Hong; Jin Yan; Han Weiying; Miao, Qiang; Bi Shuping

2006-01-01

A novel non-chromatographic approach for direct speciation of mercury, based on the selective retention inorganic mercury and methylmercury on the inner wall of a knotted reactor by using ammonium diethyl dithiophosphate and dithizone as complexing agents respectively, was developed for flow injection on-line sorption preconcentration coupled with chemical vapor generation non-dispersive atomic fluorescence spectrometry. With the sample pH kept at 2.0, the preconcentration of inorganic mercury on the inner walls of the knotted reactor was carried out based on the exclusive retention of Hg-DDP complex in the presence of methylmercury via on-line merging the sample solution with ammonium diethyl dithiophosphate solution, and selective preconcentration methylmercury was achieved with dithizone instead of ammonium diethyl dithiophosphate. A 15% (v/v) HCl was introduced to elute the retained mercury species and merge with KBH 4 solution for atomic fluorescence spectrometry detection. Under the optimal experimental conditions, the sample throughputs of inorganic mercury and methylmercury were 30 and 20 h -1 with the enhancement factors of 13 and 24. The detection limits were found to be 3.6 ng l -1 for Hg 2+ and 2.0 ng l -1 for CH 3 Hg + . The precisions (RSD) for the 11 replicate measurements of each 0.2 μg l -1 of Hg 2+ and CH 3 Hg + were 2.2% and 2.8%, respectively. The developed method was validated by the analysis of certified reference materials (simulated natural water, rice flour and pork) and by recovery measurements on spiked samples, and was applied to the determination of inorganic mercury and methylmercury in biological and environmental water samples

Separation/preconcentration and determination of vanadium with dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) and electrothermal atomic absorption spectrometry.

Science.gov (United States)

Asadollahi, Tahereh; Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji

2010-06-30

A novel dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) for separation/preconcentration of ultra trace amount of vanadium and its determination with the electrothermal atomic absorption spectrometry (ETAAS) was developed. The DLLME-SFO behavior of vanadium (V) using N-benzoyl-N-phenylhydroxylamine (BPHA) as complexing agent was systematically investigated. The factors influencing the complex formation and extraction by DLLME-SFO method were optimized. Under the optimized conditions: 100 microL, 200 microL and 25 mL of extraction solvent (1-undecanol), disperser solvent (acetone) and sample volume, respectively, an enrichment factor of 184, a detection limit (based on 3S(b)/m) of 7 ng L(-1) and a relative standard deviation of 4.6% (at 500 ng L(-1)) were obtained. The calibration graph using the preconcentration system for vanadium was linear from 20 to 1000 ng L(-1) with a correlation coefficient of 0.9996. The method was successfully applied for the determination of vanadium in water and parsley. Copyright 2010 Elsevier B.V. All rights reserved.

Non-chromatographic speciation analysis of mercury by flow injection on-line preconcentration in combination with chemical vapor generation atomic fluorescence spectrometry

Energy Technology Data Exchange (ETDEWEB)

Wu Hong [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China); Department of Chemistry, Xuzhou Normal University, Xuzhou 221116 (China); Jin Yan [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China); Han Weiying [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China); Miao, Qiang [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China); Bi Shuping [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China)]. E-mail: bisp@nju.edu.cn

2006-07-15

A novel non-chromatographic approach for direct speciation of mercury, based on the selective retention inorganic mercury and methylmercury on the inner wall of a knotted reactor by using ammonium diethyl dithiophosphate and dithizone as complexing agents respectively, was developed for flow injection on-line sorption preconcentration coupled with chemical vapor generation non-dispersive atomic fluorescence spectrometry. With the sample pH kept at 2.0, the preconcentration of inorganic mercury on the inner walls of the knotted reactor was carried out based on the exclusive retention of Hg-DDP complex in the presence of methylmercury via on-line merging the sample solution with ammonium diethyl dithiophosphate solution, and selective preconcentration methylmercury was achieved with dithizone instead of ammonium diethyl dithiophosphate. A 15% (v/v) HCl was introduced to elute the retained mercury species and merge with KBH{sub 4} solution for atomic fluorescence spectrometry detection. Under the optimal experimental conditions, the sample throughputs of inorganic mercury and methylmercury were 30 and 20 h{sup -1} with the enhancement factors of 13 and 24. The detection limits were found to be 3.6 ng l{sup -1} for Hg{sup 2+} and 2.0 ng l{sup -1} for CH{sub 3}Hg{sup +}. The precisions (RSD) for the 11 replicate measurements of each 0.2 {mu}g l{sup -1} of Hg{sup 2+} and CH{sub 3}Hg{sup +} were 2.2% and 2.8%, respectively. The developed method was validated by the analysis of certified reference materials (simulated natural water, rice flour and pork) and by recovery measurements on spiked samples, and was applied to the determination of inorganic mercury and methylmercury in biological and environmental water samples.

Model experiments to test the use of a liquid membrane for separation and preconcentration of copper from natural water

Energy Technology Data Exchange (ETDEWEB)

Granado-Castro, Maria D.; Galindo-Riano, Maria D.; Garcia-Vargas, Manuel

2004-03-17

The transfer and separation of Cu(II) ions across a bulk liquid membrane (BLM) containing pyridine-2-acetaldehyde benzoylhydrazone (2-APBH) as the mobile carrier dissolved in toluene has been investigated and optimised. The system was applied to the preconcentration of copper from natural waters prior to analysis by flame atomic absorption spectroscopy. The flux of copper across the membrane has been studied, and characterised as a function of analytical variables such as the carrier concentration, volume of organic phase, pH of feed and strip receiving solutions, stirring rate and temperature of solutions. The preconcentration yield at optimum conditions was 100.54{+-}0.94%, even with a high saline matrix (30 g l{sup -1} NaCl), with good precision (1.49%). A preconcentration factor of approximately 18 times could be obtained. The detection limit of a blank sample was 0.24 {mu}g l{sup -1} of Cu. The method was validated using a certified reference material (TMDA-62) and was applied successfully to the analysis of copper in two samples of seawater collected from the coast of Huelva (Spain). The relative errors were 2.42% for CRM and 0.48 and 3.66%, for seawaters (obtained between the results of the proposed and DPASV methods), respectively.

Determination of inorganic arsenic species in natural waters--benefits of separation and preconcentration on ion exchange and hybrid resins.

Science.gov (United States)

Ben Issa, Nureddin; Rajaković-Ognjanović, Vladana N; Jovanović, Branislava M; Rajaković, Ljubinka V

2010-07-19

A simple method for the separation and determination of inorganic arsenic (iAs) species in natural and drinking water was developed. Procedures for sample preparation, separation of As(III) and As(V) species and preconcentration of the total iAs on fixed bed columns were defined. Two resins, a strong base anion exchange (SBAE) resin and a hybrid (HY) resin were utilized. The inductively-coupled plasma-mass spectrometry method was applied as the analytical method for the determination of the arsenic concentration in water. The governing factors for the ion exchange/sorption of arsenic on resins in a batch and a fixed bed flow system were analyzed and compared. Acidity of the water, which plays an important role in the control of the ionic or molecular forms of arsenic species, was beneficial for the separation; by adjusting the pH values to less than 8.00, the SBAE resin separated As(V) from As(III) in water by retaining As(V) and allowing As(III) to pass through. The sorption activity of the hydrated iron oxide particles integrated into the HY resin was beneficial for bonding of all iAs species over a wide range of pH values from 5.00 to 11.00. The resin capacities were calculated according to the breakthrough points in a fixed bed flow system. At pH 7.50, the SBAE resin bound more than 370 microg g(-1) of As(V) while the HY resin bound more than 4150 microg g(-1) of As(III) and more than 3500 microg g(-1) of As(V). The high capacities and selectivity of the resins were considered as advantageous for the development and application of two procedures, one for the separation and determination of As(III) (with SBAE) and the other for the preconcentration and determination of the total arsenic (with HY resin). Methods were established through basic analytical procedures (with external standards, certified reference materials and the standard addition method) and by the parallel analysis of some samples using the atomic absorption spectrometry-hydride generation

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...

Review of procedures involving separation and preconcentration for the determination of cadmium using spectrometric techniques

International Nuclear Information System (INIS)

Ferreira, Sergio L.C.; Andrade, Jailson B. de; Korn, Maria das Gracas A.; Pereira, Madson de G.; Lemos, Valfredo A.; Santos, Walter N.L. dos; Rodrigues, Frederico de Medeiros; Souza, Anderson S.; Ferreira, Hadla S.; Silva, Erik G.P. da

2007-01-01

Spectrometric techniques for the analysis of trace cadmium have developed rapidly due to the increasing need for accurate measurements at extremely low levels of this element in diverse matrices. This review covers separation and preconcentration procedures, such as electrochemical deposition, precipitation, coprecipitation, solid phase extraction, liquid-liquid extraction (LLE) and cloud point extraction (CPE), and consider the features of the their application with several spectrometric techniques

Battery operated preconcentration-assisted lateral flow assay.

Science.gov (United States)

Kim, Cheonjung; Yoo, Yong Kyoung; Han, Sung Il; Lee, Junwoo; Lee, Dohwan; Lee, Kyungjae; Hwang, Kyo Seon; Lee, Kyu Hyoung; Chung, Seok; Lee, Jeong Hoon

2017-07-11

Paper-based analytical devices (e.g. lateral flow assays) are highly advantageous as portable diagnostic systems owing to their low costs and ease of use. Because of their low sensitivity and detection limits for biomolecules, these devices have several limitations in applications for real-field diagnosis. Here, we demonstrate a paper-based preconcentration enhanced lateral flow assay using a commercial β-hCG-based test. Utilizing a simple 9 V battery operation with a low power consumption of approximately 81 μW, we acquire a 25-fold preconcentration factor, demonstrating a clear sensitivity enhancement in the colorimetric lateral flow assay; consequently, clear colors are observed in a rapid kit test line, which cannot be monitored without preconcentration. This device can also facilitate a semi-quantitative platform using the saturation value and/or color intensity in both paper-based colorimetric assays and smartphone-based diagnostics.

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...

Determination of trace thorium in water samples by flow injection fluorescence spectrophotometry with microcolumn on-line preconcentration

International Nuclear Information System (INIS)

Shen Zhuqin; Zhang Yanan; Guo Dongfa; Huang Yun

1991-01-01

An on-line preconcentration time resolved fluorimetric method was developed for the determination of trace thorium in water, based on luminescence of complex Th-morin-TOPO (or TRPO)-sodium lauryl sulfate in sulfuric acid medium. Interferences from companied cations, such as Al 3+ and Zr 4+ , which emit fluorescence with much slower rising rate at the same condition were effectively eliminated through optimization of the manifold parameters and precisely controlling of the elution flow rate. Effects of nearly 40 ions were also investigated. The detection limit, the liner range and relative standard deviation for 50 ng Th are 2.5 ng/L, 0∼80 ng and 3.6%, respectively. Sampling rate is 30 per hour

Coupling on-line preconcentration by ion-exchange with ETAAS. A novel flow injection approach based on the use of a renewable microcolumn as demonstrated for the determination of nickel in environmental and biological samples

DEFF Research Database (Denmark)

Wang, Jianhua; Hansen, Elo Harald

2000-01-01

microcolumn incorporated within an integrated micro FI-system, the column is loaded with a defined volume of small beads of an SP Sephadex C-25 cation-exchange resin and subsequently exposed to a metered amount of sample solution. However, instead of eluting the retained analyte from the organic ion-exchange......A novel way of exploiting flow injection/sequential injection (FIA/SIA) on-line ion-exchange preconcentration with detection by electrothermal atomic absorption spectrometry (ETAAS) is described and demonstrated for the determination of trace-levels of nickel. Based on the use of a renewable...... resin, the beads are along with 30 mul of carrier (buffer) solution transported via air segmentation directly into the graphite tube, where they are ashed during the pyrolysis and atomization process. The ETAAS determination is performed in parallel with the preconcentration process of the ensuing...

Economic evaluation of preconcentration of uranium ores

International Nuclear Information System (INIS)

1981-04-01

The economics of two options for the preconcentration of low-grade uranium ores prior to hydrochloric acid leaching were studied. The first option uses flotation followed by wet high-intensity magnetic separation. The second option omits the flotation step. In each case it was assumed that most of the pyrite in the ore would be recovered by froth flotation, dewatered, and roasted to produce sulphuric acid and a calcine suitable for acid leaching. Savings in operating costs from preconcentration are offset by the value of uranium losses. However, a capital saving of approximately 6 million dollars is indicated for each preconcentration option. As a result of the capital saving, preconcentration appears to be economically attractive when combined with hydrochloric acid leaching. There appears to be no economic advantage to preconcentration in combination with sulphuric acid leaching of the ore

Selective Flow-Injection Quantification of Ultra-trace Amounts of Cr(VI) via On-line Complexation and Preconcentration with APDC Followed by Determination by Electrothermal Atomic Absorption Spectrometry

DEFF Research Database (Denmark)

Nielsen, Steffen; Hansen, Elo Harald

1998-01-01

A rapid, sensitive and selective time-based flow injection (FI) preconcentration procedure is described for the determination of ultra-trace amounts of Cr(VI) via on-line reaction with ammonium pyrrolidine dithiocarbamate (APDC) and formation of the Cr(VI)-PDC complex. The preconcentration...... to direct introduction of 55 mu l samples, yielding a detection limit (3 sigma) of 4.2 ng l(-1). The sample frequency was 21.2 samples per hour. The proposed method was evaluated by analyzing drinking water, a NIST Cr(VI)-reference material and synthetic sea water. A major contribution to successful...

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

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.)

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...

On-line preconcentration system using a minicolumn of polyurethane foam loaded with Me-BTABr for zinc determination by Flame Atomic Absorption Spectrometry

International Nuclear Information System (INIS)

Azevedo Lemos, Valfredo; Nei Lopes dos Santos, Walter; Silva Santos, Juracir; Bezerra de Carvalho, Marcilio

2003-01-01

In the present paper, an on-line system for preconcentration and determination of zinc by Flame Atomic Absorption Spectrometry (FAAS) is proposed. It is based in the sorption of zinc(II) ions on a minicolumn packed with polyurethane foam loaded with 2-[2'-(6-methyl-benzothiazolylazo)]-4-bromophenol (Me-BTABr) reagent. Chemical and flow variables as pH effect, sample flow rate and eluent concentration were optimized using univariate methodology. The results demonstrated that zinc can determinate using the sample pH in the range of 6.5-9.2, sample flow rate of 6.0 ml min -1 , and the elution step using 0.10 mol l -1 hydrochloric acid solution at flow rate of 5.5 ml min -1 . In these conditions, an enrichment factor of 23 and a sampling rate of 48 samples per hour were achieved. The detection limit (DL, 3σ) as IUPAC recommendation was 0.37 μg l -1 and the precision (assessed as the relative standard deviation, R.S.D.) reached values of 5.9-1.8% in zinc solutions of 1.0-10.0 μg l -1 concentration, respectively. The method was successfully applied to the determination of trace amounts of zinc in natural water samples from Salvador (Brazil)

From carbon nanostructures to high-performance sorbents for chromatographic separation and preconcentration

International Nuclear Information System (INIS)

Postnov, V N; Rodinkov, O V; Moskvin, L N; Novikov, A G; Bugaichenko, A S; Krokhina, O A

2016-01-01

Information on carbon nanostructures (fullerenes, nanotubes, graphene, nanodiamond and nanodispersed active carbon) used to develop high-performance sorbents of organics and heavy metal ions from aqueous solutions is collected and analyzed. The advantages in the synthesis of hybrid carbon nanostructures and the possibilities of surface modification of these systems in order to carry out fast sorption pre-concentration are considered. Prospects for application of these materials in sorption technologies and analytical chemistry are discussed. The bibliography includes 364 references

Sequential injection on-line matrix removal and trace metal preconcentration using a PTFE beads packed column as demonstrated for the determination of cadmium by electrothermal atomic absorption spectrometry

DEFF Research Database (Denmark)

Wang, Jianhua; Hansen, Elo Harald

2002-01-01

A sequential injection (SI) on-line matrix removal and trace metal preconcentration procedure by using a novel microcolumn packed with PTFE beads is described, and demonstrated for trace cadmium analysis with detection by electrothermal atomic absorption spectrometry (ETAAS). The analyte...

Preconcentration system for cadmium and lead determination in environmental samples using polyurethane foam/Me-BTANC

International Nuclear Information System (INIS)

Moreira Gama, Ednilton; Silva Lima, Adriana da; Azevedo Lemos, Valfredo

2006-01-01

In this work, polyurethane foam (PUF) loaded with 2-(6'-methyl-2'-benzothiazolylazo)chromotropic acid (Me-BTANC) was packed in a minicolumn and it was used in an on-line preconcentration system for cadmium and lead determination. Optimum hydrodynamic and chemical conditions for metal sorption were investigated. The effects of several foreign substances on the adsorption of cadmium and lead were also reported. The enrichment factor obtained was 37 (Cd and Pb) for 180 s preconcentration time. The proposed procedures allowed the determination of metals with detection limits (3σ) of 0.80 and 3.75 μg L -1 (0.10 and 0.47 μg g -1 of solid sample) for cadmium and lead, respectively. The precision of the procedures was also calculated: 3.1 (Cd 10 μg L -1 ) and 4.4% (Pb 100 μg L -1 ). The accuracy of the procedure was checked by analysis of the certified reference materials Spinach Leaves and Fish Tissue. Cadmium and lead contents in environmental samples (black tea, spinach leaves, natural and tap water) were determined by applying the proposed procedure

Separation and preconcentration of cadmium ions in natural water using a liquid membrane system with 2-acetylpyridine benzoylhydrazone as carrier by flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Granado-Castro, M.D.; Galindo-Riano, M.D. E-mail: dolores.galindo@uca.es; Garcia-Vargas, Manuel

2004-04-30

A method for the determination of Cd in natural water by flame atomic absorption spectrometry after separation and preconcentration with a bulk liquid membrane containing 2-acetylpyridine benzoylhydrazone as mobile carrier dissolved in toluene has been developed. Effects of carrier concentration, volume of organic phase and pH of feed and receiving solutions on the flux for Cd across the membrane have been studied, being optimized by the modified simplex method. Optimum values for these variables were: carrier concentration of 0.84 g l{sup -1}, 74 ml of toluene, pH 7.8 in the feed solution and 0.06 mol l{sup -1} of HNO{sub 3} in the receiving solution, allowing a preconcentration factor of 17.9. The preconcentration step required 7 h to be accomplished. The recovery of Cd at optimum conditions was 101.0{+-}2.7%, even with saline matrix, with good relative standard deviation (2.5%) at 95% confidence level. The detection limit of blank sample was 6 ng l{sup -1} of Cd. The method was validated using a certified reference material (TMDA-62) and also applied successfully to the analysis of Cd in four samples of seawater collected from the coast of Huelva (Spain). The relative errors of determinations were -7.6% for certified reference material and ranging between +2.4 and +7.1%, for samples of seawater (obtained between the results of the proposed and differential pulse anodic stripping voltammetry methods)

Very low-energy conversion electron detection (VLECED) system at the isocele on-line isotope separator, Orsay

International Nuclear Information System (INIS)

Kilcher, P.; Sauvage, J.; Munsch, J.; Obert, J.; Caruette, A.; Ferro, A.; Boissier, G.; Fournet-Fayas, J.; Ducourtieux, M.; Landois, G.

1988-01-01

A system designed and installed at the on-line isotope separator ISOCELE II allows the high resolution detection of low-energy conversion electrons (down to 1 keV) emitted by mass separated radioactive sources: the use of a special tape transport permits both the slowing down of the incoming beam of radioactive ions up to a collection point and the acceleration of the electrons emitted by the collected sources brought to a flat magnetic spectrograph. Typical spectra so obtained are presented

Flow-injection determination of thorium and uranium after on-line ion-exchange preconcentration in Dowex 50-X8

International Nuclear Information System (INIS)

Perez Pavon, J.L.; Garcia Pinto, C.G.; Rodriguez Garcia, Estrella; Moreno Cordero, Bernardo

1992-01-01

The preconcentration of thorium and uranium on Dowex 50-X8 was studied as a method for the preconcentration of these cations prior to their determination by flow injection with spectrophotometric detection using Arsenazo III in 3.6 M HCl stabilized with Triton X-100 as chromogenic reagent. The preconcentration device is a minicolumn included in the sample loop of the injection valve. A second valve contains a reducing minicolumn filled with lead powder to reduce U(VI) to U(IV) before the confluence of the sample with the reagent stream. The method can be applied to samples containing 0.5-100 μg l -1 and was tested with different spiked water samples. (author). 15 refs.; 3 figs.; 3 tabs

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)

Flow injection preconcentration system using a new functionalized resin for determination of cadmium and nickel in tobacco samples

International Nuclear Information System (INIS)

Lemos, Valfredo Azevedo; Novaes, Cleber Galvao; Lima, Adriana da Silva; Vieira, Daniel Rodrigues

2008-01-01

A solid-phase extraction method combined with flow injection (FI) on-line flame atomic absorption spectrometry (FAAS) for the determination of cadmium and nickel in tobacco samples is presented. The 2-aminothiophenol functionalized Amberlite XAD-4 (AT-XAD) resin was synthesized by covalent coupling of the ligand with the copolymer through a methylene group. A minicolumn packed with AT-XAD was connected into the automated on-line preconcentration system. Elution of metal ions from minicolumn can be made with 0.50 mol L -1 hydrochloric acid solution. With a consumption of 21.0 mL of sample solution, detection limits (3 s) of 0.3 (Cd) and 0.8 μg L -1 (Ni) were achieved at a sample throughput of 18 h -1 . Enrichment factors (EF) of 99 (cadmium) and 43 (nickel) were obtained compared with the slope of the linear portion of the calibration curves before and after preconcentration. The contents of Cd and Ni in a certified reference material (NIST 1570a, spinach leaves) determined by the present method was in good agreement with the certified value. The developed procedure was also successfully applied to the determination of Cd and Ni in local tobacco samples

Separation and preconcentration of copper in environmental samples on Amberlite XAD-8 resin after complexation with a carbothioamide derivative

Directory of Open Access Journals (Sweden)

Hamide Elvan

2013-01-01

Full Text Available A new solid phase extraction (SPE method has been developed for the selective separation and preconcentration of Cu (II ions in food and water samples prior to its flame atomic absorption spectrometry determination. The method is based on the adsorption of the Cu(II - 2-{[4-Amino-3-(4-methylphenyl-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]acetyl}-N-phenyl hydrazinecarbothioamide complex on Amberlite XAD-8 resin. The metal complex retained on the resin was eluted with 7.5 mL of 2.0 mol L-1 HCl in acetone. The optimum conditions for the SPE of Cu(II ions were investigated, and the method was subsequently applied to sea water, stream water, rice, tea, and tobacco samples for the determination of Cu(II levels.

Online preconcentration ICP-MS analysis of rare earth elements in seawater

Science.gov (United States)

Hathorne, Ed C.; Haley, Brian; Stichel, Torben; Grasse, Patricia; Zieringer, Moritz; Frank, Martin

2012-01-01

The rare earth elements (REEs) with their systematically varying properties are powerful tracers of continental inputs, particle scavenging intensity and the oxidation state of seawater. However, their generally low (˜pmol/kg) concentrations in seawater and fractionation potential during chemical treatment makes them difficult to measure. Here we report a technique using an automated preconcentration system, which efficiently separates seawater matrix elements and elutes the preconcentrated sample directly into the spray chamber of an ICP-MS instrument. The commercially available "seaFAST" system (Elemental Scientific Inc.) makes use of a resin with ethylenediaminetriacetic acid and iminodiacetic acid functional groups to preconcentrate REEs and other metals while anions and alkali and alkaline earth cations are washed out. Repeated measurements of seawater from 2000 m water depth in the Southern Ocean allows the external precision (2σ) of the technique to be estimated at mine water reference materials diluted with a NaCl matrix with recommended values in the literature. This makes the online preconcentration ICP-MS technique advantageous for the minimal sample preparation required and the relatively small sample volume consumed (7 mL) thus enabling large data sets for the REEs in seawater to be rapidly acquired.

Combined micro-droplet and thin-film-assisted pre-concentration of lead traces for on-line monitoring using anodic stripping voltammetry.

Science.gov (United States)

Belostotsky, Inessa; Gridin, Vladimir V; Schechter, Israel; Yarnitzky, Chaim N

2003-02-01

An improved analytical method for airborne lead traces is reported. It is based on using a Venturi scrubber sampling device for simultaneous thin-film stripping and droplet entrapment of aerosol influxes. At least threefold enhancement of the lead-trace pre-concentration is achieved. The sampled traces are analyzed by square-wave anodic stripping voltammetry. The method was tested by a series of pilot experiments. These were performed using contaminant-controlled air intakes. Reproducible calibration plots were obtained. The data were validated by traditional analysis using filter sampling. LODs are comparable with the conventional techniques. The method was successfully applied to on-line and in situ environmental monitoring of lead.

Combined micro-droplet and thin-film-assisted pre-concentration of lead traces for on-line monitoring using anodic stripping voltammetry

Energy Technology Data Exchange (ETDEWEB)

Belostotsky, Inessa; Gridin, Vladimir V.; Schechter, Israel; Yarnitzky, Chaim N. [Department of Chemistry, Technion Israel Institute of Technology, 32000, Haifa (Israel)

2003-02-01

An improved analytical method for airborne lead traces is reported. It is based on using a Venturi scrubber sampling device for simultaneous thin-film stripping and droplet entrapment of aerosol influxes. At least threefold enhancement of the lead-trace pre-concentration is achieved. The sampled traces are analyzed by square-wave anodic stripping voltammetry. The method was tested by a series of pilot experiments. These were performed using contaminant-controlled air intakes. Reproducible calibration plots were obtained. The data were validated by traditional analysis using filter sampling. LODs are comparable with the conventional techniques. The method was successfully applied to on-line and in situ environmental monitoring of lead. (orig.)

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.

Magnetic separation for pre-concentration of uranium values from copper plant tailings

International Nuclear Information System (INIS)

Jha, R.S.; Sreenivas, T.; Natarajan, R.; Sridhar, U.; Rao, N.K.

1991-01-01

Using the paramagnetic character of uranium minerals, the preconcentration of uranium bearing ores and copper plant tailings of Singhbhum area have been investigated in a pilot plant scale wet high intensity magnetic separator (WHIMS). The variables studied include magnetic field intensity, matrix drum speed feed slurry flow rate and its pulp density. The results of these investigations have shown that 75-85% of the contained uranium values could be recovered in 45-55% weight in the magnetic fraction in the case of copper plant tailings from Rakha, Surda and Mosabani. The losses in the non magnetics were primarily due to the ultrafine liberated uraninite particles not collected by WHIMS due to machine limitations and the values occurring as fine inclusions in quartz. Improved recovery can be obtained by offering higher field gradients and preventing loss of very fine liberated uranium values. High gradient magnetic separator (HGMS) offers higher field gradients. A test sample of Mosabani copper tailings studied at the Sala Magnetic Inc in HGMS has indicated superior results in comparison to WHIMS. (author). 7 refs., 3 figs., 6 tabs

Efficiency of an on-line isotope separator system employing cooled and NaCl-loaded He-jet methods

International Nuclear Information System (INIS)

Aeystoe, J.; Rantala, V.; Valli, K.; Hillebrand, S.; Kortelahti, M.; Eskola, K.; Raunemaa, T.

1976-01-01

A pure helium-jet at liquid nitrogen temperature coupled to a Nielsen type ion source, and a NaCl-loaded helium-jet coupled to a hollow-cathode ion source have been investigated as means to connect a cyclotron target chamber on-line to a mass separator. Technical details and performances of some critical parts of the system are described. Total separation efficiencies measured under various experimental conditions for several nuclides vary between 0.01 and 1.0%. (Auth.)

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.

Characteristics of a gas-jet transport system for an on-line isotope separator

International Nuclear Information System (INIS)

Kawade, K.; Yamamoto, H.; Amano, H.; Hanada, M.; Katoh, T.; Okano, K.; Kawase, Y.; Fujiwara, I.

1982-01-01

Basic characteristics of a gas-jet transport system for an on-line isotope separator have been investigated using a 252 Cf source and a 235 U fission source. The transport efficiency of fission products through a capillary has been measured to be about 60% for the 235 U fission source. The sweep-out time of fission products through a target chamber and the transit time through a capillary have been measured for He, N 2 and CO 2 gases at several pressures. The measured sweep-out times have been almost equal to the exchange over time of the gas. The transit times have been found to be reasonably predicted by calculations. The transport system has been incorporated into the KUR-ISOL and is used for the study of short-lived nuclei. (orig.)

Analysis of hydroxamate siderophores in soil solution using liquid chromatography with mass spectrometry and tandem mass spectrometry with on-line sample preconcentration.

Science.gov (United States)

Olofsson, Madelen A; Bylund, Dan

2015-10-01

A liquid chromatography with electrospray ionization mass spectrometry method was developed to quantitatively and qualitatively analyze 13 hydroxamate siderophores (ferrichrome, ferrirubin, ferrirhodin, ferrichrysin, ferricrocin, ferrioxamine B, D1 , E and G, neocoprogen I and II, coprogen and triacetylfusarinine C). Samples were preconcentrated on-line by a switch-valve setup prior to analyte separation on a Kinetex C18 column. Gradient elution was performed using a mixture of an ammonium formate buffer and acetonitrile. Total analysis time including column conditioning was 20.5 min. Analytes were fragmented by applying collision-induced dissociation, enabling structural identification by tandem mass spectrometry. Limit of detection values for the selected ion monitoring method ranged from 71 pM to 1.5 nM with corresponding values of two to nine times higher for the multiple reaction monitoring method. The liquid chromatography with mass spectrometry method resulted in a robust and sensitive quantification of hydroxamate siderophores as indicated by retention time stability, linearity, sensitivity, precision and recovery. The analytical error of the methods, assessed through random-order, duplicate analysis of soil samples extracted with a mixture of 10 mM phosphate buffer and methanol, appears negligible in relation to between-sample variations. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Two-Dimensional Capillary Electrophoresis with On-Line Sample Preparation and Cyclodextrin Separation Environment for Direct Determination of Serotonin in Human Urine.

Science.gov (United States)

Piešťanský, Juraj; Maráková, Katarína; Mikuš, Peter

2017-10-07

An advanced two-dimensional capillary electrophoresis method, based on on-line combination of capillary isotachophoresis and capillary zone electrophoresis with cyclodextrin additive in background electrolyte, was developed for effective determination of serotonin in human urine. Hydrodynamically closed separation system and large bore capillaries (300-800 µm) were chosen for the possibility to enhance the sample load capacity, and, by that, to decrease limit of detection. Isotachophoresis served for the sample preseparation, defined elimination of sample matrix constituents (sample clean up), and preconcentration of the analyte. Cyclodextrin separation environment enhanced separation selectivity of capillary zone electrophoresis. In this way, serotonin could be successfully separated from the rest of the sample matrix constituents migrating in capillary zone electrophoresis step so that human urine could be directly (i.e., without any external sample preparation) injected into the analyzer. The proposed method was successfully validated, showing favorable parameters of sensitivity (limit of detection for serotonin was 2.32 ng·mL -1 ), linearity (regression coefficient higher than 0.99), precision (repeatability of the migration time and peak area were in the range of 0.02-1.17% and 5.25-7.88%, respectively), and recovery (ranging in the interval of 90.0-93.6%). The developed method was applied for the assay of the human urine samples obtained from healthy volunteers. The determined concentrations of serotonin in such samples were in the range of 12.4-491.2 ng·mL -1 that was in good agreement with literature data. This advanced method represents a highly effective, reliable, and low-cost alternative for the routine determination of serotonin as a biomarker in human urine.

Isocele I, the Orsay synchrocyclotron on-line separator

International Nuclear Information System (INIS)

Caruette, A.; Ferro, A.; Foucher, R.

1976-01-01

The main characteristics of the isotope separator Isocele 1 are described. This medium current separator was on line with the Orsay synchrocyclotron (155 MeV p, or 210 MeV 3 He) from March 1974 up to May 1975. Results obtained with different targets (Au, Bi, Er, Pt, Sn, Th) are summarized. They confirm the efficiency of medium current separators of this type [fr

Tea-industry waste activated carbon, as a novel adsorbent, for separation, preconcentration and speciation of chromium

Energy Technology Data Exchange (ETDEWEB)

Duran, Celal, E-mail: cduran@ktu.edu.tr [Department of Chemistry, Faculty of Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey); Ozdes, Duygu [Department of Chemistry, Faculty of Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey); Gundogdu, Ali [Faculty of Engineering, Food Department of Food Engineering, 29100, Guemueshane (Turkey); Imamoglu, Mustafa [Department of Chemistry, Faculty of Arts and Sciences, Sakarya University, 54187 Sakarya (Turkey); Senturk, Hasan Basri [Department of Chemistry, Faculty of Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey)

2011-02-28

Activated carbon was produced from tea-industry wastes (TIWAC) and employed as a low cost and effective solid phase material for the separation, preconcentration and speciation of chromium species without using a complexing agent, prior to determination by flame atomic absorption spectrometry (FAAS). The characterization of TIWAC was performed by utilizing several techniques such as Fourier Transform Infrared (FTIR) Spectroscopy, Scanning Electron Microscopy (SEM), and elemental analysis. The adsorption experiments were conducted in a batch adsorption technique. Under the experimental conditions, Cr(VI) adsorption amount was nearly equal to zero, however the adsorption percentage of Cr(III) was in the range of 95-100%. Therefore total chromium was determined after the reduction of Cr(VI) to Cr(III) and Cr(VI) was calculated by subtracting Cr(III) concentration from total chromium concentration. The suitable conditions for adsorption and speciation processes were evaluated in terms of pH, eluent type and volume, TIWAC concentration, adsorption and desorption contact time, etc. Adsorption capacity of TIWAC was found to be 61.0 mg g{sup -1}. The detection limit for Cr(III) was found to be 0.27 {mu}g L{sup -1} and the preconcentration factor was 50 for 200 mL of sample volume. The procedure was applied to the determination and speciation of chromium in stream, tap and sea water. Also, the proposed method was applied to total chromium preconcentration in microwave digested tobacco and dried eggplant samples with satisfactory results. The method was validated by analyzing certified reference materials (CRM-TMDW-500 Drinking Water and CRM-SA-C Sandy Soil C) and the results were in good agreement with the certified values.

Tea-industry waste activated carbon, as a novel adsorbent, for separation, preconcentration and speciation of chromium

International Nuclear Information System (INIS)

Duran, Celal; Ozdes, Duygu; Gundogdu, Ali; Imamoglu, Mustafa; Senturk, Hasan Basri

2011-01-01

Activated carbon was produced from tea-industry wastes (TIWAC) and employed as a low cost and effective solid phase material for the separation, preconcentration and speciation of chromium species without using a complexing agent, prior to determination by flame atomic absorption spectrometry (FAAS). The characterization of TIWAC was performed by utilizing several techniques such as Fourier Transform Infrared (FTIR) Spectroscopy, Scanning Electron Microscopy (SEM), and elemental analysis. The adsorption experiments were conducted in a batch adsorption technique. Under the experimental conditions, Cr(VI) adsorption amount was nearly equal to zero, however the adsorption percentage of Cr(III) was in the range of 95-100%. Therefore total chromium was determined after the reduction of Cr(VI) to Cr(III) and Cr(VI) was calculated by subtracting Cr(III) concentration from total chromium concentration. The suitable conditions for adsorption and speciation processes were evaluated in terms of pH, eluent type and volume, TIWAC concentration, adsorption and desorption contact time, etc. Adsorption capacity of TIWAC was found to be 61.0 mg g -1 . The detection limit for Cr(III) was found to be 0.27 μg L -1 and the preconcentration factor was 50 for 200 mL of sample volume. The procedure was applied to the determination and speciation of chromium in stream, tap and sea water. Also, the proposed method was applied to total chromium preconcentration in microwave digested tobacco and dried eggplant samples with satisfactory results. The method was validated by analyzing certified reference materials (CRM-TMDW-500 Drinking Water and CRM-SA-C Sandy Soil C) and the results were in good agreement with the certified values.

Development of a portable preconcentrator/ion mobility spectrometer system for the trace detection of narcotics

Energy Technology Data Exchange (ETDEWEB)

Parmeter, J.E.; Custer, C.A.

1997-08-01

This project was supported by LDRD funding for the development and preliminary testing of a portable narcotics detection system. The system developed combines a commercial trace detector known as an ion mobility spectrometer (IMS) with a preconcentrator originally designed by Department 5848 for the collection of explosives molecules. The detector and preconcentrator were combined along with all necessary accessories onto a push cart, thus yielding a fully portable detection unit. Preliminary testing with both explosives and narcotics molecules shown that the system is operational, and that it can successfully detect drugs as marijuana, methamphetamine (speed), and cocaine based on their characteristics IMS signatures.

On-line sample-pre-treatment schemes for trace-level determinations of metals by coupling flow injection or sequential injection with ICP-MS

DEFF Research Database (Denmark)

Wang, Jianhua; Hansen, Elo Harald

2003-01-01

a polytetrafluoroethylene (PTFE) knotted reactor (KR), solvent extraction-back extraction and hydride/vapor generation. It also addresses a novel, robust approach, whereby the protocol of SI-LOV-bead injection (BI) on-line separation and pre-concentration of ultra-trace levels of metals by a renewable microcolumn...

Preconcentration of traces of radionuclides and elements with foamed polyurethane sorbents in the analysis of environmental samples

International Nuclear Information System (INIS)

Palagyi, S.; Braun, T.

1986-01-01

The importance of preconcentration and the permanent need of efficient preconcentrating agents in environmental analysis are pointed out. Foamed polyurethane sorbents draw attention as novel agents in separation chemistry. A survey is presented of recent applications of unloaded and reagent-loaded open-cell type resilient polyurethane foams in the separation and preconcentration of radionuclides from environmental samples, and of the latest uses of these foams in the preconcentration and detection of traces of some, mainly inorganic materials in environmental samples, using radioanalytical techniques. Possible future uses of polyurethane foams in trace element detection in environmental analysis are outlined. (author)

Preconcentration of silver as silver xanthate on activated carbon

International Nuclear Information System (INIS)

Ramadevi, P.; Naidu, U.V.; Naidu, G.R.K.

1988-01-01

Silver from aqueous solution was preconcentrated by adsorption on activated carbon as silver xanthate. Factors influencing the adsorption of silver were studied. Optimum conditions for the preconcentration of silver were established. (author) 9 refs.; 3 tabs

Trace mercury determination in drinking and natural water after preconcentration and separation by DLLME-SFO method coupled with cold vapor atomic absorption spectrometry

OpenAIRE

Abdollahi Atousa; Amirkavehei Mooud; Gheisari Mohammad Mehdi; Tadayon Fariba

2014-01-01

A novel dispersive liquid–liquid microextraction based on solidification of floating organic drop (DLLME-SFO) for simultaneous separation/preconcentration of ultra trace amounts of mercury was used. A method based on amalgamation was used for collection of gaseous mercury on gold coated sand (Gold trap). The concentration of mercury was determined by cold vapor atomic absorption spectrometry (CV-AAS). The DLLME-SFO behavior of mercury by using dithizone as complexing agent was systematically ...

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.

Separation, preconcentration and determination of silver ion from water samples using silica gel modified with 2,4,6-trimorpholino-1,3,5-triazin

International Nuclear Information System (INIS)

Madrakian, Tayyebeh; Afkhami, Abbas; Zolfigol, Mohammad Ali; Solgi, Mohammad

2006-01-01

A new modified silica gel using 2,4,6-trimorpholino-1,3,5-triazin was used for separation, preconcentration and determination of silver ion in natural water by atomic absorption spectrometry (AAS). This new bonded silica gel was used as an effective sorbent for the solid-phase extraction (SPE) of silver ion from aqueous solutions. Experimental conditions for effective adsorption of trace levels of silver ion were optimized with respect to different experimental parameters in column process. Common coexisting ions did not interfere with the separation and determination of silver at pH 3.5 so that silver ion completely adsorbed on the column. The preconcentration factor is 130 (1 mL elution volume for a 130 mL sample volume). The relative standard deviation (R.S.D.) under optimum conditions is 3.03% (n = 5). The accuracy of the method was estimated by using spring and tap water samples that were spiked with different amounts of silver ion. The adsorption isotherm of silver ion was obtained. The capacity of the sorbent at optimum conditions has been found to be 384 μg of silver per gram of sorbent

Determination of Ultra-Trace Amounts of Selenium(IV) by Flow Injection Hydride Generation Atomic Absorption Spectrometry with On-line Preconcentration by Co-precipitation with Lanthanium Hydroxide. Part II. On-line Addition of Coprecipating Agent

DEFF Research Database (Denmark)

Nielsen, Steffen; Sloth, Jens Jørgen; Hansen, Elo Harald

1996-01-01

-line and merged with an ammonium buffer solution of pH 9.1, which promotes precipitation and quantitative collection on the inner walls of an incorporated knotted Microline reactor. The Se(IV) preconcentrated by coprecipitation with the generated lanthanum hydroxide precipitate is subsequently eluted...... with hydrochloric acid, allowing an ensuing determination via hydride generation. At different sample flow rates, i.e., 4.8, 6.4 and 8.8 ml/min, enrichment factors of 30, 40 and 46, respectively, were obtained at a sampling frequency of 33 samples/h. The detection limit (3s) was 0.005 µg/l at a sample flow rate...

On-line separation of refractory hafnium and tantalum isotopes at the ISOCELE separator

CERN Document Server

Liang, C F; Obert, J; Paris, P; Putaux, J C

1981-01-01

By chemical evaporation technique, neutron deficient hafnium nuclei have been on-line separated at the ISOCELE facility, from the isobar rare-earth elements, in the metal-fluoride HfF/sub 3//sup +/ ion form. Half-lives of /sup 162-165/Hf have been measured. Similarly, tantalum has been selectively separated on the TaF/sub 4//sup +/ form. (4 refs) .

Extraction and preconcentration of trace levels of cobalt using functionalized magnetic nanoparticles in a sequential injection lab-on-valve system with detection by electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Wang Yang; Luo Xiaoyu; Tang Jie; Hu Xiaoya; Xu Qin; Yang Chun

2012-01-01

Graphical abstract: An approach to performing extraction and preconcentration employing functionalized magnetic particles for the determination of cobalt in the sequential injection lab-on-valve system using detection by electrothermal atomic absorption spectrometry. Highlights: ► New SPE method for cobalt separation/preconcentration was reported. ► Functionalized magnetic nanoparticles were used as adsorbent. ► Extraction, elution, and detection procedures were performed in the LOV system. ► This automatic extraction technique provided a good platform for metal analysis. - Abstract: A new approach to performing extraction and preconcentration employing functionalized magnetic nanoparticles for the determination of trace metals is presented. Alumina-coated iron oxide nanoparticles were synthesized and used as the solid support. The nanoparticles were functionalized with sodium dodecyl sulfate and used as adsorbents for solid phase extraction of the analyte. Extraction, elution, and detection procedures were performed sequentially in the sequential injection lab-on-valve (SI-LOV) system followed by electrothermal atomic absorption spectrometry (ETAAS). Mixtures of hydrophobic analytes were successfully extracted from solution using the synthesized magnetic adsorbents. The potential use of the established scheme was demonstrated by taking cobalt as a model analyte. Under the optimal conditions, the calibration curve showed an excellent linearity in the concentration range of 0.01–5 μg L −1 , and the relative standard deviation was 2.8% at the 0.5 μg L −1 level (n = 11). The limit of detection was 6 ng L −1 with a sampling frequency of 18 h −1 . The present method has been successfully applied to cobalt determination in water samples and two certified reference materials.

Development of an ion guide coupled to an on-line isotope separation system on Sara. Identification and study of isospin exotic nuclei at Isolde and Sara

International Nuclear Information System (INIS)

Bouldjedri, A.

1992-06-01

This work is concerned with the study of exotic nuclei located on both sides of the stability-line and known as neutron rich and neutron deficient respectively. For the former, produced by alpha particle-induced fission, an on-line isotope separation with an ion guide (IGISOL) has been developed and submitted to several off-line and on-line optimization tests showing capacity to spectroscopic studies. In the case of neutron deficient nuclei near the magicity Z=82, 182 Tl(3s) has been identified and its decaying modes and those of 183 Tl ground state, studied, using the on-line separator ISOLDE. On the other hand, the β decay of 172,175 Ir produced in 32 S induced reaction is studied using a helium jet system on the SARA accelerator. Existence of isomers is derived from half-lives measurements

Meniscus Membranes For Separation

Science.gov (United States)

Dye, Robert C.; Jorgensen, Betty; Pesiri, David R.

2005-09-20

Gas separation membranes, especially meniscus-shaped membranes for gas separations are disclosed together with the use of such meniscus-shaped membranes for applications such as thermal gas valves, pre-concentration of a gas stream, and selective pre-screening of a gas stream. In addition, a rapid screening system for simultaneously screening polymer materials for effectiveness in gas separation is provided.

Meniscus membranes for separations

Science.gov (United States)

Dye, Robert C [Irvine, CA; Jorgensen, Betty [Jemez Springs, NM; Pesiri, David R [Aliso Viejo, CA

2004-01-27

Gas separation membranes, especially meniscus-shaped membranes for gas separations are disclosed together with the use of such meniscus-shaped membranes for applications such as thermal gas valves, pre-concentration of a gas stream, and selective pre-screening of a gas stream. In addition, a rapid screening system for simultaneously screening polymer materials for effectiveness in gas separation is provided.

Development of on line automatic separation device for apple and sleeve

Science.gov (United States)

Xin, Dengke; Ning, Duo; Wang, Kangle; Han, Yuhang

2018-04-01

Based on STM32F407 single chip microcomputer as control core, automatic separation device of fruit sleeve is designed. This design consists of hardware and software. In hardware, it includes mechanical tooth separator and three degree of freedom manipulator, as well as industrial control computer, image data acquisition card, end effector and other structures. The software system is based on Visual C++ development environment, to achieve localization and recognition of fruit sleeve with the technology of image processing and machine vision, drive manipulator of foam net sets of capture, transfer, the designated position task. Test shows: The automatic separation device of the fruit sleeve has the advantages of quick response speed and high separation success rate, and can realize separation of the apple and plastic foam sleeve, and lays the foundation for further studying and realizing the application of the enterprise production line.

MSFIA-LOV system for {sup 226}Ra isolation and pre-concentration from water samples previous radiometric detection

Energy Technology Data Exchange (ETDEWEB)

Rodríguez, Rogelio [Environmental Radioactivity Laboratory (LaboRA), University of the Balearic Islands, Cra. Valldemossa km 7.5, 07122, Palma (Spain); Environment and Energy Department, Advanced Materials Research Center (CIMAV) S.C., Miguel de Cervantes 120, Chihuahua, Chih. 31136 (Mexico); Borràs, Antoni [Environmental Radioactivity Laboratory (LaboRA), University of the Balearic Islands, Cra. Valldemossa km 7.5, 07122, Palma (Spain); Leal, Luz [Environment and Energy Department, Advanced Materials Research Center (CIMAV) S.C., Miguel de Cervantes 120, Chihuahua, Chih. 31136 (Mexico); Cerdà, Víctor [Department of Chemistry, University of the Balearic Islands, Cra. Valldemossa km 7.5, 07122, Palma (Spain); Ferrer, Laura, E-mail: laura.ferrer@uib.es [Environmental Radioactivity Laboratory (LaboRA), University of the Balearic Islands, Cra. Valldemossa km 7.5, 07122, Palma (Spain)

2016-03-10

An automatic system based on multisyringe flow injection analysis (MSFIA) and lab-on-valve (LOV) flow techniques for separation and pre-concentration of {sup 226}Ra from drinking and natural water samples has been developed. The analytical protocol combines two different procedures: the Ra adsorption on MnO{sub 2} and the BaSO{sub 4} co-precipitation, achieving more selectivity especially in water samples with low radium levels. Radium is adsorbed on MnO{sub 2} deposited on macroporous of bead cellulose. Then, it is eluted with hydroxylamine to transform insoluble MnO{sub 2} to soluble Mn(II) thus freeing Ra, which is then coprecipitated with BaSO{sub 4}. The {sup 226}Ra can be directly detected in off-line mode using a low background proportional counter (LBPC) or through a liquid scintillation counter (LSC), after performing an on-line coprecipitate dissolution. Thus, the versatility of the proposed system allows the selection of the radiometric detection technique depending on the detector availability or the required response efficiency (sample number vs. response time and limit of detection). The MSFIA-LOV system improves the precision (1.7% RSD), and the extraction frequency (up to 3 h{sup −1}). Besides, it has been satisfactorily applied to different types of water matrices (tap, mineral, well and sea water). The {sup 226}Ra minimum detectable activities (LSC: 0.004 Bq L{sup −1}; LBPC: 0.02 Bq L{sup −1}) attained by this system allow to reach the guidance values proposed by the relevant international agencies e.g. WHO, EPA and EC. - Highlights: • Automatic, rapid and selective method for {sup 226}Ra extraction/pre-concentration from water. • MSFIA-LOV system performs a sample clean-up prior to {sup 226}Ra radiometric detection. • {sup 226}Ra sample preparation allows using two radiometric detectors (LBPC and LSC). • Environmental levels of {sup 226}Ra are easily quantified. • High sensitivity and selectivity are achieved, reaching the

On-line system for preconcentration and determination of metals in vegetables by Inductively Coupled Plasma Optical Emission Spectrometry

International Nuclear Information System (INIS)

Bezerra, Marcos A.; Santos, Walter N.L. dos; Lemos, Valfredo A.; Korn, Maria das Gracas A.; Ferreira, Sergio L.C.

2007-01-01

A procedure has been developed for the simultaneous determination of trace amounts of cadmium, copper, chromium, nickel and lead in digested vegetable samples. The method involves solid-phase extraction of the metals using a minicolumn of Amberlite XAD-4 modified with dihydroxybenzoic acid (DHB) and detection by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). The elution of the metals from minicolumn was performed with 1.0 mol L -1 hydrochloric acid. Variables associated with flow preconcentration system performance, such as pH, buffer concentration, eluent concentration and sampling flow rate, were optimized. The developed procedure provides enrichment factors of 100, 72, 16, 91 and 53, for cadmium, copper, chromium, nickel and lead, respectively. Detection limits (3σ B ) were 0.02 (Cd), 0.23 (Cu), 0.58 (Cr), 0.060 (Ni) and 0.54 (Pb) μg L -1 . The procedure was applied for determination of metals in samples of guarana and cabbage. The accuracy of the method was checked by the analysis of a certified reference material (NIST 1571, Orchard leaves). Results found were in agreement with certified values

Determination of uranium in natural waters and high-purity aluminum by flow-injection on-line preconcentration and ICP-MS detection

International Nuclear Information System (INIS)

Seki, Tatsuya; Oguma, Koichi

2004-01-01

A flow injection method has been developed for the determination of uranium is natural waters and high-purity aluminum by use of on-line preconcentration on a U/TEVA TM column and ICP-MS detection. The sample solution prepared as a nitric acid solution in 3 mol l -1 was passed through the U/TEVA TM column to collect uranium and uranium adsorbed was eluted with 0.1 mol l -1 nitric acid. The effluent was introduced directly into the nebulizer of the ICP-MS and 238 U was measured. The detection limit, calculated as 3-times the standard deviation of the background noise, was 3pg and the sample throughput was about 10 per hour. The proposed method was successfully applied to the determination of uranium in river-water reference materials, a seawater reference material and high-purity aluminum reference materials. (author)

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.

The on-line graph processing study on phase separation of two-phase flow in T-tube

International Nuclear Information System (INIS)

Qian Yong; Xu Jijun; Yang Zhilin; Chen Yifen

1997-01-01

The on-line graph processing measure system is equipped with and experimental study of phase separation of air-water bubbly flow in the horizontal T-junction is carried out. For the first time, the author have found and defined the new type of complete phase separation, by the visual experiment, which shows that under certain conditions, the air flow entering the T junction will flow into the run outlet completely, which had never been reported in the literature Also, the pressure wave feed back effect and the branch bubble flow reorganization effect were found and analyzed. The complexity of this phase separation phenomenon in the T junction has been further revealed via the on-line graph processing technology. Meanwhile the influences of the inlet mass flow rate W1, the inlet mass quality X1, and the mass extraction rate G3/G1 on phase separation were analyzed

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.

Preconcentration of trace elements

International Nuclear Information System (INIS)

Zolotov, Yu. A.; Kuz'min, N.M.

1990-01-01

This monograph deals with the theory and practical applications of trace metals preconcentration. It gives general characteristics of the process and describes in detail the methods of preconcentration: solvent extraction, sorption, co-precipitation, volatilization, and others. Special attention is given to preconcentration in combination with subsequent determination methods. The use of preconcentration in analysis of environmental and biological samples, mineral raw materials, high purity substances, and various industrial materials is also considered

Determination of trace lithium in uranium compounds by adsorption on activated alumina using a micro-column method.

Science.gov (United States)

Luo, Ming-Biao; Li, Bo-Ping; Yang, Zhi; Liu, Wei; Sun, Yu-Zhen

2008-08-01

A novel method using a micro-column packed with active alumina as solid phase was proposed for separation of trace lithium from uranium compounds prior to determination. The method is based on a preliminary chromatographic separation of the total amount of uranium. This separation involves passing the solution containing sodium carbonate through active alumina and then eluting the trace lithium retained by the solid phase with a solution of sulfuric acid. Two modes, off-line and on-line micro-column preconcentration, were performed. In conjunction with atomic absorption spectrometry, this on-line preconcentration technique allows a determination of lithium at 10(-9) level. Both off-line and on-line mode operation conditions were investigated in separation and determination of trace lithium by micro-column method (length of column bed, flow rate, etc.). The adsorption capacity of activated alumina was found to be 343 microg g(-1) for lithium. Under the optimal operation condition, the detection limit (DL) of on-line preconcentration corresponding to three times the standard deviation of the blank (S/N = 3) was found to be 1.3 ng mL(-1) and the RSD of this method is 3.32% (n = 5). The on-line calibration graph was linear over the range 20 - 200 ng mL(-1). A good preconcentration factor 820 was achieved by experiment under the on-line mode. The developed method was applied to the analysis of trace lithium in nuclear grade uranium compounds.

Grafting 3-mercaptopropyl trimethoxysilane on multi-walled carbon nanotubes surface for improving on-line cadmium(II) preconcentration from water samples

Energy Technology Data Exchange (ETDEWEB)

Corazza, Marcela Zanetti; Somera, Bruna Fabrin; Segatelli, Mariana Gava [Departamento de Quimica, Universidade Estadual de Londrina, Rodovia Celso Garcia Cid, PR 445, Km 380, Campus Universitario, Londrina-PR, CEP 86051-990 (Brazil); Tarley, Cesar Ricardo Teixeira, E-mail: tarley@uel.br [Departamento de Quimica, Universidade Estadual de Londrina, Rodovia Celso Garcia Cid, PR 445, Km 380, Campus Universitario, Londrina-PR, CEP 86051-990 (Brazil); Instituto Nacional de Ciencia e Tecnologia (INCT) de Bioanalitica, Universidade Estadual de Campinas (UNICAMP), Instituto de Quimica, Departamento de Quimica Analitica, Cidade Universitaria Zeferino, Vaz, s/n, CEP 13083-970, Campinas-SP (Brazil)

2012-12-15

Highlights: Black-Right-Pointing-Pointer 3-Mercaptopropyl trimethoxysilane grafted on MWCNT surface was prepared. Black-Right-Pointing-Pointer The material promoted an increase on performance of MWCNT for Cd{sup 2+} adsorption. Black-Right-Pointing-Pointer The life time of adsorbent was very high. Black-Right-Pointing-Pointer An improvement of 84% on the sensitivity was achieved. - Abstract: In the present study, the performance of multi-walled carbon nanotubes (MWCNTs) grafted with 3-mercaptopropyltrimethoxysilane (3-MPTMS), used as a solid phase extractor for Cd{sup 2+} preconcentration in a flow injection system coupled to flame atomic absorption spectrometry (FAAS), was evaluated. The procedure involved the preconcentration of 20.0 mL of Cd{sup 2+} solution at pH 7.5 (0.1 mol L{sup -1} buffer phosphate) through 70 mg of 3-MPTMS-grafted MWCNTs packed into a minicolumn at 6.0 mL min{sup -1}. The elution step was carried out with 1.0 mol L{sup -1} HCl. Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were used to estimate the extent of the MWCNT chemical modification. The 3-MPTMS-grafted MWCNTs provided a 1.68 times improvement in the sensitivity of the Cd{sup 2+} FAAS determination compared to the unsilanized oxidized MWCNTs. The following parameters were obtained: preconcentration factor of 31.5, consumptive index of 0.635 mL, sample throughput of 14 h{sup -1}, and concentration efficiency of 9.46 min{sup -1}. The analytical curve was constructed in the range of 1.0-60.0 {mu}g L{sup -1} (r = 0.9988), and the detection and quantification limits were found to be 0.15 {mu}g L{sup -1} and 0.62 {mu}g L{sup -1}, respectively. Different types of water samples and cigarette sample were successfully analyzed, and the results were compared using electrothermal atomic absorption spectrometry (ETAAS) as reference technique. In addition, the accuracy of proposed method was also checked by analysis of

Implementation of suitable flow injection/sequential-sample separation/preconcentration schemes for determination of trace metal concentrations using detection by electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry

DEFF Research Database (Denmark)

Hansen, Elo Harald; Wang, Jianhua

2002-01-01

Various preconditioning procedures encomprising appropriate separation/preconcentration schemes in order to obtain optimal sensitivity and selectivity characteristics when using electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICPMS...

Selective ionic liquid ferrofluid based dispersive-solid phase extraction for simultaneous preconcentration/separation of lead and cadmium in milk and biological samples.

Science.gov (United States)

Fasih Ramandi, Negin; Shemirani, Farzaneh

2015-01-01

For the first time, a selective ionic liquid ferrofluid has been used in dispersive solid phase extraction (IL-FF-D-SPE) for simultaneous preconcentration and separation of lead and cadmium in milk and biological samples combined with flame atomic absorption spectrometry. To improve the selectivity of the ionic liquid ferrofluid, the surface of TiO2 nanoparticles with a magnetic core as sorbent was modified by loading 1-(2-pyridylazo)-2-naphtol. Due to the rapid injection of an appropriate amount of ionic liquid ferrofluid into the aqueous sample by a syringe, extraction can be achieved within a few seconds. In addition, based on the attraction of the ionic liquid ferrofluid to a magnet, no centrifugation step is needed for phase separation. The experimental parameters of IL-FF-D-SPE were optimized using a Box-Behnken design (BBD) after a Plackett-Burman screening design. Under the optimum conditions, the relative standard deviations of 2.2% and 2.4% were obtained for lead and cadmium, respectively (n=7). The limit of detections were 1.21 µg L(-1) for Pb(II) and 0.21 µg L(-1) for Cd(II). The preconcentration factors were 250 for lead and 200 for cadmium and the maximum adsorption capacities of the sorbent were 11.18 and 9.34 mg g(-1) for lead and cadmium, respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

Operation manual for the INEL on-line mass-separator facility

International Nuclear Information System (INIS)

Anderl, R.A.

1984-06-01

This report is an operation manual for an on-line mass-separator facility which is located in Building 661 at the Test Reactor Area of the Idaho National Engineering Laboratory. The facility provides mass-separated sources of short-lived fission-product radionuclides whose decay properties can be studied using a variety of nuclear spectroscopic techniques. This facility is unique in that it utilizes the gas-jet technique to transport fission products from a 252 Cf source located in a hot cell to the ion source of the mass separator. This document includes the following: (a) a detailed description of the facility, (b) identification of equipment hazards and safety controls, (c) detailed operating procedures for startup, continuous operation and shutdown, (d) operating procedures for the californium hot cell, and (e) an operator's manual for the automated moving tape collector/data acquisition system. 7 references, 16 figures, 8 tables

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...

Biological preconcentrator

Science.gov (United States)

Manginell, Ronald P [Albuquerque, NM; Bunker, Bruce C [Albuquerque, NM; Huber, Dale L [Albuquerque, NM

2008-09-09

A biological preconcentrator comprises a stimulus-responsive active film on a stimulus-producing microfabricated platform. The active film can comprise a thermally switchable polymer film that can be used to selectively absorb and desorb proteins from a protein mixture. The biological microfabricated platform can comprise a thin membrane suspended on a substrate with an integral resistive heater and/or thermoelectric cooler for thermal switching of the active polymer film disposed on the membrane. The active polymer film can comprise hydrogel-like polymers, such as poly(ethylene oxide) or poly(n-isopropylacrylamide), that are tethered to the membrane. The biological preconcentrator can be fabricated with semiconductor materials and technologies.

Determination of trace heavy metals in soil and sediments by atomic spectrometry following preconcentration with Schiff bases on Amberlite XAD-4

Energy Technology Data Exchange (ETDEWEB)

Kara, Derya, E-mail: dkara@balikesir.edu.tr [Department of Chemistry, Art and Science Faculty, Balikesir University, 10100 Balikesir (Turkey); Fisher, Andrew; Hill, Steve J. [School of Earth, Ocean and Environmental Sciences, University of Plymouth, Drake Circus, Plymouth, Devon PL4 8AA (United Kingdom)

2009-06-15

A matrix separation and analyte preconcentration system using Amberlite XAD copolymer resins functionalized by Schiff base reactions coupled with atomic spectrometry has been developed. Three different functionalized Amberlite XAD resins were synthesized using 4-phenylthiosemicarbazide, 2,3-dihydroxybenzaldehyde and 2-thiophenecarboxaldehyde as reagents. These resins could be used to preconcentrate transition and other trace heavy metal analytes from nitric acid digests of soil and sediment samples. Analyte retention was shown to work well at pH 6.0. After treatment of the digests with sodium fluoride and buffering to pH 6, samples that contain extremely large concentrations of iron were analysed for trace analytes without the excess iron overloading the capacity of the resin. The analytes Cd, Co, Cu, Ni and Pb were preconcentrated from acid extracts of certified soil/sediment samples and then eluted with 0.1 M HNO{sub 3} directly to the detection system. Flame atomic absorption spectrometry was used as a means of detection during the studies. The efficiency of the chelating resin and the accuracy of the proposed method were evaluated by the analysis of soil (SO-2) and sediment (LGC 6157 and MESS-3) certified reference materials.

Vapor generation – atomic spectrometric techniques. Expanding frontiers through specific-species preconcentration. A review

International Nuclear Information System (INIS)

Gil, Raúl A.; Pacheco, Pablo H.; Cerutti, Soledad; Martinez, Luis D.

2015-01-01

This article reviews 120 articles found in SCOPUS and specific Journal cites corresponding to the terms ‘preconcentration’; ‘speciation’; ‘vapor generation techniques’ and ‘atomic spectrometry techniques’ in the last 5 years. - Highlights: • Recent advances in vapor generation and atomic spectrometry were reviewed. • Species-specific preconcentration strategies after and before VG were discussed. • New preconcentration and speciation analysis were evaluated within this framework. - Abstract: We review recent progress in preconcentration strategies associated to vapor generation techniques coupled to atomic spectrometric (VGT-AS) for specific chemical species detection. This discussion focuses on the central role of different preconcentration approaches, both before and after VG process. The former was based on the classical solid phase and liquid–liquid extraction procedures which, aided by automation and miniaturization strategies, have strengthened the role of VGT-AS in several research fields including environmental, clinical, and others. We then examine some of the new vapor trapping strategies (atom-trapping, hydride trapping, cryotrapping) that entail improvements in selectivity through interference elimination, but also they allow reaching ultra-low detection limits for a large number of chemical species generated in conventional VG systems, including complete separation of several species of the same element. This review covers more than 100 bibliographic references from 2009 up to date, found in SCOPUS database and in individual searches in specific journals. We finally conclude by giving some outlook on future directions of this field

Vapor generation – atomic spectrometric techniques. Expanding frontiers through specific-species preconcentration. A review

Energy Technology Data Exchange (ETDEWEB)

Gil, Raúl A.; Pacheco, Pablo H.; Cerutti, Soledad [Área de Química Analítica, Facultad de Química Bioquímica y Farmacia, Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Instituto de Química de San Luis, INQUISAL, Centro Científico-Tecnológico de San Luis (CCT-San Luis), Consejo Nacional de Investigaciones Científicas y Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Martinez, Luis D., E-mail: ldm@unsl.edu.ar [Área de Química Analítica, Facultad de Química Bioquímica y Farmacia, Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Instituto de Química de San Luis, INQUISAL, Centro Científico-Tecnológico de San Luis (CCT-San Luis), Consejo Nacional de Investigaciones Científicas y Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina)

2015-05-22

This article reviews 120 articles found in SCOPUS and specific Journal cites corresponding to the terms ‘preconcentration’; ‘speciation’; ‘vapor generation techniques’ and ‘atomic spectrometry techniques’ in the last 5 years. - Highlights: • Recent advances in vapor generation and atomic spectrometry were reviewed. • Species-specific preconcentration strategies after and before VG were discussed. • New preconcentration and speciation analysis were evaluated within this framework. - Abstract: We review recent progress in preconcentration strategies associated to vapor generation techniques coupled to atomic spectrometric (VGT-AS) for specific chemical species detection. This discussion focuses on the central role of different preconcentration approaches, both before and after VG process. The former was based on the classical solid phase and liquid–liquid extraction procedures which, aided by automation and miniaturization strategies, have strengthened the role of VGT-AS in several research fields including environmental, clinical, and others. We then examine some of the new vapor trapping strategies (atom-trapping, hydride trapping, cryotrapping) that entail improvements in selectivity through interference elimination, but also they allow reaching ultra-low detection limits for a large number of chemical species generated in conventional VG systems, including complete separation of several species of the same element. This review covers more than 100 bibliographic references from 2009 up to date, found in SCOPUS database and in individual searches in specific journals. We finally conclude by giving some outlook on future directions of this field.

Liquid electrode plasma-optical emission spectrometry combined with solid-phase preconcentration for on-site analysis of lead.

Science.gov (United States)

Barua, Suman; Rahman, Ismail M M; Alam, Iftakharul; Miyaguchi, Maho; Sawai, Hikaru; Maki, Teruya; Hasegawa, Hiroshi

2017-08-15

A relatively rapid and precise method is presented for the determination of lead in aqueous matrix. The method consists of analyte quantitation using the liquid electrode plasma-optical emission spectrometry (LEP-OES) coupled with selective separation/preconcentration by solid-phase extraction (SPE). The impact of operating variables on the retention of lead in SPEs such as pH, flow rate of the sample solution; type, volume, flow rate of the eluent; and matrix effects were investigated. Selective SPE-separation/preconcentration minimized the interfering effect due to manganese in solution and limitations in lead-detection in low-concentration samples by LEP-OES. The LEP-OES operating parameters such as the electrical conductivity of sample solution; applied voltage; on-time, off-time, pulse count for applied voltage; number of measurements; and matrix effects have also been optimized to obtain a distinct peak for the lead at λ max =405.8nm. The limit of detection (3σ) and the limit of quantification (10σ) for lead determination using the technique were found as 1.9 and 6.5ng mL -1 , respectively. The precision, as relative standard deviation, was lower than 5% at 0.1μg mL -1 Pb, and the preconcentration factor was found to be 187. The proposed method was applied to the analysis of lead contents in the natural aqueous matrix (recovery rate:>95%). The method accuracy was verified using certified reference material of wastewaters: SPS-WW1 and ERM-CA713. The results from LEP-OES were in good agreement with inductively coupled plasma optical emission spectrometry measurements of the same samples. The application of the method is rapid (≤5min, without preconcentration) with a reliable detection limit at trace levels. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of rare earth elements in natural water samples – A review of sample separation, preconcentration and direct methodologies

Energy Technology Data Exchange (ETDEWEB)

Fisher, Andrew, E-mail: afisher@plymouth.ac.uk [School of Geography, Earth and Environmental Sciences, Plymouth University, Drake Circus, Plymouth, Devon, PL4 8AA (United Kingdom); Kara, Derya [Department of Chemistry, Art and Science Faculty, Balikesir University, 10100, Balikesir (Turkey)

2016-09-07

This review discusses and compares the methods given for the determination of rare earth elements (REE) in natural water samples, including sea, river, lake, tap, ground and waste waters as well as Antarctic ice. Since REE are at very low concentrations in natural waters, numerous different preconcentration methods have been proposed to enable their measurement. These include liquid liquid extraction, dispersive liquid-liquid micro-extraction and solidified floating drop micro-extraction. In addition to liquid-liquid extraction methods, solid phase extraction using commercial resins, resins made in-house, silica-based exchange materials and other solid media is also discussed. These and other techniques such as precipitation/co-precipitation and flotation are compared in terms of speed, preconcentration factors achieved, precision, accuracy and limits of detection (LOD). Some papers have discussed the direct determination of REE in these sample types. Some have used specialised sample introduction systems such as ultrasonic nebulization whereas others have used a standard sample introduction system coupled with inductively coupled plasma mass spectrometry (ICP-MS) detection. These direct methods have also been discussed and compared. - Highlights: • The determination of rare earth elements in waters is reviewed. • Assorted preconcentration techniques are discussed and evaluated. • Detection techniques include atomic spectrometry, potentiometry and spectrophotometry. • Special nebulisers and electrothermal vaporization approaches are reviewed.

Dispersive solid phase microextraction with magnetic graphene oxide as the sorbent for separation and preconcentration of ultra-trace amounts of gold ions.

Science.gov (United States)

Kazemi, Elahe; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad

2015-08-15

A selective, simple and rapid dispersive solid phase microextraction was developed using magnetic graphene oxide (MGO) as an efficient sorbent for the separation and preconcentration of gold ions. The MGO was synthesized by means of the simple one step chemical coprecipitation method, characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). Gold ions retained by the sorbent were eluted using 0.5mol L(-)(1) thiourea in 0.1mol L(-1) HCl solution and determined by the flow injection flame atomic absorption spectrometry (FI-FAAS). The factors affecting the separation and preconcentration of gold were investigated and optimized. Under the optimized conditions, the method exhibited a linear dynamic range of 0.02-100.0µg L(-)(1) with a detection limit of 4ng L(-1) and an enrichment factor of 500. The relative standard deviations of 3.2% and 4.7% (n=6) were obtained at 20µg L(-1) level of gold ions for the intra and the inter day analysis, respectively. The method was successfully applied to the determination of gold ions in water and waste water samples as well as a certified reference material (CCU-1b, copper flotation concentrate). Copyright © 2015 Elsevier B.V. All rights reserved.

Development of clinical dosage forms for a poorly water-soluble drug II: formulation and characterization of a novel solid microemulsion preconcentrate system for oral delivery of a poorly water-soluble drug.

Science.gov (United States)

Li, Ping; Hynes, Sara R; Haefele, Thomas F; Pudipeddi, Madhu; Royce, Alan E; Serajuddin, Abu T M

2009-05-01

The solution of a poorly water-soluble drug in a liquid lipid-surfactant mixture, which served as a microemulsion preconcentrate, was converted into a solid form by incorporating it in a solid polyethylene glycol (PEG) matrix. The solid microemulsion preconcentrates thus formed consisted of Capmul PG8 (propylene glycol monocaprylate) as oil, Cremophor EL (polyoxyl 35 castor oil) as surfactant, and hydrophilic polymer PEG 3350 as solid matrix. The drug (aqueous solubility: 0.17 microg/mL at pH 1-8 and 25 degrees C) was dissolved in a melt of the mixture at 65-70 degrees C and then the hot solution was filled into hard gelatin capsules; the liquid gradually solidified upon cooling below 55 degrees C. The solid system was characterized by differential scanning calorimetry (DSC), scanning electron microscopy (SEM), confocal Raman microscopy (CRM), and the dispersion testing in water. It was confirmed that a solid microemulsion preconcentrate is a two-phase system, where clusters of crystalline PEG 3350 formed the solid structure (m.p. 55-60 degrees C) and the liquid microemulsion preconcentrate dispersed in between PEG 3350 crystals as a separate phase. The drug remained dissolved in the liquid phase. In vitro release testing showed that the preconcentrate dispersed readily in water forming a microemulsion with the drug dissolved in the oil particles (PEG 3350 did not interfere with the process of self-microemulsification.

Coupling sequential injection on-line preconcentration by means of a renewable microcolumn with ion-exchange beads with detection by electrothermal atomic absorption spectrometry. Comparing the performance of eluting the loaded beads with transporting them directly into the graphite tube

DEFF Research Database (Denmark)

Wang, Jianhua; Hansen, Elo Harald

2001-01-01

The design of a flow injection/sequential injection (FIA/SIA) on-line preconcentration system incorporating a renewable microcolumn with ion-exchange beads and interfaced with an electrothermal atomic absorption spectrometry (ETAAS) detector is described, and its practical applicability.......4% for the procedure in which the loaded beads are transported directly to the graphite furnace for pyrolysis and atomization, and even improved in comparison to the traditional unidirectional and bidirectional repetitive elution procedures which under comparable conditions yield R.S.D.-values of 5.8 and 4...

31 CFR 50.14 - Separate line item.

Science.gov (United States)

2010-07-01

....14 Money and Finance: Treasury Office of the Secretary of the Treasury TERRORISM RISK INSURANCE PROGRAM Disclosures as Conditions for Federal Payment § 50.14 Separate line item. An insurer is deemed to be in compliance with the requirement of providing disclosure on a “separate line item in the policy...

Adsorption studies of Cd(II) onto Al{sub 2}O{sub 3}/Nb{sub 2}O{sub 5} mixed oxide dispersed on silica matrix and its on-line preconcentration and determination by flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Mendonca Costa, Lucimara [Programa de Pos-Graduacao em Quimica da Universidade Federal de Alfenas, Rua Gabriel Monteiro da Silva, 700, Alfenas-MG, CEP 37130-000 (Brazil); Ribeiro, Emerson Schwingel [Instituto de Quimica, Universidade Federal do Rio de Janeiro, Rio de Janeiro-RJ, CEP 21941-909 (Brazil); Segatelli, Mariana Gava [Departamento de Quimica, Universidade Estadual de Londrina, Rod. Celso Garcia Cid, PR 445 Km 380, Campus Universitario, Londrina-PR, CEP 86051-990 (Brazil); Nascimento, Danielle Raphael do [Instituto de Quimica, Universidade Federal do Rio de Janeiro, Rio de Janeiro-RJ, CEP 21941-909 (Brazil); Midori de Oliveira, Fernanda [Departamento de Quimica, Universidade Estadual de Londrina, Rod. Celso Garcia Cid, PR 445 Km 380, Campus Universitario, Londrina-PR, CEP 86051-990 (Brazil); Tarley, Cesar Ricardo Teixeira, E-mail: tarley@uel.br [Programa de Pos-Graduacao em Quimica da Universidade Federal de Alfenas, Rua Gabriel Monteiro da Silva, 700, Alfenas-MG, CEP 37130-000 (Brazil); Departamento de Quimica, Universidade Estadual de Londrina, Rod. Celso Garcia Cid, PR 445 Km 380, Campus Universitario, Londrina-PR, CEP 86051-990 (Brazil)

2011-05-15

The present study describes the adsorption characteristic of Cd(II) onto Nb{sub 2}O{sub 5}/Al{sub 2}O{sub 3} mixed oxide dispersed on silica matrix. The characterization of the adsorbent has been carried out by infrared spectroscopy (IR), scanning electronic microscopy (SEM), energy dispersive spectroscopy (EDS), energy dispersive X-ray fluorescence analysis (EDXRF) and specific surface area (S{sub BET}). From batch experiments, adsorption kinetic of Cd(II) was described by a pseudo-second-order kinetic model. The Langmuir linear isotherm fitted to the experimental adsorption isotherm very well, and the maximum adsorption capacity was found to be 17.88 mg g{sup -1}. Using the effective material, a method for Cd(II) preconcentration at trace level was developed. The method was based on on-line adsorption of Cd(II) onto SiO{sub 2}/Al{sub 2}O{sub 3}/Nb{sub 2}O{sub 5} at pH 8.64, in which the quantitative desorption occurs with 1.0 mol L{sup -1} hydrochloric acid towards FAAS detector. The experimental parameters related to the system were studied by means of multivariate analysis, using 2{sup 4} full factorial design and Doehlert matrix. The effect of SO{sub 4}{sup 2-}, Cu{sup 2+}, Zn{sup 2+} and Ni{sup 2+} foreign ions showed no interference at 1:100 analyte:interferent proportion. Under the most favorable experimental conditions, the preconcentration system provided a preconcentration factor of 18.4 times, consumption index of 1.08 mL, sample throughput of 14 h{sup -1}, concentration efficiency of 4.35 min{sup -1}, linear range from 5.0 up to 35.0 {mu}g L{sup -1} and limits of detection and quantification of 0.19 and 0.65 {mu}g L{sup -1} respectively. The feasibility of the proposed method for Cd(II) determination was assessed by analysis of water samples, cigarette sample and certified reference materials TORT-2 (Lobster hepatopancreas) and DOLT-4 (Dogfish liver).

On-line mass separator of superheavy atoms

International Nuclear Information System (INIS)

Oganesyan, Yu.Ts.

2002-01-01

The concept is presented of an on-line Mass Analyzer of SuperHeavy Atoms (MASHA) dedicated to the separation and determination of the mass and decay properties of new elements and isotopes produced in heavy-ion induced reactions. The new nuclides with half-lives T 1/2 ≥ 1 s are transported to an ECR-source working at a frequency of 2.45 GHz and are separated by mass with a mass resolution of M/ΔM ∼ 1500. In the focal plane of the magnetic analyzer a front strip detector surrounded by side detectors will be placed to determine the mass according to the signals from the detected α-particles or fission fragments with efficiency of about 90 %. In comparison to other existing in-flight recoil separators, the present setup will be characterized by higher efficiency and high selectivity relative to background reaction products. The setup MASHA may be used also in the investigation of nuclear reactions of different type induced by stable and radioactive beams

On-Line Mass Separator of Superheavy Atoms

CERN Document Server

Oganessian, Yu T

2002-01-01

The concept is presented of an on-line Mass Analyzer of SuperHeavy Atoms (MASHA) dedicated to the separation and determination of the mass and decay properties of new elements and isotopes produced in heavy-ion induced reactions. The new nuclides with half-lives T_{1/2}\\ge 1 s are transported to an ECR-source working at a frequency of 2.45 GHz and are separated by mass with a mass resolution of M/\\Delta M\\sim 1500. In the focal plane of the magnetic analyzer a front strip detector surrounded by side detectors will be placed to determine the mass according to the signals from the detected alpha-particles or fission fragments with efficiency of about 90 %. In comparison to other existing in-flight recoil separators, the present setup will be characterized by higher efficiency and high selectivity relative to background reaction products. The setup MASHA may be used also in the investigation of nuclear reactions of different type induced by stable and radioactive beams.

Optimization and application of homogeneous liquid-liquid extraction in preconcentration of copper (II) in a ternary solvent system

Energy Technology Data Exchange (ETDEWEB)

Farajzadeh, Mir Ali [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)], E-mail: farajzade@yahoo.com; Bahram, Morteza [Department of Chemistry, Faculty of Science, Urmia University, Urmia (Iran, Islamic Republic of); Zorita, Saioa [Department of Analytical Chemistry, University of Lund, P.O. Box 124, 221 00 Lund (Sweden); Mehr, Behzad Ghorbani [Department of Chemistry, Faculty of Science, Urmia University, Urmia (Iran, Islamic Republic of)

2009-01-30

In this study a homogeneous liquid-liquid extraction based on the Ph-dependent phase-separation process was investigated using a ternary solvent system (water-acetic acid-chloroform) for the preconcentration of Cu{sup 2+} ions. 8-Hydroxy quinoline was used as the chelating agent prior to its extraction. Flame atomic absorption spectrophotometry using acetylene-air flame was used for the quantitation of analyte after preconcentration. The effect of various experimental parameters in extraction step was investigated using two optimization methods, one variable at a time and central composite design. The experimental design was done at five levels of operating parameters. Nearly the same optimized results were obtained using both methods: sample size, 5 mL; volume of NaOH 10 M, 2 mL; chloroform volume, 300 {mu}L; 8-hydroxy quinoline concentration more than 0.01 M and salt amount did not affect the extraction significantly. Under the optimum conditions the calibration graph was linear over the range 10-2000 {mu}g L{sup -1}. The relative standard deviation was 7.6% for six repeated determinations (C = 500 {mu}g L{sup -1}). Furthermore, the limit of detection (S/N = 3) and limit of quantification (S/N = 10) of the method were obtained as 1.74 and 6 {mu}g L{sup -1}, respectively.

Automation and integration of multiplexed on-line sample preparation with capillary electrophoresis for DNA sequencing

Energy Technology Data Exchange (ETDEWEB)

Tan, H.

1999-03-31

The purpose of this research is to develop a multiplexed sample processing system in conjunction with multiplexed capillary electrophoresis for high-throughput DNA sequencing. The concept from DNA template to called bases was first demonstrated with a manually operated single capillary system. Later, an automated microfluidic system with 8 channels based on the same principle was successfully constructed. The instrument automatically processes 8 templates through reaction, purification, denaturation, pre-concentration, injection, separation and detection in a parallel fashion. A multiplexed freeze/thaw switching principle and a distribution network were implemented to manage flow direction and sample transportation. Dye-labeled terminator cycle-sequencing reactions are performed in an 8-capillary array in a hot air thermal cycler. Subsequently, the sequencing ladders are directly loaded into a corresponding size-exclusion chromatographic column operated at {approximately} 60 C for purification. On-line denaturation and stacking injection for capillary electrophoresis is simultaneously accomplished at a cross assembly set at {approximately} 70 C. Not only the separation capillary array but also the reaction capillary array and purification columns can be regenerated after every run. DNA sequencing data from this system allow base calling up to 460 bases with accuracy of 98%.

Separation/preconcentration of silver(I) and lead(II) in environmental samples on cellulose nitrate membrane filter prior to their flame atomic absorption spectrometric determinations

International Nuclear Information System (INIS)

Soylak, Mustafa; Cay, Rukiye Sungur

2007-01-01

An enrichment method for trace amounts of Ag(I) and Pb(II) has been established prior to their flame atomic absorption spectrometric determinations. The preconcentration/separation procedure is based on chelate formation of Ag(I) and Pb(II) with ammonium pyrrolidine dithiocarbamate (APDC) and on retention of the chelates on cellulose nitrate membrane filter. The influences of some analytical parameters including pH and amounts of reagent, etc. on the recoveries of analytes were investigated. The effects of interferic ions on the quantitative recoveries of analytes were also examined. The detection limits (k = 3, N = 11) were 4.6 μg L -1 for silver(I) and 15.3 μg L -1 for lead(II). The relative standard deviations (R.S.D.) of the determinations for analyte ions were below 3%. The method was applied to environmental samples for the determination of analyte ions with satisfactory results (recoveries >95%)

A Novel Method for the Filterless Preconcentration of Iron

DEFF Research Database (Denmark)

Andersen, Jens Enevold Thaulov

2005-01-01

A novel method of analysis of iron by filterless preconcentration is presented. This is the first example of efficient preconcentration of a refractory transition metal where coprecipitation and columns were omitted. The method applies a manifold of flow injection analysis (FIA) to iron species...... that are preconcentrated on the inner walls of a tubular reactor. It was found that the adsorption of iron species to the walls was particularly pronounced in reactors of nylon material and enrichment factors of 30-35 could be attained, as dependent on the length of the reactor and on the time of preconcentration....... In the preconcentration step of the FIA accessory, the optimum efficacy was obtained when the acidity of the samples were adjusted by HCl to pH = 2.5 whereas the ammonia preconcentration buffer should be kept alkaline at pH = 9.8. After being preconcentrated on the tubular reactor, the iron species were eluted...

Synthesis of xanthate functionalized silica gel and its application for the preconcentration and separation of uranium(VI) from inorganic components

International Nuclear Information System (INIS)

Gopi Krishna, P.; Naidu, G.R.K.; Rao, K.S.

2005-01-01

A new chelating solid extractant prepared by the chemical immobilization of xanthate on silica gel was characterized by Fourier transform infra red spectrometry (FTIR), thermogravimetric analysis (TGA) and microanalysis and used for the preconcentration and separation of uranyl ion prior to its determination by Arsenazo-III. The effect of pH, weight of the solid extractant, volume of the aqueous phase and the interference of neutral electrolytes, cations and anions on the determination of uranium, have been studied in detail to optimize the conditions for trace determination of uranium(VI). The accuracy of the developed procedure was tested by analyzing marine sediment (MESS-3) and soil (IAEA-SOIL-7) reference materials. The results obtained on analysis of soil and sediment samples are comparable to standard ICP-MS values. (author)

A Micro-Preconcentrator Combined Olfactory Sensing System with a Micromechanical Cantilever Sensor for Detecting 2,4-Dinitrotoluene Gas Vapor

Directory of Open Access Journals (Sweden)

Myung-Sic Chae

2015-07-01

Full Text Available Preventing unexpected explosive attacks and tracing explosion-related molecules require the development of highly sensitive gas-vapor detection systems. For that purpose, a micromechanical cantilever-based olfactory sensing system including a sample preconcentrator was developed to detect 2,4-dinitrotoluene (2,4-DNT, which is a well-known by-product of the explosive molecule trinitrotoluene (TNT and exists in concentrations on the order of parts per billion in the atmosphere at room temperature. A peptide receptor (His-Pro-Asn-Phe-Ser-Lys-Tyr-Ile-Leu-His-Gln-Arg that has high binding affinity for 2,4-DNT was immobilized on the surface of the cantilever sensors to detect 2,4-DNT vapor for highly selective detection. A micro-preconcentrator (µPC was developed using Tenax-TA adsorbent to produce higher concentrations of 2,4-DNT molecules. The preconcentration was achieved via adsorption and thermal desorption phenomena occurring between target molecules and the adsorbent. The µPC directly integrated with a cantilever sensor and enhanced the sensitivity of the cantilever sensor as a pretreatment tool for the target vapor. The response was rapidly saturated within 5 min and sustained for more than 10 min when the concentrated vapor was introduced. By calculating preconcentration factor values, we verified that the cantilever sensor provides up to an eightfold improvement in sensing performance.

Carrier element-free coprecipitation (CEFC) method for the separation, preconcentration and speciation of chromium using an isatin derivative

Energy Technology Data Exchange (ETDEWEB)

Bulut, Volkan Numan; Ozdes, Duygu; Bekircan, Olcay; Gundogdu, Ali; Duran, Celal [Department of Chemistry, Karadeniz Technical University, Faculty of Arts and Sciences, 61080 Trabzon (Turkey); Soylak, Mustafa [Department of Chemistry, Erciyes University, Faculty of Arts and Sciences, 38039 Kayseri (Turkey)], E-mail: soylak@erciyes.edu.tr

2009-01-19

A new, simple, rapid and sensitive separation, preconcentration and speciation procedure for chromium in environmental liquid and solid samples has been established. The present speciation procedure for Cr(III) and Cr(VI) is based on combination of carrier element-free coprecipitation (CEFC) and flame atomic absorption spectrometric (FAAS) determinations. In this method a newly synthesized organic coprecipitant, 5-chloro-3-[4-(trifluoromethoxy) phenylimino]indolin-2-one (CFMEPI), was used without adding any carrier element for coprecipitation of chromium(III). After reduction of chromium(VI) by concentrated H{sub 2}SO{sub 4} and ethanol, the procedure was applied for the determination of total chromium. Chromium(VI) was calculated as the difference between the amount of total chromium and chromium(III). The optimum conditions for coprecipitation and speciation processes were investigated on several commonly tested experimental parameters, such as pH of the solution, amount of coprecipitant, sample volume, etc. No considerable interference was observed from the other investigated anions and cations, which may be found in natural water samples. The preconcentration factor was found to be 40. The detection limit for chromium(III) corresponding to three times the standard deviation of the blank (N = 10) was found 0.7 {mu}g L{sup -1}. The present procedure was successfully applied for speciation of chromium in several liquid and solid environmental samples. In order to support the accuracy of the method, the certified reference materials (CRM-TMDW-500 Drinking Water and CRM-SA-C Sandy Soil C) were analyzed, and standard APDC-MIBK liquid-liquid extraction method was performed. The results obtained were in good agreement with the certified values.

Carrier element-free coprecipitation (CEFC) method for the separation, preconcentration and speciation of chromium using an isatin derivative

International Nuclear Information System (INIS)

Bulut, Volkan Numan; Ozdes, Duygu; Bekircan, Olcay; Gundogdu, Ali; Duran, Celal; Soylak, Mustafa

2009-01-01

A new, simple, rapid and sensitive separation, preconcentration and speciation procedure for chromium in environmental liquid and solid samples has been established. The present speciation procedure for Cr(III) and Cr(VI) is based on combination of carrier element-free coprecipitation (CEFC) and flame atomic absorption spectrometric (FAAS) determinations. In this method a newly synthesized organic coprecipitant, 5-chloro-3-[4-(trifluoromethoxy) phenylimino]indolin-2-one (CFMEPI), was used without adding any carrier element for coprecipitation of chromium(III). After reduction of chromium(VI) by concentrated H 2 SO 4 and ethanol, the procedure was applied for the determination of total chromium. Chromium(VI) was calculated as the difference between the amount of total chromium and chromium(III). The optimum conditions for coprecipitation and speciation processes were investigated on several commonly tested experimental parameters, such as pH of the solution, amount of coprecipitant, sample volume, etc. No considerable interference was observed from the other investigated anions and cations, which may be found in natural water samples. The preconcentration factor was found to be 40. The detection limit for chromium(III) corresponding to three times the standard deviation of the blank (N = 10) was found 0.7 μg L -1 . The present procedure was successfully applied for speciation of chromium in several liquid and solid environmental samples. In order to support the accuracy of the method, the certified reference materials (CRM-TMDW-500 Drinking Water and CRM-SA-C Sandy Soil C) were analyzed, and standard APDC-MIBK liquid-liquid extraction method was performed. The results obtained were in good agreement with the certified values

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

Science.gov (United States)

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

2013-12-15

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

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

International Nuclear Information System (INIS)

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

2008-01-01

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

On line isotopic separator test benches at GANIL

International Nuclear Information System (INIS)

Anne, R.; Bru, B.; Joubert, A.; Leroy, R.; Obert, J.; Putaux, J.C.; Liang, C.F.; Paris, P.; Orr, N.; Steckmeyer, J.C.

1993-01-01

A first version of isotopic separator on line test bench has been built in order to test the feasibility of the production of radioactive species from 96 MeV/u of 20 Ne impinging a thick target of MgO. This test bench was equipped with a very compact ECR ion source (Nanogan) entirely made from permanent magnets and operating at 10 Ghz. 18 Ne 2,4+ ; 19N e 1,2,3,4+ and 23,24 Ne 1+ has been produced and ionized. A new more performing separator (SIRa) allowing the use of different types of ion sources will be completed by the end of 1993. (author) 4 refs., 4 figs., 1 tab

Preconcentration of a low grade uranium ore in CPDU and laboratory investigation to optimize the dewatering conditions of the preconcentration products

International Nuclear Information System (INIS)

Cristovici, M.A.; Berry, T.F.; Raicevic, M.M.; Brady, E.L.; Bredin, E.L.; Leigh, G.W.; Rouleau, J.P.

1982-04-01

A process consisting of pyrite flotation and magnetic concentration of radionuclides was developed by CANMET over several years, to preconcentrate low grade uranium ores prior to leaching. When the economics of the preconcentration-leaching technology was compared with the leaching of the entire ore after pyrite flotation (Base Case variant), the preconcentration method appeared to be economically less advantageous than expected, due to the high cost of dewatering the preconcentration products. Further investigations examined in-depth the metallurgy and dewatering of the two variants: preconcentration and base case. A typical low grade uranium ore from Elliot Lake area was used. The metallurgy was compared based on data from continuous operation (CPDU). In the preconcentration variant the amount of ore directed to leaching was reduced to more than one third of that processed in the base case, while the radionuclide concentration became more than three times higher. However, by preconcentration 7% of the uranium was lost before leaching. Systematic laboratory-scale settling and filter tests optimized the dewatering conditions of the preconcentration technology to the extent that rates similar to those of the base case were obtained

Isotopic nuclear reactor with on-line separation

International Nuclear Information System (INIS)

Liviu, Popa-Simil

2007-01-01

In the new reactor-waste cycle design the nuclear reactor gets features of the living beings - resembling the plants/vegetation -. The separation of waste starts inside the fuel by using the fission reaction to separate the fission products from the fuel. The fuel, which is preferred to be highly isotopic enriched, is fabricated in beads smaller than the fission product range, immersed in a gentle flowing liquid drain. If this liquid is Lead Bismuth (LBE) the fission products will be lighter, while in Sodium-Potassium (NaK) will be heavier, except for gases. This drain liquid will collect both the fission products and the collision damage, drawing them slow to give time to short lives disintegration chains to take place inside the shielded nuclear reactor area outside the reactor core in a separation unit. While the drain liquid with the fission products is outside the reactor core few choices are available: - To solidify the drain liquid freezing all elements inside and transport the metal in cryogenic conditions to a remote separation unit, or to apply a separation partitioning process online stabilizing and packing the fission products only, or a combination of these two. The radioactivity of this drain liquid is smaller than that of the actual used fuel because it represents the accumulation of a very short period (about 1 month or less) and had enough time to cool down all the short lives. The separation unit on-line with the nuclear reactor is composed of a density separation unit, followed by a phase interface concentration unit which moves out of the LBE the fission products as lighter impurities, and an electrochemical separation unit for the fission products. Further, chemical separation, stabilization processes are applied and the fission products are delivered partitioned on groups of chemical compatible products. Finally the specific waste is about 1 Kg/Gw*day, to which the stabilization products have to be added which increases this mass by 10 times

Trace mercury determination in drinking and natural water after preconcentration and separation by DLLME-SFO method coupled with cold vapor atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Abdollahi Atousa

2014-07-01

Full Text Available A novel dispersive liquid–liquid microextraction based on solidification of floating organic drop (DLLME-SFO for simultaneous separation/preconcentration of ultra trace amounts of mercury was used. A method based on amalgamation was used for collection of gaseous mercury on gold coated sand (Gold trap. The concentration of mercury was determined by cold vapor atomic absorption spectrometry (CV-AAS. The DLLME-SFO behavior of mercury by using dithizone as complexing agent was systematically investigated. The factors influencing, the complex formation and extraction of DLLME-SFO method such as type and volume of extraction and disperser solvents, pH, concentration of salt, centrifuging time and concentration of the chelating agent were optimized. The method was successfully applied to the determination of mercury in drinking and natural water and satisfactory relative recoveries (95–105% were achieved. The proposed procedure was based on very low consumption of organic solvents. The other benefits of the system were sensitive, simple, friendly to the environment, rejection of matrix constituent, low cost, the time consuming and high enrichment factor.

Implementation of suitable FI/SI-sample separation/preconcentration schemes for determinations of trace-metal concentrations when using detection by ETAAS and ICPMS

DEFF Research Database (Denmark)

Hansen, Elo Harald; Wang, Jianhua

be effected under enclosed and strictly controlled conditions. Various separation/preconcentration procedures are feasible, such as liquid-liquid extraction, (co)precipitation with collection in knotted reactors, adsorption, hydride generation, or the use of ion-exchange columns. Apart from hydride generation......, where the analyte is converted into a gaseous species, the common denominator for these approaches is that the analyte material finally is contained within a well-defined small volume of eluate, which then is introduced into the analytical instruments. While the graphite tube of the ETAAS only can...

Determination of trace elements by neutron activation analysis using dinonylnaphtalene sulfonic acid as a preconcentrating agent

International Nuclear Information System (INIS)

Yang, M.H.; Chen, P.Y.; Tseng, C.L.; Yeh, S.J.; Weng, P.S.

1977-01-01

Dinonylnaphthalene sulfonic acid (HD) has been used as a preconcentrating agent to enrich trace metal ions and to separate the interfering elements such as Na, K, Cl and Br, which normally exist in the natural aqueous systems. Experiments were performed by extracting the ions in the aqueous medium with HD in n-hexane and subsequently backextracted into a minimal volume of acid solution. Factors influencing the extraction efficiency of the ions of interest were investigated. The preconcentration technique has been successfully applied to the determination by neutron activation analysis of trace elements in natural water and biological materials. Both short-lived nuclides (Mg, Al, Ca, Mn) and long-lived nuclides (Sm, Eu, Zn, La, Cr, Sc, Fe, Co) in the ppb-level concentrations were determined. (T.G.)

Ion source development for the on-line isotope separator at GSI

International Nuclear Information System (INIS)

Kirchner, R.; Burkard, K.; Hueller, W.; Klepper, O.

1991-08-01

The progress in the understanding of ion sources for isotope separation on-line and the feasibility of bunched beams of relatively refractory elements is reported. The ultra-high temperature FEBIAD-H ion source, facilitating the mounting of catchers and window compared to the earlier F-version, enables bunched beams of the elements with adsorption enthalpies up to almost 6 eV, e.g. of Be, Al, Ca, Cr, Fe, Co, Ni, Sr, Pd, Ba, Yb, and Au. This way also chemical selectivity for these elements may be achieved, at least to some extent, for isotopes with halflives > or approx.1 minute, including especially the difficult separation of alkaline-earth isotopes from isobaric alkalines. These studies reveal, however, also a principal difficulty in the on-line separation of refractory elements, namely their tendency, increasing with ΔH a , to re-diffuse after release from the catcher into the bulk of the hot source enclosure. (orig.)

Advances in the helium-jet coupled on-line mass separator RAMA

International Nuclear Information System (INIS)

Moltz, D.M.; Aysto, J.; Cable, M.D.; Parry, R.F.; Haustein, P.E.; Wouters, J.M.; Cerny, J.

1980-01-01

General improvements to the on-line mass separator RAMA (Recoil Atom Mass Analyzer) have yielded a greater reliability and efficiency for some elements. A new utilitarian helium-jet chamber has been installed to facilitate quick target and degrader foil changes in addition to a new ion source holder. A higher efficiency hollow-cathode, cathode-extraction ion source, for lower melting point elements ( 0 C) has also been designed. Tests with the beta-delayed proton emitter 37 Ca showed a factor of five increase in yield over the old hollow-cathode, anode-extraction source. A differentially-pumped-tape drive system compatible with both γ-γ and β-γ experiments has been incorporated into the general detection system. All major operating parameters will soon be monitored by a complete stand-alone microprocessor system which will eventually be upgraded to a closed-loop control system

A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry

OpenAIRE

Tuzen, Mustafa; Soylak, Mustafa; Citak, Demirhan; Ferreira, Hadla S.; Korn, Maria das Graças Andrade; Bezerra, Marcos de Almeida

2009-01-01

Texto completo: acesso restrito. p. 1041-1045 A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L−1 nitric acid solution, the analytes are determinate employing fla...

Separation of zirconium and hafnium from acompanying elements by paper chromatography in the systems of alcohol-acid

International Nuclear Information System (INIS)

Lebedeva, G.G.; Viktorova, M.E.

1980-01-01

Solvents have been chosen and investigated which provide expressed separation of zirconium and hafnium at the analysis of mineral raw materials by paper chromatography. The systems with HNO 3 and HCl containing methyl, ethyl, propyl and butyl alcohols have been studied as mobile phases for separation of zirconium and hafnium. It has been shown that alcohol contents and solvent acidity affect the Rsub(f) value of these elements. The C 2 H 5 OH-5MHCl and C 2 H 5 OH-5MHNO 3 systems are most optimal for pre-concentration of zirconium and hafnium

Neutron activation analysis of high pure uranium using preconcentration

International Nuclear Information System (INIS)

Sadikov, I.I.; Rakhimov, A.V.; Salimov, M.I.; Zinov'ev, V.G.

2006-01-01

Full text: Uranium and its compounds are used as nuclear fuel, and requirements for purity of initial uranium are very high. Therefore highly sensitive and multielemental analysis of uranium is required. One of such methods is neutron activation analysis (NAA). During irradiation of uranium by nuclear reactor neutrons the induced radioactivity of a sample is formed by uranium radionuclide 239 U (T 1/2 = 23,4 min.) and its daughter radionuclide 239 Np (T 1/2 = 2,39 d). Short-lived 239 U almost completely decays in 24 hours after irradiation and the radioactivity of the sample is mainly due to 239 Np and is more than 10 9 Bq for 0.1 g of uranium sample (F = 1*10 14 cm -2 s -1 , t irr . = 5 h). That is why nondestructive determination of the impurities is impossible and they should be separated from 239 Np. When irradiated uranium yields fission products - radionuclides of some elements with mass numbers 91-104 and 131-144. The main problem in NAA of uranium is to take into account correctly the influence of fission products on the analysis results. We have developed a radiochemical separation procedure for RNAA of uranium [1]. Comparing the results of analysis carried out by radiochemical NAA and instrumental NAA with preconcentration of trace elements can be used for evaluating the interference of fission products on uranium analysis results. Preconcentration of trace elements have been carried out by extraction chromatography in 'TBP - 6M HNO 3 ' system [1]. Experiments have shown that if 0.1 g uranium sample is taken for analysis (F = 1*10 14 cm -2 s -1 , t irr . =5 h) the apparent concentration of Y, Zr, Mo, Cs, La, Ce, Pr, Nd exceeds the true concentration by 2500-3000 times and so determination of these elements is not possible by radiochemical NAA. (author)

Minicolumn field preconcentration and flow-injection flame atomic absorption spectrometric determination of cadmium in seawater

International Nuclear Information System (INIS)

Yebra-Biurrun, M.C.; Moreno-Cid, A.; Puig, L.

2004-01-01

A simple method for the continuous field preconcentration of trace dissolved cadmium in seawater samples has been developed based on the minicolumn field sampling technique. For this purpose, minicolumns containing Chelite P (aminomethylphosphonic groups) were connected to a field flow preconcentration system (FFPS). Once in the laboratory, these minicolumns are sequentially inserted into a flow-injection system for on-line cadmium elution and detection by flame atomic absorption spectrometry. Factorial designs have been used to optimise the FFPS and the flow-injection elution process. Six experimental variables were optimised: sample pH, sample flow-rate, eluent concentration, eluent volume, eluent flow-rate and minicolumn diameter. The detection limit (3F) of the procedure was 2.7 ng l -1 for a sample volume of 300 ml. The precision (expressed as relative standard deviation) for 11 independent determinations was 0.5-9.4% for cadmium solutions of 10-300 ng l -1 . Analysis of certified reference materials (SLEW-3 and NASS-5) showed good agreement with the certified values. This procedure has been successfully applied to the determination of cadmium in seawater samples from Galicia (Spain)

Preconcentration of heavy metals on activated carbon and their determination in fruits by inductively coupled plasma optical emission spectrometry.

Science.gov (United States)

Feist, Barbara; Mikula, Barbara

2014-03-15

A method of separation and preconcentration of cadmium, cobalt, copper, nickel, lead, and zinc at trace level using activated carbon is proposed. Activated carbon with the adsorbed trace metals was mineralised using a high-pressure microwave mineraliser. The heavy metals were determined after preconcentration by inductively coupled plasma optical emission spectrometry (ICP-OES). The influence of several parameters, such as pH, sorbent mass, shaking time was examined. Moreover, effects of inorganic matrix on recovery of the determined elements were studied. The experiment shows that foreign ions did not influence recovery of the determined elements. The detection limits (DL) of Cd, Co, Cu, Ni, Pb, and Zn were 0.17, 0.19, 1.60, 2.60, 0.92 and 1.50 μg L(-)(1), respectively. The recovery of the method for the determined elements was better than 95% with relative standard deviation from 1.3% to 3.7%. The preconcentration factor was 80. The proposed method was applied for determination of Cd, Co, Cu, Ni, Pb, and Zn in fruits materials. Accuracy of the proposed method was verified using certified reference material (NCS ZC85006 Tomato). Copyright © 2013 Elsevier Ltd. All rights reserved.

Separation and preconcentration of Arsenic(III ions from aqueous media by adsorption on MWCNTs

Directory of Open Access Journals (Sweden)

Nahid Tavakkoli

2017-05-01

Full Text Available A simple and sensitive method using mini-column packed with multi-walled carbon nanotubes (MWCNTs combined with graphite furnace atomic absorption spectrometry (GFAAS for preconcentration and determination of ultra trace amounts of As(III in an aqueous medium is proposed. The procedure is based on the solid phase extraction of the As(III-sodium diethyldithiocarbamate (As-NaDDTC chelate on MWCNTs. Various parameters such as the effect of pH, eluent type and volume, amount of sorbent, and matrix effects on the quantitative recoveries of analyte ions were evaluated. It was found that sorption is quantitative and desorption occurs with 4.0 mL of 3.0 mol L−1 HNO3 in acetone. The limit of detection of the method was 0.008 ng mL−1 for GFAAS with enrichment factor of 125 and the relative standard deviation (RSD 0.97% (n = 8, C = 10 ng mL−1. This method has been applied to the determination of ultra trace As(III in water and rice plant and its ash successfully.

Electrokinetic sample preconcentration and hydrodynamic sample injection for microchip electrophoresis using a pneumatic microvalve.

Science.gov (United States)

Cong, Yongzheng; Katipamula, Shanta; Geng, Tao; Prost, Spencer A; Tang, Keqi; Kelly, Ryan T

2016-02-01

A microfluidic platform was developed to perform online electrokinetic sample preconcentration and rapid hydrodynamic sample injection for zone electrophoresis using a single microvalve. The polydimethylsiloxane microchip comprises a separation channel, a side channel for sample introduction, and a control channel which is used as a pneumatic microvalve aligned at the intersection of the two flow channels. The closed microvalve, created by multilayer soft lithography, serves as a nanochannel preconcentrator under an applied electric potential, enabling current to pass through while preventing bulk flow. Once analytes are concentrated, the valve is briefly opened and the stacked sample is pressure injected into the separation channel for electrophoretic separation. Fluorescently labeled peptides were enriched by a factor of ∼450 in 230 s. This method enables both rapid analyte concentration and controlled injection volume for high sensitivity, high-resolution CE. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Separation/Preconcentration and Speciation Analysis of Trace Amounts of Arsenate and Arsenite in Water Samples Using Modified Magnetite Nanoparticles and Molybdenum Blue Method

Directory of Open Access Journals (Sweden)

Mohammad Ali Karimi

2014-01-01

Full Text Available A new, simple, and fast method for the separation/preconcentration and speciation analysis of arsenate and arsenite ions using cetyltrimethyl ammonium bromide immobilized on alumina-coated magnetite nanoparticles (CTAB@ACMNPs followed by molybdenum blue method is proposed. The method is based on the adsorption of arsenate on CTAB@ACMNPs. Total arsenic in different samples was determined as As(V after oxidation of As(III to As(V using potassium permanganate. The arsenic concentration has been determined by UV-Visible spectrometric technique based on molybdenum blue method and amount of As(III was calculated by subtracting the concentration of As(V from total arsenic concentration. MNPs and ACMNPs were characterized by VSM, XRD, SEM, and FT-IR spectroscopy. Under the optimal experimental conditions, the preconcentration factor, detection limit, linear range, and relative standard deviation (RSD of arsenate were 175 (for 350 mL of sample solution, 0.028 μg mL−1, 0.090–4.0 μg mL−1, and 2.8% (for 2.0 μg mL−1, n=7, respectively. This method avoided the time-consuming column-passing process of loading large volume samples in traditional SPE through the rapid isolation of CTAB@ACMNPs with an adscititious magnet. The proposed method was successfully applied to the determination and speciation of arsenic in different water samples and suitable recoveries were obtained.

Tandem on-line continuous separations for atomic spectroscopic indirect analysis: iodide determination by ICP-AES

International Nuclear Information System (INIS)

Garcia, A.M.; Sanchez Uria, J.E.; Sanz-Medel, A.; Quintero Ortega, M.C.; Bautista, J.C.

1992-01-01

A sensitive and selective indirect determination of iodide by inductively coupled plasma emission spectrometry (ICP-AES) based on the principle of tandem on-line continuous separations as an alternative means of introducing samples into plasmas is proposed. Iodide is continuously extracted as an ion-pair into xylene by mixing the sample with Hg(II) and dipyridil solutions. The organic phase (containing the analyte in [Hg(Dipy) 2 ]I 2 form) is on-line continuously mixed with NaBH 4 (in DMF) and acetic acid solutions. Mercury vapour continuously generated from this organic phase is separated in a classical U-type gas-liquid separation device. The system has been optimized for the continuous extraction of KI, for the direct generation of cold mercury vapour from xylene and for the final ICP-AES determination of mercury. The optimised method has been applied to the determination of iodide (detection limit 20 ng/ml of iodide) in table salt and in synthetic samples. Very good agreement between found and certified results was observed. The usefulness and convenience of such alternative sample chemical pretreatment/presentation to the ICP is thus demonstrated for indirect determinations to be carried out by atomic spectroscopy methods. (authors)

Pre-Concentration of Vanadium from Stone Coal by Gravity Using Fine Mineral Spiral

Directory of Open Access Journals (Sweden)

Xin Liu

2016-08-01

Full Text Available Due to the low grade of V2O5 in stone coal, the existing vanadium extraction technologies face challenges in terms of large handling capacity, high acid consumption and production cost. The pre-concentration of vanadium from stone coal before the extraction process is an effective method to reduce cost. In this study, detailed mineral characterization of stone coal was investigated. It has been confirmed that the vanadium mainly occurs in muscovite and illite. A significant demand for an effective pre-concentration process with simple manipulation for discarding quartz and other gangue minerals is expected. Based on the mineralogical study, a new vanadium pre-concentration process using a fine mineral spiral was investigated. The experimental results showed that the separation process, which was comprised of a rougher and scavenger, could efficiently discard quartz, pyrite and apatite. A final concentrate with V2O5 grade of 1.02% and recovery of 89.6% could be obtained, with 26.9% of the raw ore being discarded as final tailings.

Spotting Separator Points at Line Terminals in Compressed Document Images for Text-line Segmentation

OpenAIRE

R, Amarnath; Nagabhushan, P.

2017-01-01

Line separators are used to segregate text-lines from one another in document image analysis. Finding the separator points at every line terminal in a document image would enable text-line segmentation. In particular, identifying the separators in handwritten text could be a thrilling exercise. Obviously it would be challenging to perform this in the compressed version of a document image and that is the proposed objective in this research. Such an effort would prevent the computational burde...

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

International Nuclear Information System (INIS)

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

2013-01-01

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

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

Analytical parameter optimization of separation process of various radionuclides. Master's thesis

Energy Technology Data Exchange (ETDEWEB)

Shamsi, A M

1992-01-01

Separation and preconcentrations of Eu, Hf and Se were studied, using an adsorption technique based on TiO[sub 2]. Characterization of titanium dioxide was done on TG/DSC and the surface area, pore size and average pore diameter measured. The influence of contact time, electrolyte composition, pH of the aqueous solution, effect of anions and cations was also investigated. The adsorption data show that Eu, Se and Hf can be preconcentrated by using 0.01 molar perchloric acid, nitric acid, and pH.7 buffer solution. Iodide, acetate, and citrate increase the adsorption of these metals, while S[sub 2]O[sub 3] decrease the adsorption of Se. The adsorption of other metal ions was also investigated. Based on these data, Co(II), Mn(II) and Ag(I) can be separated from the above metals. It can be concluded that TiO2 can be used for the separation and preconcentration of Eu, Hf and Se from dilute solution.

Chemical Separation on Silver Nanorods Surface Monitored by TOF-SIMS

Directory of Open Access Journals (Sweden)

Ondrej Petruš

2017-01-01

Full Text Available The article introduces a possible chemical separation of a mixture of two compounds on the metal nanorods surface. A silver nanorods surface has been prepared by controlled electrochemical deposition in anodic alumina oxide (AAO template. Rhodamine 6G and 4-aminothiophenol have been directly applied to the sampling point on a silver nanorods surface in an aliquot mixture. The position of the resolved compounds was analysed by time-of-flight secondary ion mass spectrometry (TOF-SIMS which measured the fragments and the molecular ions of the two compounds separated on the silver nanorods surface. Rhodamine 6G has been preconcentrated as 1.5 mm radial from the sampling point while 4-aminothiophenol formed a continuous self-assembled monolayer on the silver nanorods surface with a maximum molecular ion intensity at a distance of 0.5 mm from the sampling point. The separation of the single chemical components from the two-component mixture over the examined silver nanostructured films could clearly be shown. A fast separation on the mentioned nanotextured films was observed (within 50 s. This procedure can be easily integrated into the micro/nanofluidic systems or chips and different detection systems can be applied.

The use of selective adsorbents in capillary electrophoresis-mass spectrometry for analyte preconcentration and microreactions: a powerful three-dimensional tool for multiple chemical and biological applications.

Science.gov (United States)

Guzman, N A; Stubbs, R J

2001-10-01

Much attention has recently been directed to the development and application of online sample preconcentration and microreactions in capillary electrophoresis using selective adsorbents based on chemical or biological specificity. The basic principle involves two interacting chemical or biological systems with high selectivity and affinity for each other. These molecular interactions in nature usually involve noncovalent and reversible chemical processes. Properly bound to a solid support, an "affinity ligand" can selectively adsorb a "target analyte" found in a simple or complex mixture at a wide range of concentrations. As a result, the isolated analyte is enriched and highly purified. When this affinity technique, allowing noncovalent chemical interactions and biochemical reactions to occur, is coupled on-line to high-resolution capillary electrophoresis and mass spectrometry, a powerful tool of chemical and biological information is created. This paper describes the concept of biological recognition and affinity interaction on-line with high-resolution separation, the fabrication of an "analyte concentrator-microreactor", optimization conditions of adsorption and desorption, the coupling to mass spectrometry, and various applications of clinical and pharmaceutical interest.

A four-detector spectrometer for e--γ PAC on-line with the ISOLDE-CERN isotope separator

International Nuclear Information System (INIS)

Marques, J.G.; Correia, J.G.; Melo, A.A.; Silva, M.F. da; Soares, J.C.

1995-01-01

A four-detector e - -γ spectrometer has been installed on-line with the ISOLDE isotope separator. The spectrometer consists of two magnetic lenses for detection of conversion electrons, and two BaF 2 scintillators for γ-ray detection. The spectrometer has been equipped with a 20 kV pre-acceleration system which enables detection of conversion electrons down to 2 keV. Implantation and measurement can be performed simultaneously on a large temperature range by heating or cooling the sample holder. The advantages of using the e - -γ PAC technique on-line at ISOLDE are discussed. (orig.)

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...

Improved limits and portability over currently employed cadmium monitoring systems through preconcentration for detection by way of micro-/nanofluidic mechanisms

Science.gov (United States)

Wach, Paul

Due to risk of environmental and biological accumulation of Cadmium (Cd), improved methods of early detection and monitoring must be explored as a preventative measure. Listed as one of the top three toxic heavy metals by the Environmental Protection Agency (EPA), the effects on ecological and human systems have well documented side-effects of physical mutation, reproductive sterility, kidney failure, liver disease, bone loss, and death. Found in batteries, metal plating, pigments, plastics, and cigarettes, Cd is also used as a neutron absorber in the nuclear industry as well as having 3 known radioactive isotopes. Urine Cd levels, which have been widely used to predict whole body levels, increase when kidney damage occurs, thus increasing the importance to monitor and detect as early as possible. Although several methods of detection and monitoring are currently in use, they are insufficient for reasons including massive expense, weak specificity causing false readings, and/or a lack of portability. By exploiting naturally occurring mechanisms known to micro-/nanofluidics, a novel approach to Cd detection, measurement, and preconcentration was explored using the finite element computational software COMSOL. An open flow system of a nanochannel was explored through manipulation of the surface charge density. With a dominant negatively charged density on the walls, positive surface charge densities were adjacently placed at the center of the nanochannel causing a constriction of flow and allowing preconcentration of the analytes. When the open flow system was scaled up to a microchannel, the mechanism was found to have little effect on constriction of the flow. A preconcentration effect was discovered in a closed flow system when the adjacent patches were modeled as being impermeable to charge, causing the molecules to migrate to and remain at the central region of the microchannel once the dynamic process reached steady state. It was found to have the ability to

Simultaneous pre-concentration and separation on simple paper-based analytical device for protein analysis.

Science.gov (United States)

Niu, Ji-Cheng; Zhou, Ting; Niu, Li-Li; Xie, Zhen-Sheng; Fang, Fang; Yang, Fu-Quan; Wu, Zhi-Yong

2018-02-01

In this work, fast isoelectric focusing (IEF) was successfully implemented on an open paper fluidic channel for simultaneous concentration and separation of proteins from complex matrix. With this simple device, IEF can be finished in 10 min with a resolution of 0.03 pH units and concentration factor of 10, as estimated by color model proteins by smartphone-based colorimetric detection. Fast detection of albumin from human serum and glycated hemoglobin (HBA1c) from blood cell was demonstrated. In addition, off-line identification of the model proteins from the IEF fractions with matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) was also shown. This PAD IEF is potentially useful either for point of care test (POCT) or biomarker analysis as a cost-effective sample pretreatment method.

Graphene-based solid-phase extraction disk for fast separation and preconcentration of trace polycyclic aromatic hydrocarbons from environmental water samples.

Science.gov (United States)

Wang, Zonghua; Han, Qiang; Xia, Jianfei; Xia, Linhua; Ding, Mingyu; Tang, Jie

2013-06-01

Graphene has great potentials for the use in sample preparation due to its ultra high specific surface area, superior chemical stability, and excellent thermal stability. In our work, a novel graphene-based SPE disk was developed for separation and preconcentration of trace polycyclic aromatic hydrocarbons from environmental water samples. Based on the strong π-π stacking interaction between the analytes and graphene, the analytes extracted by graphene were eluted by cyclohexane and then determined by GC-MS. Under the optimized conditions, high flow rate (30 mL/min) and sensitivity (0.84-13 ng/L) were achieved. The proposed method was successfully applied to the analysis of real environmental water samples with recoveries ranging from 72.8 to 106.2%. Furthermore, the property of anticlogging and reusability was also improved. This work reveals great potentials of graphene-based SPE disk in environmental analytical. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Selective separation, preconcentration and determination of Pd(II ions in environmental samples by coprecipitation with a 1,2,4-triazole derivative

Directory of Open Access Journals (Sweden)

D. Ozdes

2015-01-01

Full Text Available A simple, sensitive, facile and low cost methodology, combined with flame atomic absorption spectrometry (FAAS, was employed to evaluate the selective separation and preconcentration of Pd(II ions in environmental samples by using a triazole derivative as an organic coprecipitating agent without a carrier element. The developed method was systematically investigated in different set of experimental parameters that influence the quantitative recovery of Pd(II ions. The accuracy of the method was tested by analyzing certified reference material and spike tests. The developed coprecipitation procedure has been applied to road dust, anodic slime, industrial electronic waste materials and water samples to determine their Pd(II levels. DOI: http://dx.doi.org/10.4314/bcse.v29i1.1

Moisture separator for steam generator level measurement system

International Nuclear Information System (INIS)

Cantineau, B.J.

1987-01-01

A steam generator level measurement system having a reference leg which is kept full of water by a condensation pot, has a liquid/steam separator in the connecting line between the condensation pot and the steam phase in the steam generator to remove excess liquid from the steam externally of the steam generator. This ensures that the connecting line does not become blocked. The separator pot has an expansion chamber which slows down the velocity of the steam/liquid mixture to aid in separation, and a baffle, to avoid liquid flow into the line connected to the condensate pot. Liquid separated is returned to the steam generator below the water level through a drain line. (author)

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.

Combined cation-exchange and extraction chromatographic method of pre-concentration and concomitant separation of Cu(II) with high molecular mass liquid cation exchanger after its online detection.

Science.gov (United States)

Mandal, B; Roy, U S; Datta, D; Ghosh, N

2011-08-19

A selective method has been developed for the extraction chromatographic trace level separation of Cu(II) with Versatic 10 (liquid cation exchanger) coated on silanised silica gel (SSG-V10). Cu(II) has been extracted from 0.1M acetate buffer at the range of pH 4.0-5.5. The effects of foreign ions, pH, flow-rate, stripping agents on extraction and elution have been investigated. Exchange capacity of the prepared exchanger at different temperatures with respect to Cu(II) has been determined. The extraction equilibrium constant (K(ex)) and different standard thermodynamic parameters have also been calculated by temperature variation method. Positive value of ΔH (7.98 kJ mol⁻¹) and ΔS (0.1916 kJ mol⁻¹) and negative value of ΔG (-49.16 kJ mol⁻¹) indicated that the process was endothermic, entropy gaining and spontaneous. Preconcentration factor was optimized at 74.7 ± 0.2 and the desorption constants K(desorption)¹(1.4 × 10⁻²) and K(desorption)²(9.8 × 10⁻²) were determined. The effect of pH on R(f) values in ion exchange paper chromatography has been investigated. In order to investigate the sorption isotherm, two equilibrium models, the Freundlich and Langmuir isotherms, were analyzed. Cu(II) has been separated from synthetic binary and multi-component mixtures containing various metal ions associated with it in ores and alloy samples. The method effectively permits sequential separation of Cu(II) from synthetic quaternary mixture containing its congeners Bi(III), Sn(II), Hg(II) and Cu(II), Cd(II), Pb(II) of same analytical group. The method was found effective for the selective detection, removal and recovery of Cu(II) from industrial waste and standard alloy samples following its preconcentration on the column. A plausible mechanism for the extraction of Cu(II) has been suggested. Copyright © 2011 Elsevier B.V. All rights reserved.

Separation of the lanthanides on high-efficiency bonded phases and conventional ion-exchange resins

International Nuclear Information System (INIS)

Elchuk, S.; Cassidy, R.M.

1979-01-01

High-performance liquid chromatographic separations (< 20 min) of the lanthanides are illustrated for both 5- and 10-μm bonded-phase strong-acid ion exchangers. The performance of these bonded phase packings is compared with that obtained with a 13-μm styrene-divinylbenzene resin. The eluted metal ions are detected with a variable-wavelength detector after a post-column complexation reaction. The requirements and characteristics of post-column reaction for sensitive metal ion detection after separation on high-performance columns are discussed and the linearity, reproducibility, and sensitivity of the system used in the work are illustrated. The potential of on-column preconcentration for the ultratrace (pg/mL) determination of metal ions is also discussed and illustrated. 7 figures, 2 tables

Sample extraction and injection with a microscale preconcentrator.

Energy Technology Data Exchange (ETDEWEB)

Robinson, Alex Lockwood (Advanced Sensor Technologies, Albuquerque, NM); Chan, Helena Kai Lun

2007-09-01

This report details the development of a microfabricated preconcentrator that functions as a fully integrated chemical extractor-injector for a microscale gas chromatograph (GC). The device enables parts-per-billion detection and quantitative analysis of volatile organic compounds (VOCs) in indoor air with size and power advantages over macro-scale systems. The 44 mm{sup 3} preconcentrator extracts VOCs using highly adsorptive, granular forms of graphitized carbon black and carbon molecular sieves. The micron-sized silicon cavities have integrated heating and temperature sensing allowing low power, yet rapid heating to thermally desorb the collected VOCs (GC injection). The keys to device construction are a new adsorbent-solvent filling technique and solvent-tolerant wafer-level silicon-gold eutectic bonding technology. The product is the first granular adsorbent preconcentrator integrated at the wafer level. Other advantages include exhaustive VOC extraction and injection peak widths an order of magnitude narrower than predecessor prototypes. A mass transfer model, the first for any microscale preconcentrator, is developed to describe both adsorption and desorption behaviors. The physically intuitive model uses implicit and explicit finite differences to numerically solve the required partial differential equations. The model is applied to the adsorption and desorption of decane at various concentrations to extract Langmuir adsorption isotherm parameters from effluent curve measurements where properties are unknown a priori.

Methylmercury in water samples at the pg/L level by online preconcentration liquid chromatography cold vapor-atomic fluorescence spectrometry

Energy Technology Data Exchange (ETDEWEB)

Brombach, Christoph-Cornelius [Trace Element Speciation Laboratory, Department of Chemistry, Meston Walk, University of Aberdeen, Aberdeen AB24 3UE (United Kingdom); Chen, Bin; Corns, Warren T. [PS Analytical, Arthur House, Crayfields Industrial Estate, Main Road, Orpington, Kent BR5 3HP (United Kingdom); Feldmann, Jörg [Trace Element Speciation Laboratory, Department of Chemistry, Meston Walk, University of Aberdeen, Aberdeen AB24 3UE (United Kingdom); Krupp, Eva M., E-mail: e.krupp@abdn.ac.uk [Trace Element Speciation Laboratory, Department of Chemistry, Meston Walk, University of Aberdeen, Aberdeen AB24 3UE (United Kingdom)

2015-03-01

Ultra-traces of methylmercury at the sub-ppt level can be magnified in the foodweb and is of concern. In environmental monitoring a routine robust analytical method is needed to determine methylmercury in water. The development of an analytical method for ultra-trace speciation analysis of methylmercury (MeHg) in water samples is described. The approach is based on HPLC-CV-AFS with on-line preconcentration of water samples up to 200 mL, resulting in a detection limit of 40 pg/L (ppq) for MeHg, expressed as Hg. The unit consists of an optimized preconcentration column filled with a sulfur-based sorption material, on which mercury species are preconcentrated and subsequently eluted, separated and detected via HPLC-CV-AFS (high performance liquid chromatography–cold vapor atomic fluorescence spectrometry). During the method development a type of adsorbate material, the pH dependence, the sample load rate and the carry-over were investigated using breakthrough experiments. The method shows broad pH stability in the range of pH 0 to 7, without the need for buffer addition and shows limited matrix effects so that MeHg is quantitatively recovered from sewage, river and seawater directly in the acidified samples without sample preparation. - Highlights: • We demonstrate that a novel mixture of thiourea-thiolsilica shows an excellent trapping of MeHg between a broad pH range 1–6. • We develop the method so that it can potentially be automated for inorganic and methyl-mercury. • The method is matrix independent with highly accurate results for MeHg in hair CRM extracts and spiked water samples • The limit of detection is around 40 pg/L when just 200 mL sample is used, without any intensive preparation.

Methylmercury in water samples at the pg/L level by online preconcentration liquid chromatography cold vapor-atomic fluorescence spectrometry

International Nuclear Information System (INIS)

Brombach, Christoph-Cornelius; Chen, Bin; Corns, Warren T.; Feldmann, Jörg; Krupp, Eva M.

2015-01-01

Ultra-traces of methylmercury at the sub-ppt level can be magnified in the foodweb and is of concern. In environmental monitoring a routine robust analytical method is needed to determine methylmercury in water. The development of an analytical method for ultra-trace speciation analysis of methylmercury (MeHg) in water samples is described. The approach is based on HPLC-CV-AFS with on-line preconcentration of water samples up to 200 mL, resulting in a detection limit of 40 pg/L (ppq) for MeHg, expressed as Hg. The unit consists of an optimized preconcentration column filled with a sulfur-based sorption material, on which mercury species are preconcentrated and subsequently eluted, separated and detected via HPLC-CV-AFS (high performance liquid chromatography–cold vapor atomic fluorescence spectrometry). During the method development a type of adsorbate material, the pH dependence, the sample load rate and the carry-over were investigated using breakthrough experiments. The method shows broad pH stability in the range of pH 0 to 7, without the need for buffer addition and shows limited matrix effects so that MeHg is quantitatively recovered from sewage, river and seawater directly in the acidified samples without sample preparation. - Highlights: • We demonstrate that a novel mixture of thiourea-thiolsilica shows an excellent trapping of MeHg between a broad pH range 1–6. • We develop the method so that it can potentially be automated for inorganic and methyl-mercury. • The method is matrix independent with highly accurate results for MeHg in hair CRM extracts and spiked water samples • The limit of detection is around 40 pg/L when just 200 mL sample is used, without any intensive preparation

Ultra-trace monitoring of copper in environmental and biological samples by inductively coupled plasma atomic emission spectrometry after separation and preconcentration by using octadecyl silica membrane disks modified by a new schiff's base

Directory of Open Access Journals (Sweden)

Mohammad Reza Ganjali

2004-04-01

Full Text Available Ultra-trace amounts of Cu(II were separated and preconcentrated by solid phase extraction on octadecyl-bonded silica membrane disks modified with a new Schiff,s base (Bis- (2-Hydroxyacetophenone -2,2-dimethyl-1,3-propanediimine (SBTD followed by elution and inductively coupled plasma atomic emission spectrometric detection. The method was applied as a separation and detection method for copper(II in environmental and biological samples. Extraction efficiency and the influence of sample matrix, flow rate, pH, and type and minimum amount of stripping acid were investigated. The concentration factor and detection limit of the proposed method are 500 and 12.5 pg mL-1, respectively.

Separation of magnetic field lines

International Nuclear Information System (INIS)

Boozer, Allen H.

2012-01-01

The field lines of magnetic fields that depend on three spatial coordinates are shown to have a fundamentally different behavior from those that depend on two coordinates. Unlike two-coordinate cases, a flux tube in a magnetic field that depends on all three spatial coordinates that has a circular cross section at one location along the tube characteristically has a highly distorted cross section at other locations. In an ideal evolution of a magnetic field, the current densities typically increase. Crudely stated, if the current densities increase by a factor σ, the ratio of the long to the short distance across a cross section of a flux tube characteristically increases by e 2σ , and the ratio of the longer distance to the initial radius increases as e σ . Electron inertia prevents a plasma from isolating two magnetic field structures on a distance scale shorter than c/ω pe , which is about 10 cm in the solar corona, and reconnection must be triggered if σ becomes sufficiently large. The radius of the sun, R ⊙ =7×10 10 cm is about e 23 times larger, so when σ≳23, two lines separated by c/ω pe at one location can be separated by the full scale of any magnetic structures in the corona at another. The conditions for achieving a large exponentiation, σ, are derived, and the importance of exponentiation is discussed.

Preconcentration of plutonium radionuclides from natural waters

International Nuclear Information System (INIS)

Wong, K.M.; Nioshkin, V.E.; Jokela, T.A.

1978-02-01

A large volume water sampler using manganese dioxide impregnated cartridges for the in situ separation of plutonium in sea water and ground water was studied. Plutonium concentrations obtained by this technique are compared with a radiochemical coprecipitation method. Consistent results were obtained between the two methods for water samples from the Pacific Ocean and Enewetak lagoon. Different results were noted from samples collected in the Enewetak reef and ground water stations. Using this preconcentration technique and the coprecipitation method it was shown that the physical-chemical characteristics of Pu in Enewetak reef and ground water are different from the lagoon and open ocean

Isotope separation system

International Nuclear Information System (INIS)

Lehmann, J.-C.

1975-01-01

A description is given of an isotope separation device comprising a system for converting into gaseous form a first and second isotope to be separated, a monochromatic excitation light source to excite the gaseous molecules of these two isotopes in a distinct manner, a first and second receiver to collect selectively the molecules of the first and second distinctly excited isotopes. The frequency FL of the excitation light is selected between a lower limit and a higher limit F2 + 1/2 LD, depending on the frequences F1 and F2 of two absorption lines near this first and second isotope. The difference DF between these two frequencies F1 and F2 is less than the Doppler width LD of each one of these lines and greater than the natural width LN of each of these two lines and also the width of line LR of the excitation light source. The probability that the molecules will be excited by this light depends on the direction of their displacement to a major and different extent for both isotopes. An ionising light source LI is set up to irradiate the seat of interaction between the excitation light and the gaseous molecules with an ionisation light able to ionise the excited molecules without ionising the molecules that are not excited. The receivers are able to collect selectively the ionised molecules. A sufficiently low gas pressure is selected for the distance between the place of interaction and the first receiver to be less than double the free mean travel of the molecules in the gas [fr

26 CFR 1.414(r)-3 - Separate line of business.

Science.gov (United States)

2010-04-01

... business must have its own separate management. A line of business has its own separate management only if... houses a centralized procurement, marketing, and billing operation for all of its lines of business. None of the procurement, marketing, or billing employees specializes in any particular line of business...

Automated 2D peptide separation on a 1D nano-LC-MS system

DEFF Research Database (Denmark)

Taylor, Paul; Nielsen, Peter A; Trelle, Morten Beck

2009-01-01

the on-line separation of highly complex peptide mixtures directly coupled with mass spectrometry-based identification. Here, we present a variation of the traditional MudPIT protocol, combining highly sensitive chromatography using a nanoflow liquid chromatography system (nano-LC) with a two...

Solid phase selective separation and preconcentration of Cu(II) by Cu(II)-imprinted polymethacrylic microbeads.

Science.gov (United States)

Dakova, Ivanka; Karadjova, Irina; Ivanov, Ivo; Georgieva, Ventsislava; Evtimova, Bisera; Georgiev, George

2007-02-12

Ion-imprinted polymer (IIP) particles are prepared by copolymerization of methacrylic acid as monomer, trimethylolpropane trimethacrylate as crosslinking agent and 2,2'-azo-bis-isobutyronitrile as initiator in the presence of Cu(II), a Cu(II)-4-(2-pyridylazo)resorcinol (Cu(II)-PAR) complex, and PAR only. A batch procedure is used for the determination of the characteristics of the Cu(II) solid phase extraction from the IIP produced. The results obtained show that the Cu(II)-PAR IIP has the greatest adsorption capacity (37.4 micromol g(-1) of dry copolymer) among the IIPs investigated. The optimal pH value for the quantitative preconcentration is 7, and full desorption is achieved by 1 M HNO(3). The selectivity coefficients (S(Cu/Me)) for Me=Ni(II), Co(II) are 45.0 and 38.5, respectively. It is established that Cu(II)-PAR IIPs can be used repeatedly without a considerable adsorption capacity loss. The determination of Cu(II) ions in seawater shows that the interfering matrix does not influence the preconcentration and selectivity values of the Cu(II)-PAR IIPs. The detection and quantification limits are 0.001 micromol L(-1) (3sigma) and 0.003 micromol L(-1) (6sigma), respectively.

Plasma emission spectroscopy (DCP) for rare earths determination in waters from Morro do Ferro (MG) Brazil, after chromatographic preconcentration

International Nuclear Information System (INIS)

Figueiredo, A.M.R. de.

1987-01-01

Rare earth determinations in surface and well waters from Morro do Ferro was studied using chemical preconcentration methods of the group and plasma emission spectroscopy excited by direct current are - DCP. A method that combines retention in alumina is HF medium with ion exchange for the preconcentration of the group was developed in semi micro scale. DCP determination, in the sequencial mode by using mixed standards containing, Y, La, Ce, Nd, Pr, Sm, Eu, Ga, Tb, Dy, Er, Yb and Al, principal concentrate componentes was studied by analysis of the profile of each spectral line. Principal cations, anions, ph and Eh were determined. Semi-micro techniques were developed for anions preconcentration and for determination of sulphate, phosphate and carbonate. (M.J.C.) [pt

Selenium speciation in human urine samples by LC- and CE-ICP-MS-separation and identification of selenosugars

DEFF Research Database (Denmark)

Gammelgaard, Bente; Bendahl, L.

2004-01-01

at ambient temperature and methanol extraction. A pre-concentration factor of 10 was achieved with this procedure. On occasions when a pre-concentration factor of 100 was obtained by lyophilsation and methanol extraction, at least 10 selenium compounds were separated in the urine sample. Urine samples were...

A Fully-Integrated MEMS Preconcentrator for Rapid Gas Sampling (Preprint)

National Research Council Canada - National Science Library

Bae, Byunghoon; Yeom, Junghoon; Radadia, Adarsh D; Masel, Richard I; Shannon, Mark A

2006-01-01

.... The unprecedented speed of this preconcentrator (chemical warfare agents, toxic industrial compounds (TICs), and other volatile compounds in seconds, rather than tens of minutes with conventional systems.

Sb(III) and Sb(V) separation and analytical speciation by a continuous tandem on-line separation device in connection with inductively coupled plasma atomic emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Menendez Garcia, A. [Oviedo Univ. (Spain). Dept. of Phys. and Anal. Chem.; Perez Rodriguez, M.C. [Oviedo Univ. (Spain). Dept. of Phys. and Anal. Chem.; Sanchez Uria, J.F. [Oviedo Univ. (Spain). Dept. of Phys. and Anal. Chem.; Sanz-Medel, A. [Oviedo Univ. (Spain). Dept. of Phys. and Anal. Chem.

1995-09-01

A sensitive, precise and automated non-chromatographic method for Sb(III) and Sb(V) analytical speciation based on a continuous tandem on-line separation device in connection with inductively coupled plasma-atomic emission (ICP-AES) detection is proposed. Two on-line successive separation steps are included into this method: a continuous liquid-liquid extraction of Sb(III) with ammonium pyrrolidine dithiocarbamate (APDC) into methylisobuthylketone (MIBK), followed by direct stibine generation from the organic phase. Both separation steps are carried out in a continuous mode and on-line with the ICP-AES detector. Optimization of experimental conditions for the tandem separation and ICP-AES detection are investigated in detail. Detection limits for Sb(III) were 3 ng.mL{sup -1} and for Sb(V) 8 ng.mL{sup -1}. Precisions observed are in the range {+-} 5%. The proposed methodology has been applied to Sb(III) and Sb(V) speciation in sea-water samples. (orig.)

Electrochemical preconcentration and hydride generation methods for trace determination of selenium by atomic absorption spectrometry

International Nuclear Information System (INIS)

Bye, R.

1986-01-01

The use of atomic absorption spectrometry in combination with two different preconcentration/separation techniques for the determination of trace concentrations of selenium is described. Electrochemical preconcentration onto a platinum electrode with a subsequent atomization of selenium is discussed briefly. Several parameters are considered such as the presence of depolarizers, and the temperature of the electrolyzed solutions. Special attention is payed to the efficiency of the atomization step, and a method to improve this is proposed. Applications of the technique to real samples are also reported. Secondly, the separation of the selenium as the volatile selenium hydride from the sample solution is considered. Several papers in this thesis deal with commonly occurring interferants as nickel and copper and with ways of minimizing or avoiding the interferring effects, whereas other papers relate to more theoretical aspects of the hydride generation process. New methods for the determination of selenium in technical samples with high contents of nickel and copper are also presented

On-line preconcentration of ultra-trace thallium(I in water samples with titanium dioxide nanoparticles and determination by graphite furnace atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Saeid Asadpour

2016-11-01

Full Text Available A new method has been developed for the determination of Tl(I based on simultaneous sorption and preconcentration with a microcolumn packed with TiO2 nanoparticle with a high specific surface area prepared by Sonochemical synthesis prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS. The optimum experimental parameters for preconcentration of thallium, such as elution condition, pH, and sample volume and flow rate have been investigated. Tl(I can be quantitatively retained by TiO2 nanoparticles at pH 9.0, then eluted completely with 1.0 mol L−1 HCl. The adsorption capacity of TiO2 nanoparticles for Tl(I was found to be 25 mg g−1. Also detection limit, precision (RSD, n = 8 and enrichment factor for Tl(I were 87 ng L−1, 6.4% and 100, respectively. The method has been applied for the determination of trace amounts of Tl(I in some environmental water samples with satisfactory results.

Catechol functionalized aminopropyl silica gel: synthesis, characterization and preconcentrative separation of uranium(VI) from thorium(IV)

International Nuclear Information System (INIS)

Metilda, P.; Mary Gladis, J.; Prasada Rao, T.P.

2005-01-01

A novel solid phase extractant is prepared by chemically immobilizing catechol with diazotized aminopropyl silica gel. The resulting catechol functionalized silica gel (CASG) was characterized by FTIR, and microanalysis and was used for selective enrichment of uranium(VI) from other inorganic ions. The optimum pH range for maximum sorption of uranium(VI) and thorium(IV) was found to be in the range 3.5-6.0. The above actinides were eluted with 10 cm 3 of 1.0 mol dm -3 HCl and determined by using an Arsenazo III spectrophotometric procedure. The calibration graph was rectilinear over the uranium(VI) concentration in the range 2-100 μg dm -3 with a relative standard deviation of 2.15% (for 25 μg of uranium(VI) present in 1.0 dm 3 of sample). The validation of the developed preconcentration procedure was carried out by analyzing marine sediment (MESS-3, NRC, Canada) and soil (IAEA soil-7, Austria) reference materials. The developed preconcentration method enables a simple instruments like a spectrophotometer gave comparable values of uranium(VI) to that of standard inductively coupled plasma-mass spectrometric values during the analysis of real soil and sediment samples. (orig.)

Determination of tellurium at ultra-trace levels in drinking water by on-line solid phase extraction coupled to graphite furnace atomic absorption spectrometer

International Nuclear Information System (INIS)

Pedro, Juana; Stripekis, Jorge; Bonivardi, Adrian; Tudino, Mabel

2008-01-01

In this paper, two time-based flow injection (FI) separation pre-concentration systems coupled to graphite furnace atomic absorption spectrometry (GFAAS) for tellurium determination are studied and compared. The first alternative involves the pre-concentration of the analyte onto Dowex 1X8 employed as packaging material of a micro-column inserted in the flow system. The second set-up is based on the co-precipitation of tellurium with La(OH) 3 followed by retention onto XAD resins. Both systems are compared in terms of limit of detection, linear range, RSD%, sample throughput, micro-columns lifetime and aptitude for fully automatic operation. The features of the Dowex system are: 37% efficiency of retention and an enhancement factor of 42 for a pre-concentration time of 180 seconds (sample flow rate = 3 ml min -1 ) with acetic acid elution volumes of 80 μl. The detection limit (3 s) is 7 ng l -1 and the relative standard deviation (n = 7200 ng l -1 ) is 5.8%. The analytical performance of the XAD system is: 72% efficiency of retention and an enhancement factor of 25 for a pre-concentration time of 180 s (sample flow rate = 3 ml min -1 ) with nitric acid elution volumes of 300 μl. The detection limit is 66 ng l -1 and the relative standard deviation (n = 7200 ng l -1 ) is 8.3%. Applications to the determination of tellurium in tap water and the validation of the analytical methodology employing SRM 1643e as certified reference material are shown

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

International Nuclear Information System (INIS)

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

2009-01-01

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

Online preconcentration and determination of trace levels cadmium in water samples using flow injection systems coupled with flame AAS

Energy Technology Data Exchange (ETDEWEB)

Zhao, Songlin; Liang, Huading; Yan, Hua; Yan, Zhengzhong; Chen, Suqing; Zhu, Xiandi; Cheng, Miaoxian [School of Pharmaceutical and Chemical Engineering, Taizhou University (China)

2010-02-15

A rapid and sensitive method for the determination of trace levels cadmium in water samples by flame atomic absorption spectrometry was developed. It is based on the online sorption of Cd(II) ions on a microcolumn packed with HCl treated bamboo charcoal. In a pH range of 5.0-7.5, Cd(II) ions were effectively retained on the microcolumn, which exhibited fast kinetics, permitting the use of high sample flow rates up to at least 12.8 mL/min without the loss of retention efficiency. The retained Cd(II) ions were quantitatively eluted with HCl (2.0 mol/L) for an online determination. With a preconcentration time of 80 s at a sample loading flow rate of 8.6 mL/min, a sensitivity enhancement factor of 63 was obtained compared with the slope of the linear portion of the calibration curves before and after preconcentration. The calibration graph using the preconcentration system for cadmium was linear with a correlation coefficient of 0.9997, at levels from 1-40 ng/mL. The precision (RSD) for 11 replicate measurements were 3.2% for the determination of 5 ng/mL Cd(II) and 1.8% for 20 ng/mL Cd(II), respectively, and the detection limit (3s) was 0.36 ng/mL. The accuracy was assessed through the determination of a certified reference material, and also through recovery experiments. (Abstract Copyright [2010], Wiley Periodicals, Inc.)

Nano-level determination of copper with atomic absorption spectrometry after pre-concentration on N,N-(4-methyl-1,2-phenylene)diquinoline-2-carboxamide-naphthalene

Energy Technology Data Exchange (ETDEWEB)

Rezaei, Behzad, E-mail: rezaei@cc.iut.ac.ir [Department of Chemistry, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of); Sadeghi, Elham; Meghdadi, Soraia [Department of Chemistry, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of)

2009-09-15

A novel, simple, sensitive and effective method has been developed for selective extraction and pre-concentration of copper on N,N-(4-methyl-1,2-phenylene)diquinoline-2-carboxamide-naphthalene. After pre-concentration, copper was eluted from sorbent with hydrochloric acid, and then flame atomic absorption spectrometry (FAAS) was used for its determination. The effect of pH, sample flow rate and the volume and concentration of eluent on the recovery of the analyte was investigated and the optimum conditions were established. A pre-concentration factor of 400, and an adsorption capacity of 6.9 mg g{sup -1} of the solid-phase sorbent or 82.8 mg g{sup -1} of ligand was achieved using the optimum conditions. The calibration graph was linear in the range of 1.0-4000 ng mL{sup -1} with the detection limit of 1.0 ng mL{sup -1}. A R.S.D. value of 2.4% was obtained by this method for 400 ng mL{sup -1} of Cu{sup 2+} solution. This procedure has been successfully applied to separate and determine the ultra trace levels of copper in the environmental samples, free from the interference of some diverse ions.

Preconcentration of Arsenic in Water Samples Using the Composition-Induced Phase Separation Method and Determination by ETAAS

Directory of Open Access Journals (Sweden)

Güçoğlu M.

2013-04-01

Full Text Available A new phase transition microextraction method was developed for determination of trace amount of arsenic ions in water samples in this work. The method is based on the critical point of miscibility of solvents. In this method the mixed solution of sample and organic solvent is initially homogeneous but is separated into two phases by adding a secondary solvent (modifier. In acidic medium As(V was complexed with ammonium molybdate, this complex was quantitatively extracted to the mixture of organic solvent (acetonitrile/methyl isobutyl ketone before ETAAS determination. Total inorganic arsenic (III, V was extracted similarly after oxidation of As(III to As(V with nitric acid. Concentration of As(III was calculated by difference in the concentration between total arsenic and As(V. Optimization of the experimental conditions and instrumental parameters was investigated in detail. A detection limit of 0.05 μgL−1 with enrichment factor of 85 was achieved for only 5 mL of sample. The analytical curve was linear in the concentration range of 0.25-4.00 μgL−1. Relative standard deviation (RSD for 10 replicate determinations of 2.0 μgL−1 of As(V was 4,1%. The method was successfully applied to preconcentration and determination of arsenic in real water samples.

Human comment dynamics in on-line social systems

Science.gov (United States)

Wu, Ye; Zhou, Changsong; Chen, Maoying; Xiao, Jinghua; Kurths, Jürgen

2010-12-01

Human comment is studied using data from ‘tianya’ which is one of the most popular on-line social systems in China. We found that the time interval between two consecutive comments on the same topic, called inter-event time, follows a power-law distribution. This result shows that there is no characteristic decay time on a topic. It allows for very long periods without comments that separate bursts of intensive comments. Furthermore, the frequency of a different ID commenting on a topic also follows a power-law distribution. It indicates that there are some “hubs” in the topic who lead the direction of the public opinion. Based on the personal comments habit, a model is introduced to explain these phenomena. The numerical simulations of the model fit well with the empirical results. Our findings are helpful for discovering regular patterns of human behavior in on-line society and the evolution of the public opinion on the virtual as well as real society.

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.

Preconcentration and extraction of copper(II) on activated carbon ...

African Journals Online (AJOL)

Activated carbon modified method was used for the preconcentration and ... in real samples such as tap water, wastewater and a synthetic water sample by flame ... KEY WORDS: Copper(II), Solid phase extraction, Activated carbon, Flame ...

The Cryo-Thermochromatographic Separator (CTS) A new rapid separation and alpha-detection system for on-line chemical studies of highly volatile osmium and hassium (Z=108) tetroxides

CERN Document Server

Kirbach, U W; Gregorich, K E; Lee, D M; Ninov, V; Omtvedt, J P; Patin, J B; Seward, N K; Strellis, D A; Sudowe, R; Türler, A; Wilk, P A; Zielinski, P M; Hoffman, D C; Nitsche, H

2002-01-01

The Cryo-Thermochromatographic Separator (CTS) was designed and constructed for rapid, continuous on-line separation and simultaneous detection of highly volatile compounds of short-lived alpha-decaying isotopes of osmium and hassium (Hs, Z=108). A flowing carrier gas containing the volatile species is passed through a channel formed by two facing rows of 32 alpha-particle detectors, cooled to form a temperature gradient extending from 247 K at the channel entrance down to 176 K at the exit. The volatile species adsorb onto the SiO sub 2 -coated detector surfaces at a characteristic deposition temperature and are identified by their observed alpha-decay energies. The CTS was tested on-line with OsO sub 4 prepared from sup 1 sup 6 sup 9 sup - sup 1 sup 7 sup 3 Os isotopes produced in sup 1 sup 1 sup 8 sup , sup 1 sup 2 sup 0 Sn( sup 5 sup 6 Fe, 3,4,5n) reactions. An adsorption enthalpy for OsO sub 4 of -40.2+-1.5 kJ/mol on SiO sub 2 was deduced by comparing the measured deposition distribution with Monte Carlo...

Production of chemically reactive radioactive ion beams through on-line separation

International Nuclear Information System (INIS)

Joinet, A.

2003-10-01

The ISOL (isotope separation on line) allows the production of secondary radioactive ion beams through spallation or fragmentation or fission reactions that take place in a thick target bombarded by a high intensity primary beam. The challenge is to increase the intensity and purity of the radioactive beam. The optimization of the system target/source requires the right choice of material for the target by taking into account the stability of the material, its reactivity and the ionization method used. The target is an essential part of the system because radioactive elements are generated in it and are released more or less quickly. Tests have been made in order to select the best fitted material for the release of S, Se, Te, Ge and Sn. Materials tested as target filling are: ZrO 2 , Nb, Ti, V,TiO 2 , CeO x , ThO 2 , C, ZrC 4 and VC). Other molecules such as: COSe, COS, SeS, COTe, GeS, SiS, SnS have been studied to ease the extraction of recoil nuclei (Se, S, Te, Ge and Sn) produced inside the target

Preconcentration and atomization of arsane in a dielectric barrier discharge with detection by atomic absorption spectrometry

Czech Academy of Sciences Publication Activity Database

Novák, Petr; Dědina, Jiří; Kratzer, Jan

2016-01-01

Roč. 88, č. 11 (2016), s. 6064-6070 ISSN 0003-2700 R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : dielectric barrier discharge * hydride generation * arsenic preconcentration Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 6.320, year: 2016

Application of a field flow preconcentration system with a minicolumn packed with amberlite XAD-4/1-(2-pyridylazo)-2-naphtol and a flow injection-flame atomic adsorption spectrometric system for lead determination in sea water

International Nuclear Information System (INIS)

Carmen Yebra, M. del; Rodriguez, L.; Puig, L.; Moreno-Cid, A.

2002-01-01

A field flow preconcentration technique involving a minicolumn containing Amberlite XAD-4 impregnated with the complexing agent 1-(2-pyridylazo)-2-naphthol was used to preconcentrate lead from seawater. Elution of retained lead on the minicolumns was performed by a flow-injection-flame atomic absorption spectrometric system. Factorial designs have been used to optimize the field flow preconcentration system and the flow injection elution process. Factors such as sample pH, sample flow-rate, eluent concentration and volume (hydrochloric acid), elution flow-rate and minicolumn diameter were considered. The results suggest that the sample flow-rate and the eluent volume are statistically significant factors. The detection limit (3σ) of the procedure was 5 ng/L for a sample volume of 1000 ml. The precision (expressed as relative standard deviation) for eleven independent determinations reached values of 4.0-3.1 % in lead solutions of 50-200 ng/L. This procedure has been successfully applied to the determination of lead in seawater from Galicia (Spain). (author)

Preconcentration of uranium, thorium, zirconium, titanium, molybdenum and vanadium with oxine supported on microcrystalline naphthalene and their determinations by ICP-AES

International Nuclear Information System (INIS)

Kumar, Naveen; Kumar, Sanjay; Kumar, Vijay; Nandakishore, S.S.; Bangroo, P.N.

2013-01-01

As an effective technique for separation and preconcentration of trace elements, solid-liquid extraction with microcrystalline naphthalene has received great attention in recent years. The application of the adsorption of the metal complexes on microcrystalline naphthalene has greatly enhanced the utility of solid-liquid extraction in trace analysis. A survey of the literature revealed that single element detection techniques such as spectrophotometry, atomic absorption spectrometry, and polarography were mostly combined with this separation method. However, multi-element simultaneous detection techniques, like ICP-AES and ICP-MS were seldom used as the detectors in this solid-liquid extraction method. The aim of this work was to attempt to adopt the reagent oxine for the separation and subsequent determination of U, Th, Zr, Ti, Mo and V by ICP-AES, after adsorption of their oxinate complexes on microcrystalline naphthalene

Separation/preconcentration of trace Pb(II and Cd(II with 2-mercaptobenzothiazole impregnated Amberlite XAD-1180 resin and their determination by flame atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Şerife Tokalıoğlu

2017-01-01

Full Text Available A new chelating resin, 2-mercaptobenzothiazole loaded Amberlite XAD-1180 was prepared and used for separation and preconcentration of Cd(II and Pb(II ions prior to their determinations by flame atomic absorption spectrometry. The optimum pH for simultaneous retention of the elements and the best elution means for their simultaneous elution were 9.5 and 2 mol L−1 HNO3, respectively. The detection limits for Cd(II and Pb(II were 0.35 and 5.0 μg L−1, respectively. The accuracy of the method was confırmed both by analyzing the certified reference material (RM 8704 Buffalo river sediment and performing recovery studies.

An introduction to the Advanced Testing Line for Actinide Separations (ATLAS)

International Nuclear Information System (INIS)

Pope, N.G.; Yarbro, S.L.; Schreiber, S.B.; Day, R.S.

1992-03-01

The Advanced Testing Line for Actinide Separations (ATLAS) will evaluate promising plutonium recovery process modifications and new technologies. It combines advances in process chemistry, process control, process analytical chemistry, and process engineering. ATLAS has a processing capability equal to other recovery systems but without the pressure to achieve predetermined recovery quotas

Catechol functionalized aminopropyl silica gel: synthesis, characterization and preconcentrative separation of uranium(VI) from thorium(IV)

Energy Technology Data Exchange (ETDEWEB)

Metilda, P.; Mary Gladis, J.; Prasada Rao, T.P. [Regional Research Lab. (CSIR), Trivandrum (India)

2005-07-01

A novel solid phase extractant is prepared by chemically immobilizing catechol with diazotized aminopropyl silica gel. The resulting catechol functionalized silica gel (CASG) was characterized by FTIR, and microanalysis and was used for selective enrichment of uranium(VI) from other inorganic ions. The optimum pH range for maximum sorption of uranium(VI) and thorium(IV) was found to be in the range 3.5-6.0. The above actinides were eluted with 10 cm{sup 3} of 1.0 mol dm{sup -3} HCl and determined by using an Arsenazo III spectrophotometric procedure. The calibration graph was rectilinear over the uranium(VI) concentration in the range 2-100 {mu}g dm{sup -3} with a relative standard deviation of 2.15% (for 25 {mu}g of uranium(VI) present in 1.0 dm{sup 3} of sample). The validation of the developed preconcentration procedure was carried out by analyzing marine sediment (MESS-3, NRC, Canada) and soil (IAEA soil-7, Austria) reference materials. The developed preconcentration method enables a simple instruments like a spectrophotometer gave comparable values of uranium(VI) to that of standard inductively coupled plasma-mass spectrometric values during the analysis of real soil and sediment samples. (orig.)

Gold volatile species atomization and preconcentration in quartz devices for atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Arslan, Yasin [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Mehmet Akif Ersoy University, Faculty of Arts & Sciences, Chemistry Department, 15030 Burdur (Turkey); Musil, Stanislav; Matoušek, Tomáš; Kratzer, Jan [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Dědina, Jiří, E-mail: dedina@biomed.cas.cz [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic)

2015-01-01

The on-line atomization of gold volatile species was studied and the results were compared with thermodynamic calculations in several quartz atomizers, namely: diffusion flame, flame-in-gas-shield, flame-in-plain-tube, externally heated T-tube and externally heated flame-in-T-tube. Atomization mechanism in the explored devices is proposed, where volatile species are converted to thermodynamically stable AuH at elevated temperature over 500 °C and then atomized by an interaction with a cloud of hydrogen radicals. Because of its inherent simplicity and robustness, diffusion flame was employed as a reference atomizer. It yielded atomization efficiency of 70 to 100% and a very good long time reproducibility of peak area sensitivity: 1.6 to 1.8 s μg{sup −1}. Six and eleven times higher sensitivity, respectively, was provided by atomizers with longer light paths in the observation volume, i.e. externally heated T-tube and externally heated flame-in-T-tube. The latter one, offering limit of detection below 0.01 μg ml{sup −1}, appeared as the most prospective for on-line atomization. Insight into the mechanism of atomization of gold volatile species, into the fate of free atoms and into subsequent analyte transfer allowed to assess possibilities of in-atomizer preconcentration of gold volatile species: it is unfeasible with quartz atomizers but a sapphire tube atomizer could be useful in this respect. - Highlights: • On-line atomization of gold volatile species for AAS in quartz devices was studied. • Atomization mechanism was proposed and atomization efficiency was estimated. • Possibilities of in-atomizer preconcentration of gold volatile species were assessed.

An electrodynamic preconcentrator integrated thermoelectric biosensor chip for continuous monitoring of biochemical process

International Nuclear Information System (INIS)

Choi, Yong-Hwan; Kim, Min-gu; Kang, Dong-Hyun; Sim, Jaesam; Kim, Jongbaeg; Kim, Yong-Jun

2012-01-01

This paper proposes an integrated sensor chip for continuous monitoring of a biochemical process. It is composed of a preconcentrator and a thermoelectric biosensor. In the preconcentrator, the concentration of the injected biochemical sample is electrodynamically condensed. Then, in the downstream thermoelectric biosensor, the preconcentrated target molecules react with sequentially injected capture molecules and generate reaction heat. The reaction heat is detected based on the thermoelectric effect, and an integrated split-flow microchannel improves the sensor stability by providing ability to self-compensate thermal noise. These sequential preconcentration and detection processes are performed in completely label-free and continuous conditions and consequently enhance the sensor sensitivity. The performance of the integrated biosensor chip was evaluated at various flow rates and applied voltages. First, in order to verify characteristics of the fabricated preconcentrator, 10 µm -diameter polystyrene (PS) particles were used. The particles were concentrated by applying ac voltage from 0 to 16 V pp at 3 MHz at various flow rates. In the experimental result, approximately 92.8% of concentration efficiency was achieved at a voltage over 16 V pp and at a flow rate below 100 µl h −1 . The downstream thermoelectric biosensor was characterized by measuring reaction heat of biotin–streptavidin interaction. The preconcentrated streptavidin-coated PS particles flow into the reaction chamber and react with titrated biotin. The measured output voltage was 288.2 µV at a flow rate of 100 µl h −1 without preconcentration. However, by using proposed preconcentrator, an output voltage of 812.3 µV was achieved with a 16 V pp -applied preconcentration in the same given sample and flow rate. According to these results, the proposed label-free biomolecular preconcentration and detection technique can be applied in continuous and high-throughput biochemical applications

Can the waiting-point nucleus 78Ni be studied at an on-line mass-separator?

Science.gov (United States)

Wöhr, A.; Andreyev, A.; Bijnens, N.; Breitenbach, J.; Franchoo, S.; Huyse, M.; Kudryavtsev, Y. A.; Piechaczek, A.; Raabe, R. R.; Reusen, I.; Vermeeren, L.; Van Duppen, P.

1997-02-01

Short-lived nickel isotopes have been studied using a chemically selective Ion Guide Laser Ion Source (IGLIS) based on resonance ionisation of atoms at the Leuven Isotope Separator On-Line (LISOL) separator. The decay properties of different Ni isotopes have been studied using β-γ-coincidences. Experimental production rates of proton induced fission of 238U are obtained for 69,71Ni. These numbers are in a strong disagreement with Silberg-Tsao calculations.

Application of modified multiwalled carbon nanotubes as a sorbent for simultaneous separation and preconcentration trace amounts of Au(III) and Mn(II)

International Nuclear Information System (INIS)

Shamspur, Tayebeh; Mostafavi, Ali

2009-01-01

A solid phase extraction procedure is proposed for simultaneous separation and preconcentration trace amounts of Au(III) and Mn(II) in an aqueous medium by using a column of multiwalled carbon nanotubes modified with the analytical reagent N,N'-bis(2-hydroxybenzylidene)-2,2'(aminophenylthio)ethane. An implementation, it was found that the sorption is quantitative in the pH range 5.0-7.5, whereas quantitative desorption occurs instantaneously with 4.0 mL of 0.1 mol L -1 Na 2 S 2 O 3. Selected elements were also determined by flame atomic absorption spectrometry. Linearity was maintained between 0.2 ng mL -1 to 25 μg mL -1 for gold and 0.08 ng mL -1 to 5 μg mL -1 for manganese in the original solution. Various parameters such as the effect of pH, flow rate, type and amount of eluent, breakthrough volume and interference of a large number of anions and cations on the recovery of the selected ions was studied. Under optimum conditions, the detection limits (3 s, n = 10) for analytes were 0.03 ng mL -1 (gold) and 0.01 ng mL -1 (manganese). The method was successfully applied for separation and determination of gold and manganese ions in water and standard samples.

Carrier element-free coprecipitation with 3-phenly-4-o-hydroxybenzylidenamino-4,5-dihydro-1,2,4-triazole-5-one for separation/preconcentration of Cr(III), Fe(III), Pb(II) and Zn(II) from aqueous solutions

Energy Technology Data Exchange (ETDEWEB)

Duran, Celal; Bulut, Volkan N.; Gundogdu, Ali; Ozdes, Duygu; Yildirim, Nuri [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey); Soylak, Mustafa, E-mail: soylak@erciyes.edu.tr [Department of Chemistry, Faculty of Arts and Sciences, Erciyes University, 38039 Kayseri (Turkey); Senturk, H. Basri [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey); Elci, Latif [Pamukkale University, Faculty of Arts and Sciences, Department of Chemistry, 20020 Denizli (Turkey)

2009-08-15

A separation/preconcentration procedure, based on the coprecipitation of Cr{sup 3+}, Fe{sup 3+}, Pb{sup 2+} and Zn{sup 2+} ions using a new organic coprecipitant, 3-phenly-4-o-hydroxybenzylidenamino-4,5-dihydro-1,2,4-triazole-5-one (POHBAT) without adding any carrier element has been developed. The method, thus, has been called carrier element-free coprecipitation (CEFC). The resultant concentrated elements were determined by flame atomic absorption spectrometric determinations. The influences of some analytical parameters including pH of the solution, amount of the coprecipitant, standing time, centrifugation rate and time, sample volume and diverse ions were investigated on the quantitative recoveries of analyte ions. The validation of the present preconcentration procedure was performed by the analysis of two certified reference materials. The recoveries of understudy analytes were found in the range of 93-98%, while the detection limits were calculated in the range of 0.3-2.0 {mu}g L{sup -1}. The precision of the method evaluated as relative standard deviation (R.S.D.), was in the range of 3-7% depend on the analytes. The proposed method was successfully applied to environmental samples for the determination of the analytes.

Carrier element-free coprecipitation with 3-phenly-4-o-hydroxybenzylidenamino-4,5-dihydro-1,2,4-triazole-5-one for separation/preconcentration of Cr(III), Fe(III), Pb(II) and Zn(II) from aqueous solutions

International Nuclear Information System (INIS)

Duran, Celal; Bulut, Volkan N.; Gundogdu, Ali; Ozdes, Duygu; Yildirim, Nuri; Soylak, Mustafa; Senturk, H. Basri; Elci, Latif

2009-01-01

A separation/preconcentration procedure, based on the coprecipitation of Cr 3+ , Fe 3+ , Pb 2+ and Zn 2+ ions using a new organic coprecipitant, 3-phenly-4-o-hydroxybenzylidenamino-4,5-dihydro-1,2,4-triazole-5-one (POHBAT) without adding any carrier element has been developed. The method, thus, has been called carrier element-free coprecipitation (CEFC). The resultant concentrated elements were determined by flame atomic absorption spectrometric determinations. The influences of some analytical parameters including pH of the solution, amount of the coprecipitant, standing time, centrifugation rate and time, sample volume and diverse ions were investigated on the quantitative recoveries of analyte ions. The validation of the present preconcentration procedure was performed by the analysis of two certified reference materials. The recoveries of understudy analytes were found in the range of 93-98%, while the detection limits were calculated in the range of 0.3-2.0 μg L -1 . The precision of the method evaluated as relative standard deviation (R.S.D.), was in the range of 3-7% depend on the analytes. The proposed method was successfully applied to environmental samples for the determination of the analytes.

Sorption and Preconcentration of Lead on Silica Nanoparticles Modified with Resacetophenone

Directory of Open Access Journals (Sweden)

Anupreet Kaur

2009-01-01

Full Text Available The silica-resacetophenone (SiO2-RATP nanoparticles were used as a new sorbent for extraction of trace amounts of Pb(II by batch technique. Conditions of the analysis such as preconcentration factor, effect of pH, sample volume, shaking time, elution conditions and effects of interfering ions for the recovery of analyte were investigated. The adsorption capacity of nanometer SiO2-RATP was found to be 167.24 µ mol/g at optimum pH and the detection limit (3σ was 0.58 µg/L. The adsorption equilibrium of Pb(II on nanometer SiO2-RATP was achieved in 20 min. Adsorbed Pb(II was easily eluted with 5 mL of 0.5 M hydrochloric acid. The maximum preconcentration factor was 60. The method was applied for the determination of trace amounts of Pb(II in various natural water rivers.

Possibilities for reorientation the activity of heavy water plants

International Nuclear Information System (INIS)

Pop, F.; Croitoru, C.; Titescu, Gh.; Stefanescu, I.; Hodor, I.; Cuna, S. . E-mail of corresponding author: pop.floarea@icsi.ro; Pop, F.)

2005-01-01

In Romania heavy water is produced by H 2 O-H 2 S chemical exchange (GS process) and by water distillation, simultaneously working two lines. The distillation plants have high separation capacity, a distillation line being able to concentrate water from two GS lines. The paper presents data regarding possibilities to use one distillation line for oxygen 18 production, as pre-concentrates or finite products. Using a simulation program it was calculated oxygen 18 concentration in heavy water produced, maximum 18 O concentration of pre-concentrate obtained on distillation line and the separation cascade dimensions for obtain 95% 18 O, with first and second stage having same dimensions like a distillation plant from Romanian heavy water factory. Oxygen-18 separation factor is much lower than deuterium separation factor. For this reason, oxygen-18 is a very expensive product. (author)

On-line separation of iodine species in reactor water using mixer-settlers

International Nuclear Information System (INIS)

Malmbeck, R.; Skarnemark, G.

1995-01-01

A method for separation of iodine species from water has been developed. It is based on liquid-liquid extraction and separation is achieved in four extraction steps. A system based on this method for continuous separation of iodine species using mixer-settlers has been developed. It consists of four mixer-settler batteries with 4,4,6 and 6 mixer-settler stages each. As organic phase an aliphatic kerosene is used and the separation is improved if the organic solvent has been pretreated with iodine carrier, stripped and washed. With an aqueous feed flowrate of 10 ml/min and mixer-settler battery phase flowratios of approximately 0.1 except for the elementary iodine strip battery with a phase flowratio of 1, the system separation performance is 92% for methyl iodide, 97% for iodate and elementary iodine and 99% for iodide. (orig.)

Separation and preconcentration of 2,3,7,8-tetrachlorodibenzo-p-dioxin in blood samples by inclusion emulsion membranes and its determination by gas chromatography.

Science.gov (United States)

Mokhtari, Bahram; Pourabdollah, Kobra

2012-10-15

The nano-mediated preconcentration of 2,3,7,8-tetrachlorodibenzo-p-dioxin from blood samples was reported by inclusion-facilitated emulsion liquid membrane process. The novelty of this study was application of nano-baskets of calixarene and emulsion liquid membranes in selective and efficient preconcentration of 2,3,7,8-tetrachlorodibenzo-p-dioxin. For this aim, four derivatives of p-tert-calix[4]arene bearing different sulfonamide moieties were synthesized and their inclusion-extraction parameters were optimized including calixarenes' scaffold and concentration (3, 4 wt%), diluent type in membrane, phase and treat ratios (0.8 and 0.3), mixing speed (300 rpm), and initial solute concentrations (0.1-10 pg g(-1)). The extraction efficiency was determined by dioxin's concentration using gas chromatography equipped with electron capture detector and the results revealed that in optimized operating conditions, the preconcentration of 2,3,7,8-tetrachlorodibenzo-p-dioxin was improved and the limit of detection decreased. Copyright © 2012 Elsevier B.V. All rights reserved.

Hyphenating multisyringe flow injection lab-on-valve analysis with atomic fluorescence spectrometry for on-line bead-injection preconcentration and determination of trace levels of hydride-forming elements in environmental samples

DEFF Research Database (Denmark)

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

2006-01-01

the determination of ultratrace level concentrations of total inorganic arsenic in freshwater. Employing quantitative preoxidation of As(III) to As(V) in the samples by means of permanganate, the method involves the preconcentration of arsenate at pH 10 on a renewable anion exchanger, namely Q-Sepharose, packed...

Detection of vegetation LUE based on chlorophyll fluorescence separation algorithm from Fraunhofer line

Science.gov (United States)

Liu, Liangyun; Zhang, Bing

2009-09-01

Photosynthetic efficiency is very important, and not yet generally assessable by remote sensing. Much research has proved the possibility of the separation of solar-induced chlorophyll fluorescence (ChlF) from the reflected hyperspectral data. As the 'probe' of plant photosynthesis, it is possible to detect photosynthetic light use efficiency (LUE) by the separated solar-induced ChlF. A diurnal experiment was carried out on winter wheat on Apr. 18, 2008, and the canopy radiance spectra and leaf LUE data were measured synchronously. The solar-induced chlorophyll fluorescence signals at 760nm and 688nm were separated from the reflected radiance spectral based on Fraunhofer lines in two oxygen absorption bands. The result showed that LUE was negatively correlated to the separated chlorophyll signals. The statistical models for LUE based on the solar-induced chlorophyll fluorescence values at 688 nm and 760 nm bands had correlation coefficients (R2) of 0.64 and 0.78, respectively. In addition, photochemical reflectance index (PRI) was also linked to LUE, and a statistical model for LUE based on PRI has a correlation coefficient (R2) of 0.66. The presented method provides a novel solution for monitoring LUE from remote sensing data.

Graphene oxide sheets immobilized polystyrene for column preconcentration and sensitive determination of lead by flame atomic absorption spectrometry.

Science.gov (United States)

Islam, Aminul; Ahmad, Hilal; Zaidi, Noushi; Kumar, Suneel

2014-08-13

A novel solid-phase extractant was synthesized by coupling graphene oxide (GO) on chloromethylated polystyrene through an ethylenediamine spacer unit to develop a column method for the preconcentration/separation of lead prior to its determination by flame atomic absorption spectrometry. It was characterized by Fourier transform infrared spectroscopy, far-infrared spectroscopy, thermogravimetric analysis/differential thermal analysis, scanning electron microscopy, energy-dispersive spectrometry, and transmission electron microscopy. The abundant oxygen-containing surface functional groups form a strong complex with lead, resulting in higher sorption capacity (227.92 mg g(-1)) than other nanosorbents used for sorption studies of the column method. Using the column procedure here is an alternative to the direct use of GO, which restricts irreversible aggregation of GO and its escape into the ecosystem, making it an environmentally sustainable method. The column method was optimized by varying experimental variables such as pH, flow rate for sorption/desorption, and elution condition and was observed to exhibit a high preconcentration factor (400) with a low preconcentration limit (2.5 ppb) and a high degree of tolerance for matrix ions. The accuracy of the proposed method was verified by determining the Pb content in the standard reference materials and by recovery experiments. The method showed good precision with a relative standard deviation <5%. The proposed method was successfully applied for the determination of lead in tap water, electroplating wastewater, river water, and food samples after preconcentration.

Preconcentrative separation of chromium(III) species from chromium(VI) by cloud point extraction and determination by flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Yildiz, Z.; Arslan, G.; Tor, A.

2011-01-01

We describe a high-throughput technique for the determination of chromium species in water samples by flame atomic absorption spectrometry (FAAS) after preconcentrative separation of Cr(III) species from Cr(VI) by cloud point extraction (CPE) using diethyldithiocarbamate (DDTC) as the chelating agent and the nonionic surfactant Triton X-100 as the extractant. The Cr(III)-DDTC complex is extracted if the temperature is higher than the CPE temperature of Triton X-100, while Cr(VI) remains in the aqueous phase. The Cr(III) in the surfactant phase was analyzed by FAAS, and the concentration of Cr(VI) was calculated by subtraction of Cr(III) from total chromium which was directly determined by FAAS. The effect of pH, concentration of chelating agent, surfactant, and equilibration temperature were investigated. The detection limit for Cr(III) was 0. 08 μg L -1 with an enrichment factor of 98, and the relative standard deviation was 1. 2% (n = 3, c = 100 μg L -1 ). A certified reference material and several water samples were analyzed with satisfactory results. (author)

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.

Preparation of 1-(2-pyridylazo)-2-naphthol functionalized benzophenone/naphthalene and their uses in solid phase extractive preconcentration/separation of uranium(VI)

International Nuclear Information System (INIS)

Preetha, C.R.; Prasada Rao, T.

2003-01-01

The preparation of solid reagent 1-(2-pyridylazo)-2-naphthol functionalized benzophenone/naphthalene for preconcentration/separation of uranium(VI) is described. These reagents enriches uranium(VI) quantitatively from dilute aqueous solutions in the pH range 10.5-11.0. The solid mixture consisting of the enriched metal ion along with solid phase extractant were dissolved in 2 ml of acetone and uranium(VI) content was established spectrophotometrically by using Arsenazo III procedure. Calibration graphs were rectilinear over the uranium(VI) concentration in the range 0.002-0.1 μg cm -3 . Five replicate determinations of 40 μg of uranium present in 1 dm 3 of sample solution gave a mean absorbance of 0.185 with a relative standard deviation of 1.4%. The detection limit (corresponding to 3 times the standard deviation of the blank) and the enrichment factor were found to be 2 μg dm -3 and 500 respectively. Further the possible separation of uranium(VI) from several bivalent, trivalent and tetravalent elements was also established. In addition to validating the developed method by successfully analysing marine sediment reference material (MESS-3), uranium content was established in soil, river and marine sediment samples by the developed method and compared with standard inductively coupled plasma mass spectrometry (ICP-MS) values. (orig.)

Preconcentration of Zn2+ and Cu2+ ions from food and vegetable samples using modified activated carbon.

Science.gov (United States)

Ghaedi, M; Tavallali, H; Montazerozohori, M; Zahedi, E; Amirineko, M; Khodadoust, S; Karimipour, G

2012-11-01

In this work, two N/S-containing chelating agents 2-(4-methoxybenzylideneamino)thiophenol (2-4-MBAT) and 2-(4-chlorobenzylideneamino) benzenethiol (2-4-CBABT) were synthesized as new sorbents and were used for preconcentration of Zn(2+) and Cu(2+) ions in food and vegetable samples. In the proposed procedure, the trace amount of Zn(2+) and Cu(2+) ions from 250 mL of sample solution at pH = 5.0 was preconcentrated by 1 g of activated carbon (AC) loaded with 15 mg of 2-4-MBAT and 2-4-CBABT separately. The breakthrough volumes (maximum sample volume that their metal ions quantitatively can be enriched) for solid-phase extraction (SPE) procedure based on the AC modified with 2-4-MBAT and 2-4-CBABT were 800 and 750 mL, respectively. The sorbed Zn(2+) and Cu(2+) ions were efficiently eluted by 8 mL of 4 mol L(-1) HNO(3) and preconcentration factor of 112.5 and 93.7 and experimental enhancement factor of 30 and 35 ions were obtained for Zn(2+) and Cu(2+), respectively. The application of this enrichment procedure allowed the extraction of trace metal ions with recoveries exceeding of 90%.

Rapid determination of environmental plutonium in large water samples by means of manganese dioxide Co-precipitation and extraction chromatographic separation

International Nuclear Information System (INIS)

Sidhu, R.S.; Hoff, P.

1999-01-01

Plutonium activity determinations in environmental water samples are routinely performed in many laboratories. Due to the low plutonium concentrations and the complexity of the plutonium aqueous chemistry, these analysis involve cumbersome preconcentration and separation procedures and long measurement times. We describe a procedure where MnO 2 (s) is used as scavenger to preconcentrate Pu prior to separation by the transuranium specific extraction chromatographic resin TRU-Resin. The ability of MnO 4 - /MnO 2 (s) to destroy organic matter and oxidise plutonium is combined with the specific behaviour of the TRU-resin for transuranium elements. The method facilitates a rapid preconcentration and separation of plutonium. With the use of this procedure, the laboratory work on one sample can be performed in one day with minimum attention. The overall yields from a 200 litre fresh- or seawater sample to a measurable Pu source are between 70-85%. (orig.)

Resonance ionization laser ion sources for on-line isotope separators (invited)

International Nuclear Information System (INIS)

Marsh, B. A.

2014-01-01

A Resonance Ionization Laser Ion Source (RILIS) is today considered an essential component of the majority of Isotope Separator On Line (ISOL) facilities; there are seven laser ion sources currently operational at ISOL facilities worldwide and several more are under development. The ionization mechanism is a highly element selective multi-step resonance photo-absorption process that requires a specifically tailored laser configuration for each chemical element. For some isotopes, isomer selective ionization may even be achieved by exploiting the differences in hyperfine structures of an atomic transition for different nuclear spin states. For many radioactive ion beam experiments, laser resonance ionization is the only means of achieving an acceptable level of beam purity without compromising isotope yield. Furthermore, by performing element selection at the location of the ion source, the propagation of unwanted radioactivity downstream of the target assembly is reduced. Whilst advances in laser technology have improved the performance and reliability of laser ion sources and broadened the range of suitable commercially available laser systems, many recent developments have focused rather on the laser/atom interaction region in the quest for increased selectivity and/or improved spectral resolution. Much of the progress in this area has been achieved by decoupling the laser ionization from competing ionization processes through the use of a laser/atom interaction region that is physically separated from the target chamber. A new application of gas catcher laser ion source technology promises to expand the capabilities of projectile fragmentation facilities through the conversion of otherwise discarded reaction fragments into high-purity low-energy ion beams. A summary of recent RILIS developments and the current status of laser ion sources worldwide is presented

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

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.

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.

Possibilities for reorientation of activity in Heavy Water Plants

International Nuclear Information System (INIS)

Pop, F.; Croitoru, C.; Titescu, Gh.; Stefanescu, I.; Hodor, I.; Cuna, S.

2004-01-01

In Romania heavy water is produced by H 2 O-H 2 S chemical exchange (GS process) and by water distillation, in two lines working simultaneously. The distillation plants have high separation capacity, a distillation line being able to concentrate water from two GS lines. The paper presents data regarding possibilities to use one distillation line for oxygen - 18 production, as pre-concentrates or finite products. A simulation program was used to calculate the oxygen - 18 concentration in the heavy water produced, maximum 18 O concentration of pre-concentrate obtained on distillation line and the separation cascade sizes to obtain 95% 18 O, with first and second stage having the same sizes like the distillation plant from the Romanian heavy water factory. Oxygen-18 separation factor is much lower than deuterium separation factor. For this reason, oxygen-18 is a very expensive product. (authors)

Chemical investigations of isotope separation on line target units for carbon and nitrogen beams

CERN Document Server

Franberg, H; Gäggeler, H W; Köster, U

2006-01-01

Radioactive ion beams (RIBs) are of significant interest in a number of applications. Isotope separation on line (ISOL) facilities provide RIB with high beam intensities and good beam quality. An atom that is produced within the ISOL target will first diffuse out from the target material. During the effusion towards the transfer line and into the ion source the many contacts with the surrounding surfaces may cause unacceptable delays in the transport and, hence, losses of the shorter-lived isotopes. We performed systematic chemical investigations of adsorption in a temperature and concentration regime relevant for ISOL targets and ion source units, with regard to CO/sub x/ and NOmaterials are potential construction materials for the above-mentioned areas. Off-line and on-line tests have been performed using a gas thermochromatography setup with radioactive tracers. The experiments were performed at the production of tracers for atmospheric chemistry (PROTRAC) facility at the Paul Schener Institute in Villigen...

The promise of nanotechnology for separation devices - from a top-down approach to nature-inspired separation devices

NARCIS (Netherlands)

Eijkel, Jan C.T.; van den Berg, Albert

An overview is given of the possible applications of nanotechnology to optimise existing separation methods and to enable new methods. Attention is paid to nanotechnological contributions in the fields of HPLC, CEC, sieves, Brownian ratchets and preconcentration units. A brief description is also

Preconcentration and Determination of Antimony in Drinking Water Bottled by Modified Nano-Alumina

Directory of Open Access Journals (Sweden)

M Mohammad Zakizade

2016-01-01

Full Text Available Abstract Introduction: Antimony trioxide (Sb2O3 has been utilized as a catalyst in polyethylene terephtalate (PET production, and the studies conducted on the bottled water has demonstrated that antimony can be leached from PET bottles into drinking water. Methods: In this study, a simple method was applied in order to determine the trace amount of antimony in bottled drinking water based on preconcentration /solid phase extraction. The nano alumina modified with Schiff base ligand was used in regard with Sb preconcentration. The experiments were performed in a continuous system and HCI was used as eluent of Sb ion. Several chemical and flow variables were optimized for a quantitative preconcentration and determination of Sb ion. The atomic absorption spectroscopy was used to determine Sb ion concentration. In order to study the keeping conditions on the leaching of Sb ion from PET plastic, drinking water bottles were kept in different conditions(room temperature, sunny light and -18˚C. Results: The calibration graph was linear in the range of 0.5 to 15.0 ppm Sb with detection limit of 0.055 ppm. The flow rate of sample was optimized in range of 1.0-9.0 mLmin-1 and Sb ion can be quantitatively eluted at 90 Vsample: Veluent retio. Conclusion: The study results revealed that the modified nano alumina is an effective sorbent in regard with absorbing Sb ion from water and HCI 1M can be used as an appropriate eluent. Maximum leaching of Sb ion is observed when the bottled drinking water was exposed to the sun light. Keywords: Antimony; Bottled drinking water; Modified alumina; Preconcentration

Separation of V(V)-4-(2-pyridylazo)resorcinolato complex from a large excess reagent using an ODS cartridge for high-performance liquid chromatography.

Science.gov (United States)

Takahashi, Toru; Kaneko, Emiko; Yotsuyanagi, Takao

2006-12-01

A selective off-line preconcentration technique for the V(V) complex with 4-(2-pyridylazo)resorcinol has been developed and successfully applied to the determination of V(V) in an air-borne sample. The target complex was separated from excess reagent using an ODS cartridge and water as the eluent. The complex was then concentrated on another ODS cartridge using tetrabutylammonium bromide and eluted with methanol; the eluate was applied to a one-drop concentration/HPLC. A detection limit as low as (6.05 +/- 0.82)x 10(-11) M (5 ppt) was achieved.

Preconcentration of low-grade uranium ores with environmentally acceptable tailings, part I

International Nuclear Information System (INIS)

Raicevic, D.; Raicevic, M.; McCarthy, D.R.

1979-08-01

The low-grade ore sample used for this investigation originated from Agnew Lake Mines Limited, Espanola, Ontario. It contained about 1% pyrite and 0.057% uranium, mainly as uranothorite with a small amount of brannerite. Both of these minerals occur in the quartz-sericite matrix of a conglomerate. A preconcentration process has been developed to give a high uranium recovery, reject pyrite, radium and thorium from the ore and produce environmentally acceptable tailings. This process applies flotation in combination with high intensity magnetic separation and gravity concentration

Metal Recovery and Preconcentration by Edta and Dtpa Modified Silica Surfaces

Directory of Open Access Journals (Sweden)

Eveliina Repo

2017-03-01

Full Text Available This study focuses on the adsorption and preconcentration of various metals by silica gel surfaces modified with aminopolycarboxylic acids namely ethylenediaminetetraacetic acid or diethylenetriamine-pentaacetic acid. The adsorption performance of the studied materials was determined in mixed metal solutions and the adsorption isotherm studies were conducted for cobalt, nickel, cadmium, and lead. The results were modeled using various theoretical isotherm equations, which suggested that two different adsorption sites were involved in metal removal although lead showed clearly different adsorption behavior attributed to its lowest hydration tendency. Efficient regeneration of the adsorbents and preconcentration of metals was conducted with nitric acid. Results indicated that the metals under study could be analyzed rather accurately after preconcentration from both pure, saline and ground water samples.

A congestion line flow control in deregulated power system

Directory of Open Access Journals (Sweden)

Venkatarajan Shanmuga Sundaram

2011-01-01

Full Text Available Under open access, market-driven transactions have become the new independent decision variables defining the behavior of the power system. The possibility of transmission lines getting over-loaded is relatively more under deregulated operation because different parts of the system are owned by separate companies and in part operated under varying service charges. This paper discusses a two-tier algorithm for correcting the lone overloads in conjunction with the conventional power-flow methods. The method uses line flow sensitivities, which are computed by the East Decoupled Power-flow algorithm and can be adapted for on-line implementation.

Preconcentration and determination of trace chromium using 1-(2-pyridylazo-2 -naphthol) immobilization on surfactant- coated alumina

International Nuclear Information System (INIS)

Shemirani, F.; Zamani, M

2002-01-01

Full text: Chromium is one of the essential elements for all vertebrates, as it appears to play a role in the metabolism of glucose and some lipids such as cholesterol. Since chromium is used widely in various industries, such as in the galvanization, steel, leather and paint industries, the resulting anthropogenic contamination of chromium is observed in the coastal sediments and seawater. Chromium in natural waters is normally present at low concentration levels, typically 0.3 - 1.0 μg/L in river water, and 0.1.5 μg/L in sea water. In many cases, the separation and preconcentration techniques are generally required to determined chromium at low concentration levels in natural waters, even when the most sensitive techniques, for instance electrothermal atomic absorption spectrometry and inductively coupled plasma-mass spectrometry (ICP - MS), are used. In the present work, the column of alumina modified with SDS and PAN was prepared in order to achieve a simple, low - cost and effective method for the improvement of the detection limit of ETAAS by preconcentration of chromium from a large volume of the aqueous through immobilization of PAN on surfactant coated alumina. The influence of P H, flow rate of sample solution and eluent, amount of eluent and effect of cationic interferences on percent recovery of chromium were studied. A concentration factor of 100 can be achieved by passing 500 ml of sample through the column. The method was applied to the determination of chromium in waste and mineral waters

The Monitor System for the LHCb on-line farm

CERN Document Server

Bonifazi, F; Carbone, A; Galli, D; Gregori, D; Marconi, U; Peco, G; Vagnoni, V

2005-01-01

The aim of the LHCb on-line farm Monitor System is to keep under control all the working indicators which are relevant for the farm operation, and to set the appropriate alarms whenever an error or a critical condition comes up. Since the most stressing tasks of the farm are the data transfer and processing, relevant indicators includes the CPU and the memory load of the system, the network interface and the TCP/IP stack parameters, the rates of the interrupts raised by the network interface card and the detailed status of the running processes. The monitoring of computers’ physical conditions (temperatures, fan speeds and motherboard voltages) are the subject of a separate technical note, since they are accessed in a different way, by using the IPMI protocol.

Determination of gold in natural waters by neutron activation-#betta#-spectrometry after preconcentration on activated charcoal

International Nuclear Information System (INIS)

Hamilton, T.W.; Ellis, J.; Florence, T.M.

1983-01-01

A method for the determination of gold at very low levels in waters is presented. The method involves batchwise pre-concentration of gold from 1 l of water at pH 3-4 onto 0.1 g of activated charcoal by shaking for 5 min and subsequent treatment of the activated charcoal by instrumental neutron activation-#betta#-spectrometry. Activated charcoal quantitatively adsorbs ionic and colloidal gold from solutions prepared with distilled water and also from natural surface waters spiked and equilibrated with these two forms of gold. Three ion-exchange resins were evaluated for pre-concentration purposes; ionic gold removal was quantitative but colloidal gold removal was incomplete. Electrodeposition at a carbon fibre electrode gave similar results. The charcoal pre-concentration technique was tested on solutions containing 198 Au tracer and a total gold concentration of 1 μg l - 1 . The limit of detection of total gold (ionic and colloidal) for the carbon adsorption/neutron activation-#betta#-spectrometry procedure is 0.3 ng l - 1 . The method was used to determine gold in surface waters from auriferous regions. (Auth.)

Filterless preconcentration, flow injection analysis and detection by inductively-coupled plasma mass spectrometry

DEFF Research Database (Denmark)

Andersen, Jens Enevold Thaulov

The influence of interferences in the analysis of elements by inductively-coupled-plasma mass-spectrometry (ICP-MS) may be significantly diminished by utilising a protocol of flow-injection analysis (FIA). The method is based on filterless preconcentration of metallic elements at the walls...... of a knotted reactor that was made of nylon tubings. In the load mode, the preconcentration was accomplished by precipitation of metallic species in alkaline-buffered carriers onto the inner walls of the hydrofilic tube. After a preconcen-tration period of 40-120 seconds using sample volumes of 4-10 m...... of 10-30 were obtained in the analysis of aluminium, of chromium and of iron, which resulted in detection limits (3) down to 20 g/L at a sampling frequency of 50 per hour. The preconcentration protocol improves the selectivity thus allowing direct determination of the elements in saline media. Anionic...

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.

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)

Trace determination of antimony by hydride generation atomic absorption spectrometry with analyte preconcentration/atomization in a dielectric barrier discharge atomizer

Czech Academy of Sciences Publication Activity Database

Zurynková, Pavla; Dědina, Jiří; Kratzer, Jan

2018-01-01

Roč. 1010, JUN (2018), s. 11-19 ISSN 0003-2670 R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : dielectric barrier discharge * Stibane * atomization and preconcentration Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 4.950, year: 2016

Application of liquid column chromatography to preconcentration, separation and determination of platinum metals

International Nuclear Information System (INIS)

Alimarin, I.P.; Basova, E.M.; Bol'shova, T.A.; Ivanov, V.M.

1986-01-01

Separation and determination of platimum metals using the methods of adsorption, ion-pair, ion-exchange, distributing and sieve chromatography are discussed in the review of literature in 1971-1984. Separation and determination of metals as chelates using the method of adsorption and ion-pair chromatograpy are noted to be most perspective directions of developing highly effective liquid chromatography of inorganic systems

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

Science.gov (United States)

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

2013-12-04

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

Separation and preconcentration trace amounts of gold by using modified organo nanoclay closite 15A

Directory of Open Access Journals (Sweden)

Sayed Zia Mohammadi

2010-01-01

Full Text Available The application of organo nanoclay 5-(4-dimethylamino-benzylidene rhodanine-immobilized as a new, easily prepared, and stable solid sorbent for preconcentration trace amounts of Au(III ions in aqueous solution is presented. The sorption of Au(III ions was quantitative in the pH range of 2-4, and quantitative desorption occurred instantaneously with 10.0 mL of a mixture containing 0.5 mol L-1 Na2S2O3 and KSCN. Various parameters, such as the effect of pH, breakthrough volume, extraction time, and interference of a large number of anions and cations have been studied. The proposed method has been applied for determination of trace amount of gold in water samples.

Determination of chromium in water samples by neutron activation analysis after preconcentration on activated carbon

Energy Technology Data Exchange (ETDEWEB)

van der Sloot, H A [Stichting Reactor Centrum Nederland, Petten

1977-01-01

A method is presented for the determination of chromium in sea- and fresh water. Chromium is concentrated on activated carbon from a neutral solution after a previous reduction of chromate with sodium sulfite at pH 1.5. The adsorption conditions, acidity, concentrations, amount of carbon, stirring-time, sample-volume, salinity, the influence of storage on the ratio of tervalent to hexavalent chromium, were investigated. The final determination of the total chromium content is performed by instrumental neutron-activation analysis. By preconcentration on activated carbon, a differentiation between tervalent and hexavalent chromium is possible. A separate determination of both species is not yet feasible due to the high carbon blank and to the necessity of measuring the adsorption percentage on carbon. The lower limit of determination, which depends on the value of the carbon blank, is 0.05 ..mu..g Cr/l with a precision of 20%. The determination is hampered by the considerable blank from the carbon. The use of activated carbon prepared from recrystallized sugar will probably improve the lower limit of determination and possibly allow the determination of chromate.

Determination of rare earth elements in seawater by inductively coupled plasma mass spectrometry with off-line column preconcentration using 2,6-diacetylpyridine functionalized Amberlite XAD-4

Energy Technology Data Exchange (ETDEWEB)

Karadas, Cennet [Department of Chemistry, Art and Science Faculty, Balikesir University, 10100 Balikesir (Turkey); Kara, Derya, E-mail: dkara@balikesir.edu.tr [Department of Chemistry, Art and Science Faculty, Balikesir University, 10100 Balikesir (Turkey); Fisher, Andrew [School of Geography, Earth and Environmental Sciences, University of Plymouth, Drake Circus, Plymouth, Devon PL4 8AA (United Kingdom)

2011-03-18

An off-line column preconcentration technique using a micro-column of 2,6 diacetylpyridine functionalized Amberlite XAD-4 with inductively coupled plasma mass spectrometry (ICP-MS) as a means of detection has been developed. The aim of the method was to determine rare earth elements (REEs) (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu) in seawater. Sample solutions (2-10 mL) were passed through the column which was then washed with ultra-pure water to remove residual matrix. The adsorbed cations on the resin were eluted by using 2 mL of 0.1 mol L{sup -1} HNO{sub 3} containing 10 ng mL{sup -1} indium as an internal standard. The eluent was analyzed for the metal concentrations using ICP-MS. Sample pH as well as the sample and eluent flow rates were optimized. The sorption capacity of resin was determined by the batch process, by equilibrating 0.05 g of the resin with solutions of 50 mL of 25 mg L{sup -1} of individual metal ions for 4 h at pH 6.0 at 26 deg. C. The sorption capacities for the resin were found to range between 47.3 {mu}mol g{sup -1} (for Lu) and 136.7 {mu}mol g{sup -1} (for Gd). Limits of detection (3{sigma}), without any preconcentration, ranged from 2 ng L{sup -1} to 10.3 ng L{sup -1} (for Tm and Lu respectively). The proposed method was applied to the determination of REEs in seawater and tap water samples.

Application and recovery of ionic liquids in the preparative separation of four flavonoids from Rhodiola rosea by on-line three-dimensional liquid chromatography.

Science.gov (United States)

Ma, Shufeng; Hu, Liming; Ma, Chaoyang; Lv, Wenping; Wang, Hongxin

2014-09-01

A novel on-line three-dimensional liquid chromatography method was developed to separate four main flavonoids from Rhodiola rosea. Ethyl acetate/0.5 mol/L ionic liquid 1-butyl-3-methylimidazolium chloride aqueous solution was selected as the solvent system. In the first-dimension separation, the target flavonoids were entrapped and subsequently desorbed into the second-dimension high-speed countercurrent chromatographic column for separation. In the third-dimension chromatography, the residual ionic liquid in the four separated flavonoids was removed and the used ionic liquid was recovered. As a result, 35.1 mg of compound 1, 20.4 mg of compound 2, 8.5 mg of compound 3, and 10.6 mg of compound 4 were obtained from 1.53 g R. rosea extract. They were identified as rhodiosin, rhodionin, herbacetin, and kaempferol, respectively. The recovery of ionic liquid reached 99.1% of the initial amount. The results showed that this method is a powerful technology for the separation of R. rosea flavonoids and that the ionic-liquid-based solvent system has advantages over traditional solvent systems in renewable and environmentally friendly properties. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Determination of trace lead and cadmium in transgenic rice by crosslinked carboxymethyl konjac glucomannan microcolumn preconcentration combined with graphite furnace atomic absorption spectrometry].

Science.gov (United States)

Liu, Hua-qing; Li, Sheng-qing; Qu, Yang; Chen, Hao

2012-02-01

A novel method was developed for the determination of trace lead and cadmium in transgenic brown rice based on separation and preconcentration with a micro column packed with crosslinked carboxymethyl konjac glucomannan (CCMKGM) prior to its determination by graphite furnace atomic absorption spectrometry. Variables affecting the separation and preconcentration of lead and cadmium, such as the acidity of the aqueous solution, sample flow rate and volume, and eluent concentration and volume, were optimized. Under optimized condition, detection limits of the method for the determination of trace lead and cadmium in transgenic brown rice were 0.11 and 0.002 microg x L(-1), respectively. The obtained results of lead and cadmium in the certified reference material (GBW10010, GBS1-1) were in good agreement with the certified values. The recoveries were in the range of 90%-103% and 93%-105% for detection of Pb and Cd in transgenic brown rice and the wild-type brown rice samples respectively. This study could provide technical support for determination of trace Pb and Cd in transgenic rice.

New on-line separation workflow of microbial metabolites via hyphenation of analytical and preparative comprehensive two-dimensional liquid chromatography.

Science.gov (United States)

Yan, Xia; Wang, Li-Juan; Wu, Zhen; Wu, Yun-Long; Liu, Xiu-Xiu; Chang, Fang-Rong; Fang, Mei-Juan; Qiu, Ying-Kun

2016-10-15

Microbial metabolites represent an important source of bioactive natural products, but always exhibit diverse of chemical structures or complicated chemical composition with low active ingredients content. Traditional separation methods rely mainly on off-line combination of open-column chromatography and preparative high performance liquid chromatography (HPLC). However, the multi-step and prolonged separation procedure might lead to exposure to oxygen and structural transformation of metabolites. In the present work, a new two-dimensional separation workflow for fast isolation and analysis of microbial metabolites from Chaetomium globosum SNSHI-5, a cytotoxic fungus derived from extreme environment. The advantage of this analytical comprehensive two-dimensional liquid chromatography (2D-LC) lies on its ability to analyze the composition of the metabolites, and to optimize the separation conditions for the preparative 2D-LC. Furthermore, gram scale preparative 2D-LC separation of the crude fungus extract could be performed on a medium-pressure liquid chromatograph×preparative high-performance liquid chromatography system, under the optimized condition. Interestingly, 12 cytochalasan derivatives, including two new compounds named cytoglobosin Ab (3) and isochaetoglobosin Db (8), were successfully obtained with high purity in a short period of time. The structures of the isolated metabolites were comprehensively characterized by HR ESI-MS and NMR. To be highlighted, this is the first report on the combination of analytical and preparative 2D-LC for the separation of microbial metabolites. The new workflow exhibited apparent advantages in separation efficiency and sample treatment capacity compared with conventional methods. Copyright © 2016 Elsevier B.V. All rights reserved.

Combined cation-exchange and solid phase extraction for the selective separation and preconcentration of zinc, copper, cadmium, mercury and cobalt among others using azo-dye functionalized resin.

Science.gov (United States)

Chatterjee, Mousumi; Srivastava, Bhavya; Barman, Milan K; Mandal, Bhabatosh

2016-04-01

A facile synthesis of an ion exchange material (FSG-PAN) has been achieved by functionalizing silica gel with an azo-dye. Its composition and structure are well assessed by systematic analysis. Extractor possesses high BET surface area (617.794m(2)g(-1)), exchange capacity and break-through capacity (BTC) (Q0 Zn(II): 225; Cd(II): 918; Hg(II): 384, Cu(II): 269 and Co(II): 388μMg(-1)). The sorption process was endothermic (+ΔH), entropy-gaining (+ΔS) and spontaneous (-ΔG) in nature. Preconcentration factor has been optimized at 172(Zn(II)); 157.2(Cd(II)); 193.6(Hg(II)); 176(Cu(II)); 172.4(Co(II)). Density functional theory calculation has been performed to analyze the sorption pathway. BTC (μMg(-1)) of FSG-PAN was found to be the product of its frontier orbitals and state of sorbed metal ion species, x (at x=1, mononuclear and x>1, a polynuclear species; i.e., BTC=[amount of HOMO]×x). FSG-PAN is used for the selective separation and preconcentration of Zn(II), Cd(II), Hg(II), Cu(II),Co(II) from large volume sample (800mL) of low concentration (0.017-0.40mML(-1)) in presence of foreign ions (50-300mML(-1)) at optimum conditions (pH: 7.0±1.5, flow rate: 2.5mLmin(-1), temperature: 27°C, equilibration-time: 5min). The method was found to be effective for real samples also. Copyright © 2016 Elsevier B.V. All rights reserved.

A chemically selective laser ion source for the on-line isotope separation

International Nuclear Information System (INIS)

Scheerer, F.

1993-03-01

In this thesis a laser ion source is presented. In a hot chamber the atoms of the elements to be studied are resonantly by light of pulsed dye lasers, which are pumped by pulsed copper-vapor lasers with extremely high pulse repetition rate (ν rep ∼ 10 kHz), stepwise excited and ionized. By the storage of the atoms in a hot chamber and the high pulse repetition rate of the copper-vapor lasers beyond the required high efficiency (ε ∼ 10%) can be reached. First preparing measurements were performed at the off-line separator at CERN with the rare earth elements ytterbium and thulium. Starting from the results of these measurements further tests of the laser ion source were performed at the on-line separator with in a thick tantalum target produced neutron-deficient ytterbium isotopes. Under application of a time-of-flight mass spectrometer in Mainz an efficient excitation scheme on the resonance ionization of tin was found. This excitation scheme is condition for an experiment at the GSI for the production of the extremely neutron-deficient, short-lived nucleus 102 Sn. In the summer 1993 is as first application of the newly developed laser ion source at the PSB-ISOLDE at CERN an astrophysically relevant experiment for the nuclear spectroscopy of the neutron-rich silver isotopes 124-129 Ag is planned. This experiment can because of the lacking selectivity of conventional ion sources only be performed by means of the here presented laser ion source. The laser ion source shall at the PSB-ISOLDE 1993 also be applied for the selective ionization of manganese. (orig./HSI) [de

Initial results with the Berkeley on-line mass separator-RAMA

International Nuclear Information System (INIS)

Cerny, J.; Moltz, D.M.; Evans, H.C.; Vieira, D.J.; Parry, R.F.; Wouters, J.M.; Gough, R.A.; Zisman, M.S.

1977-11-01

Initial performance is described for a reasonably fast and universal (having little or no chemical selectivity) on-line mass analysis system used to expand capabilities in studying nuclei far from stability. The system is termed RAMA, an acronym for Recoil Atom Mass Analyzer. Basically, this system utilizes the helium-jet method to transport activity to a Sidenius hollow-cathode ion source which is coupled to a mass spectrometer. Initial experiments and planned improvements are discussed. Transport efficiencies of between 10 and 60 percent have routinely been achieved, though the latter is much more typical when conditions are optimized

Simultaneous preconcentration of cadmium and lead in water samples with silica gel and determination by flame atomic absorption spectrometry.

Science.gov (United States)

Xu, Hongbo; Wu, Yun; Wang, Jian; Shang, Xuewei; Jiang, Xiaojun

2013-12-01

A new method that utilizes pretreated silica gel as an adsorbent has been developed for simultaneous preconcentration of trace Cd(II) and Pb(II) prior to the measurement by flame atomic absorption spectrometry. The effects of pH, the shaking time, the elution condition and the coexisting ions on the separation/preconcentration conditions of analytes were investigated. Under optimized conditions, the static adsorption capacity of Cd(II) and Pb(II) were 45.5 and 27.1mg/g, the relative standard deviations were 3.2% and 1.7% (for n = 11), and the limits of detection obtained were 4.25 and 0.60 ng/mL, respectively. The method was validated by analyzing the certified reference materials GBW 07304a (stream sediment) and successfully applied to the analysis of various treated wastewater samples with satisfactory results. Copyright © 2013 The Research Centre for Eco-Environmental Sciences, Chinese Academy of Sciences. Published by Elsevier B.V. All rights reserved.

Effect of temperature gradient on liquid-liquid phase separation in a polyolefin blend.

Science.gov (United States)

Jiang, Hua; Dou, Nannan; Fan, Guoqiang; Yang, Zhaohui; Zhang, Xiaohua

2013-09-28

We have investigated experimentally the structure formation processes during phase separation via spinodal decomposition above and below the spinodal line in a binary polymer blend system exposed to in-plane stationary thermal gradients using phase contrast optical microscopy and temperature gradient hot stage. Below the spinodal line there is a coupling of concentration fluctuations and thermal gradient imposed by the temperature gradient hot stage. Also under the thermal gradient annealing phase-separated domains grow faster compared with the system under homogeneous temperature annealing on a zero-gradient or a conventional hot stage. We suggest that the in-plane thermal gradient accelerates phase separation through the enhancement in concentration fluctuations in the early and intermediate stages of spinodal decomposition. In a thermal gradient field, the strength of concentration fluctuation close to the critical point (above the spinodal line) is strong enough to induce phase separation even in one-phase regime of the phase diagram. In the presence of a temperature gradient the equilibrium phase diagrams are no longer valid, and the systems with an upper critical solution temperature can be quenched into phase separation by applying the stationary temperature gradient. The in-plane temperature gradient drives enhanced concentration fluctuations in a binary polymer blend system above and below the spinodal line.

Selective solid phase extraction for separation and preconcentration of palladium from Gold Ore and anode slime after complexation with a N{sub 4}O{sub 2} mixed donor ligand derivative

Energy Technology Data Exchange (ETDEWEB)

Bulut, Volkan Numan [Macka Vocational School, Karadeniz Technical University, Macka/ Trabzon (Turkey); Tufekci, Mehmet; Duran, Celal; Kantekin, Halit [Faculty of Arts and Sciences, Department of Chemistry, Karadeniz Technical University, Trabzon (Turkey); Soylak, Mustafa [Faculty of Science, Department of Chemistry, Erciyes University, Kayseri (Turkey)

2010-07-15

A selective and sensitive method for the preconcentration, separation, and determination of palladium with flame atomic absorption spectrometry using 4,15-bis[(4-methylphenyl)sulfonyl]-20,21-dinitro-2,3,4,5,6,7,9,10,12,13,14,15,16,17-tetradecahydro-8,11-ethano-1,18,4,8,11,15-benzodioxa tetraaza cycloicosine (TNACIN) on XAD-2010 was developed. TNACIN-Pd(II) complex formed acidic aqueous solution (0.075-0.100 M HNO{sub 3}) was accumulated on XAD-2010 and then eluted with 1 M HCl in acetone. The effects of some analytical parameters including pH, TNACIN amount, sample volume, eluent type, and concentration, sample flow rate and matrix ions were studied for optimization of the method. Detection limit and precision were calculated for Pd(II). This method was also verified with CRM and internal standard, and satisfactory results were obtained. (Abstract Copyright [2010], Wiley Periodicals, Inc.)

Comparison of different filtration techniques for the pre-concentration of natural colloidal dispersions for field-flow-fractionation (FFF); Vergleich verschiedener Filtrationstechniken zur Aufkonzentrierung natuerlicher kolloidaler Dispersionen fuer die Feld-Fluss-Fraktionierung (FFF)

Energy Technology Data Exchange (ETDEWEB)

Saal, C.; Kammer, F. v.d. [Technische Univ. Hamburg-Harburg, Arbeitsbereich Umweltschutztechnik, Hamburg (Germany)

2002-07-01

The objektive of this study was to compare different pre-treatment techniques (active and passive filtration techniques applying various membranes) for field-flow-fractionation (FFF) analysis of natural aquatic colloids. In most cases FFF of natural water samples requires a pre-concentration step prior to analysis. The used FFF-method with online multi-detector-analysis (MDA) is a versatile method to specify the size distribution of particles (> 10 nm) in aqueous systems. Coupling FFF with trace element analysis (e. g. ICP-MS or total reflextion X-ray fluorescence (TXRF)) is a possibility for the determination of element/ size distributions. Analysing natural water samples with FFF a sample pre-treatment is needed in most cases, which can be a coarse filtration (> 5 {mu}m) to separate algea from the sample and a preconcentration of the colloidal fraction. The pre-treatment of the sample has to assure a minimum loss of colloidal particulate matter (CPM) and no change of size distribution. The different pre-concentration techniques were tested with water extractable soil colloids. We have developed methods with concentration factors F < 50 showing minor effects on the colloidal composition of the sample, so that these methods can be used to concentrate CPM of natural waters for size- and trace metal analysis. (orig.)

Preconcentration of low grade uranium ores by gravity and magnetic methods: a case study with copper tailings from Singhbhum, Bihar, India

International Nuclear Information System (INIS)

Natarajan, R.; Sreenivas, T.; Krishna Rao, N.

1992-01-01

The physical beneficiation methods applied to uranium ores are gravity and magnetic techniques. Feasibility of application of these two techniques has been industrially demonstrated in the case of Palabora copper-uranium ores and Witwatersrand gold-uranium ores respectively. In India exhaustive studies have been carried out on the application of gravity and magnetic methods for preconcentration of uranium values from tailings of copper plants at Surda, Rakha and Mosabani in Singhbhum. While recovery by shaking tables is poor owing to non-liberation and inefficient recovery in finer particle sizes (-37μm), gravity machines like Bartles Mozely Separator and Bartles Cross Belt Concentrator are able to give improved recovery in sizes down to about 15μm. Application of Wet High Intensity Magnetic Separator (WHIMS) is able to improve the recovery to about 75 to 85% from the three tailings, and the improvement is due to the ability of WHIMS collect the micaceous mineral particles containing composite uranium values, as well as uraninite particles down to about 10μm in size. WHIMS is inefficient in recovering uraninite particles below 5μm. High Gradient Magnetic Separator and Super Conducting High Gradient Magnetic Separator, on the other hand, are able to give enhanced recovery of even < 5μm uraninite particles. With the improved technology of gravity and magnetic methods now available, it should now be techno-economically feasible to employ preconcentration of low tenor uranium ores by physical beneficiation, prior to chemical processing. (author). 25 refs. 8 figs, 5 tabs

Zincon-modified activated carbon for solid-phase extraction and preconcentration of trace lead and chromium from environmental samples.

Science.gov (United States)

Li, Zhenhua; Chang, Xijun; Hu, Zheng; Huang, Xinping; Zou, Xiaojun; Wu, Qiong; Nie, Rong

2009-07-15

A new method that utilizes zincon-modified activated carbon (AC-ZCN) as a solid-phase extractant has been developed for simultaneous preconcentration of trace Cr(III) and Pb(II) prior to the measurement by inductively coupled plasma optical emission spectrometry (ICP-OES). The separation/preconcentration conditions of analytes were investigated, including effects of pH, the shaking time, the sample flow rate and volume, the elution condition and the interfering ions. At pH 4, the maximum adsorption capacity of Cr(III) and Pb(II) onto the AC-ZCN were 17.9 and 26.7 mg g(-1), respectively. The adsorbed metal ions were quantitatively eluted by 1 mL of 0.1 mol L(-1) HCl. Common coexisting ions did not interfere with the separation. According to the definition of IUPAC, the detection limits (3 sigma) of this method for Cr(III) and Pb(II) were 0.91 and 0.65 ng mL(-1), respectively. The relative standard deviation under optimum condition is less than 3.5% (n=8). The method has been applied for the determination of Cr(III) and Pb(II) in biological materials and water samples with satisfactory results.

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

Separation of uranyl ion using polyaniline

International Nuclear Information System (INIS)

Jayshree Ramkumar; Chandramouleeswaran, S.

2013-01-01

Polyaniline (Pani) was synthesized by the chemical oxidation of aniline. The use of persulphate instead of dichromate was desired in order to avoid the incorporation of chromium in the polymer matrix. The presence of chromium in the matrix, when dichromate was used as an oxidant, was confirmed by various techniques. The batch mode experiments showed that Pani could be used for separation of different metal ions. These ions were converted into their anionic complexes using suitable complexing agents. It was found that EDTA was used as a suitable reagent for the separation of Cu 2+ from Zn 2+ whereas the uranyl ion uptake could be increased to about 95 % when carbonate was used instead of EDTA as complexing agent. A possible application of the above exchange system to preconcentration of uranyl ion from seawater has also been examined. (author)

On-line Monitoring System for Power Transformers

Directory of Open Access Journals (Sweden)

Alexandru HOTEA

2016-12-01

Full Text Available Power transformers are the most important and expensive equipment from the electricity transmission system, so it is very important to know the real state of health of such equipment in every moment. De-energizing the power transformer accidentally due to internal defects can generate high costs. Annual maintenance proved to be ineffective in many cases to determine the internal condition of the equipment degradation due to faults rapidly evolving. An On-line Monitoring System for Power Transformers help real-time condition assessment and to detect errors early enough to take action to eliminate or minimize them. After abnormality detected, it is still important to perform full diagnostic tests to determine the exact condition of the equipment. On-line monitoring systems can help increase the level of availability and reliability of power transformers and lower costs of accidental interruption. This paper presents cases studies on several power transformers equipped with on-line monitoring systems from Transelectrica substation.

Determination of Hg(2+) by on-line separation and pre-concentration with atmospheric-pressure solution-cathode glow discharge atomic emission spectrometry.

Science.gov (United States)

Li, Qing; Zhang, Zhen; Wang, Zheng

2014-10-03

A simple and sensitive method to determine Hg(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(2+) elution conditions, namely, an FI flow rate of 2.0 mL min(-1) and an eluent comprised of 10% thiourea in 0.2 mol L(-1) HNO3. The detection limit of FI-SCGD-AES was determined to be 0.75 μg L(-1), and the precision of the 11 replicate Hg(2+) measurements was 0.86% at a concentration of 100 μg L(-1). The proposed method was validated by determining Hg(2+) in certified reference materials such as human hair (GBW09101b) and stream sediment (GBW07310). Copyright © 2014. Published by Elsevier B.V.

PRE-CONCENTRATION AND DETERMINATION OF HEAVY METALS ON MODIFIED ACTIVATED CARBON IN REAL SAMPLES

Directory of Open Access Journals (Sweden)

F. Ahmadi

2010-06-01

Full Text Available A sensitive and simple method for the simultaneous pre-concentration of nutritionally important minerals in real samples has been reported. The method is based on the formation of metal complexes by N, N'-diacetyl-4-bromo-2, 6-di (aminomethyl phenol (DBDP loaded on activated carbon. The metals content on the complexes are then eluted using 6mL 4M HNO3, which are detected by AAS at resonance line. In this procedure, minerals such as Ni, Cu, Co, Pb Zn and Cd can be analyzed in one run by caring out the simultaneous separation and quantification of them. At optimum condition the response are linear over concentration range of for 0.03-1.1 µg mL-1 for Ni2+ , 0.03-1.0 µg mL-1 for Cu2+, 0.02-1.0 µg mL-1 for  Pb2+ , 0.02-1.0 µg mL-1 for  Co2+,0.02-1.1 µg mL-1 Zn2+ and 0.05-1.3 µg mL-1for Cd2+. The detection limits of each element are expressed as the amount of analytes in µg mL-1 giving a signal to noise ratio of 3 are equal to 2.5, 2.4, 1.6, 2.4, 1.9 and 2.1 for Ni2+ , Cu2+, Pb2+ , Co2+,Zn2+ and Cd2+. The ability of method for repeatable recovery of trace ion are 99.9, 98.7, 99.2 , 98.7, 98.5and 95.6 with R.S.D of 1.3, 1.4, 1.2, 1.4, 1.7 and 1.4 for Ni2+ , Cu2+, Pb2+ , Co2+,Zn2+ and Cd2+. The method has been successfully applied for these metals content evaluation in some real samples including natural water and vegetable.     Keywords: Heavy Metals, N, N'-diacetyl-4-bromo-2,6-di(aminomethyl phenol (DBDP, Activated Carbon

Studies on neutron activation analysis using ion exchange preconcentration Pt. 6

International Nuclear Information System (INIS)

Hirose, A.; Ishii, D.

1978-01-01

Three convenient procedures are described for applying anion exchange resins to the preconcentration and irradiation support in neutron activation analysis. For each procedure the amounts of interferences were determined. The effect of the form, cross-linkage, pore size, and particle size of the resins on the elimination of interferences was investigated. Some other associated problems are also presented, viz. effect of concentration and temperature of washing solution, effect of irradiation time, and comparison with filter paper. Tabulated data are presented. (author)

Nano magnetic solid phase extraction for preconcentration of lead ions in environmental samples by a newly synthesized reagent.

Science.gov (United States)

Golshekan, Mostafa; Shariati, Shahab

2013-01-01

In this study, magnetite nanoparticles with particle size lower than 47 nm were synthesized and were applied for preconcentration of Pb2+ ions from aqueous solutions. To preconcentrate the Pb2+ ions, the surface of the synthesized nano particles was modified with sodium dodecyl sulfate (SDS) as an anionic surfactant. A new chelating agent (2-((E)-2-amino-4,5-dinitrophenylimino)methyl)phenol) was synthesized and used to form a very stable complex with Pb2+ ions. The lead ions formed complexes and were quantitatively extracted with SDS-coated magnetite nanoparticles. After magnetic separation of adsorbent, the adsorbent was eluted with 0.5% (v/v) HC1 in dimethyl sulfoxide (DMSO) prior to analysis by flame atomic absorption spectrometry (FAAS). Orthogonal array design (OAD) was used to study and optimize the different experimental parameters. Under the optimum conditions, enhancement factor up to 63.5 was achieved for extraction from only 10 mL of sample solution and the relative standard deviation (RSD %) of the method was lower than 2.8%. The obtained calibration curve was linear in the range of 1-300 pg L-' with reasonable linearity (r2 > 0.998). The limit of detection (LOD) based on S/N = 3 was 0.04 microg L(-1) for 10 mL sample volumes. Finally, applicability of the proposed method was successfully confirmed by preconcentration and determination of trace amounts of lead ions in environmental samples and satisfactory results were obtained.

Preconcentration, determination and speciation of iron by solid-phase extraction using dimethyl (E)-2-[(Z)-1-acetyl)-2-hydroxy-1-propenyl]-2-butenedioate

Energy Technology Data Exchange (ETDEWEB)

Khayatian, Gholamreza; Hassanpoor, Shahed; Nasiri, Farough; Zolali, Amin [Chemistry Department, Faculty of Science, University of Kurdistan, Sanandaj (Iran, Islamic Republic of)

2012-07-01

A new sensitive and selective procedure for speciation of trace dissolved Fe(III) and Fe(II), using modified octadecyl silica membrane disks and determination by flame atomic absorption spectrometry was developed. A ML{sub 3} complex is formed between the ligand and Fe(III) responsible for extraction of metal ion on the disk. Various factors influencing the separation of iron were investigated and the optimized operation conditions were established. Under optimum conditions, an enrichment factor of 166 was obtained for Fe{sup 3+}ions. The calibration graph using the preconcentration system for Fe{sup 3+} was linear between 40.0 and 1000.0 {sup m}u{sup g} L{sup -1}. (author)

Preconcentration of Co, Ni, Cd and Zn on naphthalene–2,4,6-trimorpholino-1,3,5-triazin adsorbent and flame atomic absorption determination

Directory of Open Access Journals (Sweden)

TAYYEBEH MADRAKIAN

2010-05-01

Full Text Available A preconcentration method was developed for the determination of trace amounts of Co, Ni, Cd and Zn by atomic absorption spectrometry. The method is based on the retention of the metal cations by naphthalene–2,4,6-trimorpholino-1,3,5-triazin adsorbent in a column. The adsorbed metals were then eluted from the column with hydrochloric acid and the Co, Ni, Cd and Zn were determined by flame atomic absorption spectrometry. The optimal extraction and elution conditions were studied. The effects of diverse ions on the preconcentration were also investigated. A preconcentration factor of 250 for Co(II, Ni(II and Zn(II, and 400 for Cd(II can easily be achieved. Calibration graphs were obtained and the detection limits of the method for Co(II, Ni(II, Cd(II and Zn(II were 0.51, 0.49, 0.17 and 0.10 ng mL-1, respectively. The relative standard deviations (RSD of 0.37–2.31 % for Co, 0.37–3.73 % for Ni, 2.20–2.40 % for Cd and 1.50–2.56 % for Zn were obtained. The method was also used for the simultaneous preconcentration of these elements and the method was successfully applied to their preconcentration and determination. The method was applied to the determination of Co, Ni, Cd and Zn in several real samples.

Simultaneous preconcentration of copper, zinc, cadmium, and nickel in water samples by cloud point extraction using 4-(2-pyridylazo)-resorcinol and their determination by inductively coupled plasma optic emission spectrometry

International Nuclear Information System (INIS)

Silva, Edson Luiz; Santos Roldan, Paulo dos; Gine, Maria Fernanda

2009-01-01

A procedure for simultaneous separation/preconcentration of copper, zinc, cadmium, and nickel in water samples, based on cloud point extraction (CPE) as a prior step to their determination by inductively coupled plasma optic emission spectrometry (ICP-OES), has been developed. The analytes reacted with 4-(2-pyridylazo)-resorcinol (PAR) at pH 5 to form hydrophobic chelates, which were separated and preconcentrated in a surfactant-rich phase of octylphenoxypolyethoxyethanol (Triton X-114). The parameters affecting the extraction efficiency of the proposed method, such as sample pH, complexing agent concentration, buffer amount, surfactant concentration, temperature, kinetics of complexation reaction, and incubation time were optimized and their respective values were 5, 0.6 mmol L -1 , 0.3 mL, 0.15% (w/v), 50 deg. C, 40 min, and 10 min for 15 mL of preconcentrated solution. The method presented precision (R.S.D.) between 1.3% and 2.6% (n = 9). The concentration factors with and without dilution of the surfactant-rich phase for the analytes ranged from 9.4 to 10.1 and from 94.0 to 100.1, respectively. The limits of detection (L.O.D.) obtained for copper, zinc, cadmium, and nickel were 1.2, 1.1, 1.0, and 6.3 μg L -1 , respectively. The accuracy of the procedure was evaluated through recovery experiments on aqueous samples.

Production of radioactive ion beams and resonance ionization spectroscopy with the laser ion source at on-line isotope separator ISOLDE

International Nuclear Information System (INIS)

Fedosseev, V.N.; )

2005-01-01

Full text: The resonance ionisation laser ion source (RILIS) of the ISOLDE on-line isotope separation facility at CERN is based on the method of laser step-wise resonance ionisation of atoms in a hot metal cavity. Using the system of dye lasers pumped by copper vapour lasers the ion beams of many different metallic elements have been produced at ISOLDE with an ionization efficiency of up to 27%. The high selectivity of the resonance ionization is an important asset for the study of short-lived nuclides produced in targets bombarded by the proton beam of the CERN Booster accelerator. Radioactive ion beams of Be, Mg, Al, Mn, Ni, Cu, Zn, Ga, Ag, Cd, In, Sn, Sb, Tb, Yb, Tl, Pb and Bi have been generated with the RILIS. Setting the RILIS laser in the narrow line-width mode provides conditions for a high-resolution study of hyperfine structure and isotopic shifts of atomic lines for short-lived isotopes. The isomer selective ionization of Cu, Ag and Pb isotopes has been achieved by appropriate tuning of laser wavelengths

[Study on extracting and separating curcuminoids from Curcuma longa rhizome using ultrasound strengthen by microemulsion].

Science.gov (United States)

Yue, Chun-Hua; Zheng, Li-Tao; Guo, Qi-Ming; Li, Kun-Ping

2014-05-01

To establish a new method for the extraction and separation of curcuminoids from Curcuma longa rhizome by cloud-point preconcentration using microemulsions as solvent. The spectrophotometry was used to detect the solubility of curcumin in different oil phase, emulsifier and auxiliary emulsifier, and the microemulsion prescription was used for false three-phase figure optimization. The extraction process was optimized by uniform experiment design. The curcuminoids were separated from microemulsion extract by cloud-point preconcentration. Oil phase was oleic acid ethyl ester; Emulsifier was OP emulsifier; Auxiliary emulsifier was polyethylene glycol(peg) 400; The quantity of emulsifier to auxiliary emulsifier was the ratio of 5: 1; Microemulsion prescription was water-oleic acid ethyl ester-mixed emulsifier (0.45:0.1:0.45). The optimum extraction process was: time for 12.5 min, temperature of 52 degrees C, power of 360 W, frequency of 400 kHz, and the liquid-solid ratio of 40:1. The extraction rate of curcuminoids was 92.17% and 86.85% in microemulsion and oil phase, respectively. Curcuminoids is soluble in this microemulsion prescription with good extraction rate. This method is simple and suitable for curcuminoids extraction from Curcuma longa rhizome.

On line spectrophotometry with optical fibers. Application to uranium-plutonium separation in a spent fuel reprocessing plant

International Nuclear Information System (INIS)

Boisde, G.; Mus, G.; Tachon, M.

1985-06-01

Optimization of mixer-settler operation for uranium-plutonium separation in the Purex process can be obtained by remote spectrophotometry with optical fibers. Data acquisition on uranium VI, uranium IV and plutonium III is examined in function of acidity and nitrate content of the solution. Principles for on line multicomponent monitoring and mathematical modelization of the measurements are described [fr

Preconcentration and Speciation of Trace Elements and Trace-Element Analogues of Radionuclides by Neutron Activation Analysis

International Nuclear Information System (INIS)

Chatt, A.

1999-01-01

We have developed a number of preconcentration neutron activation analysis (PNAA) methods in our laboratory for the determination of trace elements in a variety of complex sample matrices. We developed a number of cocrystallization and coprecipitation methods for the determination of trace elements in water samples. We developed several methods for the determination of I in foods and diets. We have developed a number of PNAA methods in our laboratory We determined As and Sb in geological materials and natural waters by coprecipitation with Se and Au in silicate rocks and ores by coprecipitation with Te followed by NAA. We developed an indirect NAA method for the determination of B in leachates of borosilicate glass. We have been interested in studying the speciation of Am, Tc, and Np in simulated vitrified groundwater leachates of high-level wastes under oxid and anoxic conditions using a number of techniques. We then used PNAA methods to study speciation of trace-element analogues of radionuclides. We have been able to apply biochemical techniques and NAA for the separation, preconcentration, and characterization of metalloprotein and protein-bound trace-element species in subcellular fractions of bovine kidneys. Lately, we have concentrated our efforts to develop chemical and biochemical methods in conjunction with NAA, NMR, and MS for the separation and identification of extractable organohalogens (EOX) in tissues of beluga whales, cod, and northern pink shrimp

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).

Preconcentration of gold ions from water samples by modified organo-nanoclay sorbent prior to flame atomic absorption spectrometry determination

Energy Technology Data Exchange (ETDEWEB)

Afzali, Daryoush, E-mail: daryoush_afzali@yahoo.com [Nanochemistry Department, Research Institute of Environmental Sciences, International Center for Science, High Technology and Environmental Sciences, Kerman (Iran, Islamic Republic of); Mostafavi, Ali [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Mirzaei, Mohammad [Nanochemistry Department, Research Institute of Environmental Sciences, International Center for Science, High Technology and Environmental Sciences, Kerman (Iran, Islamic Republic of); Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of)

2010-09-15

In this work, the applicability of modified organo nanoclay as a new and easy prepared solid sorbent for the preconcentration of trace amounts of Au(III) ion from water samples is studied. The organo nanoclay was modified with 5-(4'-dimethylamino benzyliden)-rhodanine and used as a sorbent for separation of Au(III) ions. The sorption of gold ions was quantitative in the pH range of 2.0-6.0. Quantitative desorption occurred with 6.0 mL of 1.0 mol L{sup -1} Na{sub 2}S{sub 2}O{sub 3}. The amount of eluted Au(III) was measured using flame atomic absorption spectrometry. In the initial solution the linear dynamic range was in the range of 0.45 ng mL{sup -1} to 10.0 {mu}g mL{sup -1}, the detection limit was 0.1 ng mL{sup -1} and the preconcentration factor was 105. Also, the relative standard deviation was {+-}2.3% (n = 8 and C = 2.0 {mu}g mL{sup -1}) and the maximum capacity of the sorbent was 3.9 mg of Au(III) per gram of modified organo nanoclay. The influences of the experimental parameters including sample pH, eluent volume and eluent type, sample volume, and interference of some ions on the recoveries of the gold ion were investigated. The proposed method was applied for preconcentration and determination of gold in different samples.

Separation and Pre-concentration of Cadmium, Copper, Lead, Nickel and Zinc by Solid-Liquid Extraction of their Cocrystallized Naphthalene Dithizone Chelate in Saline Matrices

Directory of Open Access Journals (Sweden)

Costa Antônio C. Spínola

2002-01-01

Full Text Available A procedure for separation and pre-concentration of trace amounts of cadmium, copper, lead, nickel, and zinc in brine samples has been proposed. It is based on the adsorption of metal ions onto dithizone co-crystallized with microcrystalline naphthalene, in the pH range 8.5-9.1. Nitric acid is used to back-extract the cations from the solid phase, which are measured by ICP-OES. Various parameters, such as the effect of pH, stirring time, and amounts of solid phase, have been studied in detail, to optimize the conditions for the determination of trace amounts of Cd, Cu, Pb, Ni and Zn in synthetic brine samples. The limits of detection values expressed in mug L-1 are 44 (Zn, 11 (Ni, 30 (Cd, 47 (Pb and 11 (Cu. The precision of the procedure was determined by running 10 replicate samples, each one containing 250 mug L-1 of each element and the relative standard deviations were 2.71 % (Cd, 2.15 % (Cu, 1.53 % (Pb, 2.47 % (Ni, and 2.78 % (Zn. The accuracy of the procedure was confirmed by applying the analyte additions method and the results indicated that quantitative recoveries (superscript three 95 % were obtained.

Preconcentration of uranium in water samples using dispersive ...

African Journals Online (AJOL)

Preconcentration of uranium in water samples using dispersive liquid-liquid micro- extraction coupled with solid-phase extraction and determination with inductively coupled plasma-optical emission spectrometry.

MULTIELEMENT SOLID PHASE PRECONCENTRATION USING A CHELATING RESIN OF STYRENE DIVINYLBENZENE COPOLYMER AND APPLICATION TO ANALYSIS OF SEAWATER AND FISH OTOLITHS BY INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY (ICP�MS)

Science.gov (United States)

Zereen, Fahmida; Yilmaz, Vedat; Arslan, Zikri

2013-01-01

A new chelating resin has been synthesized by immobilizing 4–(2–thiazolylazo) resorcinol (TAR) onto styrene divinlybenzene copolymer and examined for on-line solid phase extraction/preconcentration of Cd, Co, Cu, Ni, Pb and Zn in seawater and fish otoliths for determination by inductively plasma mass spectrometry (ICP-MS). A volume of 5.0 mL sample solution was loaded onto the mini column of TAR immobilized resin at 2.0 mL min−1 via a sequential injection system. The optimum pH for multielement preconcentration was around pH 5.5. Recoveries were better than 96% in artificial seawater. Elution was achieved with 1.0 mL of 0.75 mol L−1 HNO3. The resin possesses large sorption capacity ranging from 82.0 µmol g−1 for Pb to 319 µmol g−1 for Cu. The detection limits (3s) varied between 0.0016 µg L−1 (Cd) and to 0.015 µg L−1 (Zn) for preconcentration of 5.0 mL blank solutions (pH 5.5). Relative standard deviation (RSD)for three replicate runs was between 0.3% (Cd) and 6% (Zn) at 1.0 µg L−1 level. The procedure was validated by analysis of Nearshore Seawater certified reference material (CASS–4), and then successfully applied to the determination of the trace elements in fish otoliths (CRM 22) and in coastal seawater and estuarine water samples. PMID:24976635

Trends in preconcentration procedures for metal determination using atomic spectrometry techniques

International Nuclear Information System (INIS)

Godoi Pereira, M. de; Arruda, M.A.Z.

2003-01-01

Methods for metal preconcentration are often described in the literature. However, purposes are often different, depending on whether the methods are applied in environmental, clinical or technological fields. The respective method needs to be efficient, give high sensitivity, and ideally also is selective which is useful when used in combination with atomic spectroscopy. This review presents the actual tendencies in metal preconcentration using techniques such as flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS), hydride generation atomic absorption spectrometry (HGAAS), inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry (ICP-MS). Procedures based on related to electrochemical, coprecipitation/precipitation, liquid-liquid and solid-liquid extraction and atom trapping mechanisms are presented. (author)

MICELLE-MEDIATED EXTRACTION AS A TOOL FOR SEPARATION AND PRECONCENTRATION IN COPPER ANALYSIS

Directory of Open Access Journals (Sweden)

F. Ahmadia

2010-06-01

Full Text Available A cloud point extraction method was presented for preconcentration of copper in various samples. After complexation with 4-Amino-2,3-dimethyl-1-phenyl-3-pyrazoline-5-one (ADPP or N-Benzoyl-N-phenylhydroxylamine (BPA  in water, analyte ions are quantitatively extracted to the phase rich in Triton X-114 after centrifugation. 2.0 mol L-1 HNO3 solution in methanol was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS. The adopted concentrations for ADPP, Triton X-114, HNO3 and parameters such as bath temperature, centrifuge rate and time were optimized. Detection limits (3SDb/m of 1.3 and 1.9 ng mL-1 for ADPP and BPA along with enrichment factors of 30 and 38 for ADPP and BPA were achieved. The high efficiency of cloud point extraction to carry out the determination of analyte in complex matrices was demonstrated. The proposed method was applied to the analysis of biological, industrial, natural and wastewater, soil and blood samples.   Keywords: 4-Amino-2,3-dimethyl-1-phenyl-3-pyrazoline-5-one (ADPP, N-Benzoyl-N-phenylhydroxylamine (BPA ,   Cloud Point Extraction, Triton X-114, Flame Atomic Absorption Spectrometry.

Pre-concentration of Cr, Mn, Fe and Co of water sea and analysis by plasma emission spectroscopy - DCP

International Nuclear Information System (INIS)

Ferreira, E.M.M.

1985-01-01

Studies of separation and pre-concentration methods of chromium, manganese, iron and cobalt from seawater, that allow use control methods of 5 1 Cr, 5 4 Mn, 5 5 , 5 9 Fe, 5 8 , 5 9 Co with a better sensibility and the determination of this elements by atomic absorption spectroscopy or plasma emission spectroscopy are described. This methods of seawater analysis will use near the region of Angra I reactor. (author)

Preconcentration NAA for simultaneous multielemental determination in water sample

International Nuclear Information System (INIS)

Chatt, A.

1999-01-01

Full text: Environment concerns with water, air, land and their interrelationship viz., human beings, fauna and flora. One of the important environmental compartments is water. Elements present in water might face a whole lot of physico-chemical conditions. This poses challenges to measure their total concentrations as well as different species. Preconcentration of the elements present in water samples is a necessary requisites in water analysis. For multi elements concentration measurements, Neutron Activation Analysis (NAA) is one of the preferred analytical techniques due to its sensitivity and selectivity. In this talk preconcentration NAA for multielemental determination in water sample determination will be discussed

The determination of chromium in water samples by neutron activation analysis after preconcentration on activated carbon

International Nuclear Information System (INIS)

Sloot, H.A. van der

1977-01-01

A method is presented for the determination of chromium in sea- and fresh water. Chromium is concentrated on activated carbon from a neutral solution after a previous reduction of chromate with sodium sulfite at pH 1.5. The adsorption conditions, acidity, concentrations, amount of carbon, stirring-time, sample-volume, salinity, the influence of storage on the ratio of tervalent to hexavalent chromium, were investigated. The final determination of the total chromium content is performed by instrumental neutron-activation analysis. By preconcentration on activated carbon, a differentiation between tervalent and hexavalent chromium is possible. A separate determination of both species is not yet feasible due to the high carbon blank and to the necessity of measuring the adsorption percentage on carbon. The lower limit of determination, which depends on the value of the carbon blank, is 0.05 μg Cr/l with a precision of 20%. The determination is hampered by the considerable blank from the carbon. The use of activated carbon prepared from recrystallized sugar will probably improve the lower limit of determination and possibly allow the determination of chromate. (T.G.)

Development of the determination method of rare earth elements in seawater by ICP-MS with an on-line preconcentration column of improved iminodiacetate resin and its application to Tokyo Bay seawater

International Nuclear Information System (INIS)

Tsuneto, Atsushi; Suzuki, Yoshinari; Furuta, Naoki; Furusho, Yoshiaki

2009-01-01

In order to determine rare earth elements (REEs) in seawater by using inductively coupled plasma mass spectrometry (ICP-MS) with an on-line preconcentration column, we used the improved iminodiacetate chelate resin (MetaSEP ME-2) that had a cation-type alkyl group. Its operating conditions were optimized, and the recoveries of REEs and the removal rates of matrix elements were compared with other resins. Ca and Mg were removed more efficiently under a buffer solution of pH 5.0. The removal efficiencies of Ca and Mg using MetaSEP ME-2 were better than those using other resins. We determined REEs in a seawater reference material (NASS-5) with MetaSEP ME-2. The obtained results were in good agreement with the reference values. We applied this method to the determination of REEs in seawater collected from Tokyo Bay, and evaluated the distribution patterns of REEs. Consequently, the positive anomaly of Gd in the small-molecule fraction was observed. The positive anomaly of Gd can be attributed to the outflow of Gd compounds, which are used for a magnetic resonance imaging contrast medium. (author)

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.)

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

Investigation of gas discharge ion sources for on-line mass separation

International Nuclear Information System (INIS)

Kirchner, R.

1976-03-01

The development of efficient gas discharge ion sources with axial beam extraction for on-line mass separation is described. The aim of the investigation was to increase the ion source temperature, the lifetime and the ionisation yield in comparison to present low-pressure are discharge ion sources and to reduce the ion current density from usually 1 to 100 mA/cm 3 . In all ion sources the pressure range below the minimal ignition pressure of the arc discharge was investigated. As a result an ion source was developed which works at small changes in geometry and in electric device of a Nielsen source with high ionization yield (up to 50% for xenon) stabil and without ignition difficulties up to 10 -5 Torr. At a typical pressure of 3 x 10 -5 Torr ion current and ion current density are about 1 μA and 0.1 mA/cm 3 respectively besides high yield and a great emission aperture (diameter 1.2 mm). (orig.) [de

Uranium preconcentration from seawater using adsorptive membranes

International Nuclear Information System (INIS)

Das, Sadananda; Pandey, A.K.; Manchanda, V.K.; Athawale, A.A.

2009-01-01

Uranium recovery from bio-aggressive but lean feed like seawater is a challenging problem as it requires in situ preconcentration of uranium in presence of huge excess of competing ions with fast sorption kinetics. In our laboratory, widely used amidoxime membrane (AO-membrane) was evaluated for uranium sorption under seawater conditions. This study indicated that AO-membrane was inherently slow because of the complexation chemistry involved in transfer of U(VI) from (UO 2 (CO 3 ) 3 ) 4 - to AO sites in membrane. In order to search better options, several chemical compositions of membrane were scanned for their efficacy for uranium preconcentration from seawater, and concluded that EGMP-membrane offers several advantages over AO-membrane. In this paper, the comparison of EGMP-membrane with AO-membrane for uranium sorption under seawater conditions has been reviewed. (author)

Innovative in-line separators: removal of water or sand in oil/water and gas/liquid/solid pipelines

Energy Technology Data Exchange (ETDEWEB)

Jepson, Paul; Cheolho Kang; Gopal, Madan [CC Technologies, Dublin, OH (United States)

2003-07-01

In oil and gas production, multiphase mixtures are often separated before downstream processing. The separators are large, often 20 - 40 feet long and large diameter and use sophisticated internals. The costs are in the millions of dollars. Further, the sand and water in the flow can cause severe internal erosion and corrosion respectively before the flow reaches the separators. The CC Technologies/MIST In line Separation System is a cost-effective, efficient device for use in multiphase environments. The device is applicable for gas/solid, gas/liquid/solid and oil/water systems and offers exceptional separation between phases for a fraction of the cost of expensive gravity separators and hydro cyclones. The System contains no moving parts and is designed to be of the same diameter as the pipe, and experiences low shear forces. It can be fabricated with standard pipes. The efficiency of the separator has been determined in an industrial scale, pilot plant test facility at CC Technologies in 4-inch diameter pipes and has been found to be in excess of 98-99% for the removal of sand. Two phase oil/water separation effectiveness is in excess of 90% in 1-stage and 95% in 2 - stage. (author)

Separate collection of plastic waste, better than technical sorting from municipal solid waste?

Science.gov (United States)

Feil, Alexander; Pretz, Thomas; Jansen, Michael; Thoden van Velzen, Eggo U

2017-02-01

The politically preferred solution to fulfil legal recycling demands is often implementing separate collection systems. However, experience shows their limitations, particularly in urban centres with a high population density. In response to the European Union landfill directive, mechanical biological waste treatment plants have been installed all over Europe. This technology makes it possible to retrieve plastic waste from municipal solid waste. Operators of mechanical biological waste treatment plants, both in Germany and the Netherlands, have started to change their mechanical separation processes to additionally produce plastic pre-concentrates. Results from mechanical biological waste treatment and separate collection of post-consumer packaging waste will be presented and compared. They prove that both the yield and the quality of plastic waste provided as feedstock for the production of secondary plastic raw material are largely comparable. An economic assessment shows which conditions for a technical sorting plant are economically attractive in comparison to separate collection systems. It is, however, unlikely that plastic recycling will ever reach cost neutrality.

Flame atomic absorption spectrometric determination of trace amounts of Pb(II) and Cr(III) in biological, food and environmental samples after preconcentration by modified nano-alumina

International Nuclear Information System (INIS)

Afkhami, A.; Madrakian, T.; Saber-Tehrani, M.; Bagheri, H.

2011-01-01

A new solid-phase extraction sorbent was used for the preconcentration of Pb(II) and Cr(III) ions prior to their determination by flame atomic absorption spectrometry. It was prepared by immobilization of 2,4-dinitrophenylhydrazine on nano-alumina coated with sodium dodecyl sulfate. The sorbent was characterized by scanning electron microscopy, N 2 adsorption and Fourier transform infrared spectrometry, and used for preconcentration and separation of Pb(II) and Cr(III) from aqueous solutions. The ions on the sorbent were eluted with a mixture of nitric acid and methanol. The effects of sample pH, flow rates of samples and eluent, type of eluent, breakthrough volume and potentially interfering ions were studied. Linearity is maintained between 1.2 and 350 μg L -1 of Pb(II), and between 2.4 and 520 μg L -1 of Cr(III) for an 800-mL sample. The detection limit (3 s, N=10) for Pb(II) and Cr(III) ions is 0.43 and 0.55 μg L -1 , respectively, and the maximum preconcentration factor is 267. The method was successfully applied to the evaluation of these trace and toxic metals in various water, food, industrial effluent and urine samples. (author)

Preparation of modified magnetic nanoparticles as a sorbent for the preconcentration and determination of cadmium ions in food and environmental water samples prior to flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Mirabi, Ali; Dalirandeh, Zeinab [Department of Chemistry, Qaemshahr Branch, Islamic Azad University, Qaemshahr (Iran, Islamic Republic of); Rad, Ali Shokuhi, E-mail: a.shokuhi@qaemshahriau.ac.ir [Department of Chemical Engineering, Qaemshahr Branch, Islamic Azad University, Qaemshahr (Iran, Islamic Republic of)

2015-05-01

A new method has been developed for the separation/preconcentration of trace level cadmium ions using diphenyl carbazone/sodium dodecyl sulfate immobilized on magnetic nanoparticle Fe{sub 3}O{sub 4} as a new sorbent SPE and their determination by flame atomic absorption spectrometry (FAAS). Synthesized nanoparticle was characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). Various influencing parameters on the separation and preconcentration of trace level cadmium ions such as, pH value, amount of nanoparticles, amount of diphenyl carbazone, condition of eluting solution, the effects of matrix ions were examined. The cadmium ions can be eluted from the modified magnetic nanoparticle using 1 mol L{sup −1} HCl as a desorption reagent. The detection limit of this method for cadmium was 3.71 ng ml{sup −1} and the R.S.D. was 0.503% (n=6). The advantages of this new method include rapidity, easy preparation of sorbents and a high concentration factor. The proposed method has been applied to the determination of Cd ions at trace levels in real samples such as, green tea, rice, tobacco, carrot, lettuce, ginseng, spice, tap water, river water, sea water with satisfactory results. - Highlights: • MNPs method is economical, simple, rapid and sensitive for trace analysis of Cd. • High preconcentration factor was obtained easily through this method. • A detection limit at ng mL{sup −1} level was achieved with 100.0 mL of sample. • This method provides good repeatability and extraction efficiency in a short time.

Preparation of modified magnetic nanoparticles as a sorbent for the preconcentration and determination of cadmium ions in food and environmental water samples prior to flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Mirabi, Ali; Dalirandeh, Zeinab; Rad, Ali Shokuhi

2015-01-01

A new method has been developed for the separation/preconcentration of trace level cadmium ions using diphenyl carbazone/sodium dodecyl sulfate immobilized on magnetic nanoparticle Fe 3 O 4 as a new sorbent SPE and their determination by flame atomic absorption spectrometry (FAAS). Synthesized nanoparticle was characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). Various influencing parameters on the separation and preconcentration of trace level cadmium ions such as, pH value, amount of nanoparticles, amount of diphenyl carbazone, condition of eluting solution, the effects of matrix ions were examined. The cadmium ions can be eluted from the modified magnetic nanoparticle using 1 mol L −1 HCl as a desorption reagent. The detection limit of this method for cadmium was 3.71 ng ml −1 and the R.S.D. was 0.503% (n=6). The advantages of this new method include rapidity, easy preparation of sorbents and a high concentration factor. The proposed method has been applied to the determination of Cd ions at trace levels in real samples such as, green tea, rice, tobacco, carrot, lettuce, ginseng, spice, tap water, river water, sea water with satisfactory results. - Highlights: • MNPs method is economical, simple, rapid and sensitive for trace analysis of Cd. • High preconcentration factor was obtained easily through this method. • A detection limit at ng mL −1 level was achieved with 100.0 mL of sample. • This method provides good repeatability and extraction efficiency in a short time

An on-line adaptive core monitoring system

International Nuclear Information System (INIS)

Verspeek, J.A.; Bruggink, J.C.; Karuza, J.

1997-01-01

An on-line core monitoring system has been in operation for three years in the Dodewaard Nuclear Power Plant. The core monitor uses the on-line measured reactor data as an input for a power distribution calculation. The measurements are frequently performed. The system is used for monitoring as well as for predicting purposes. The limiting thermal hydraulic parameters are monitored as well as the pellet-clad interaction limits. The data are added to a history file used for cycle burn-up calculations and trending of parameters. The reactor states are presented through a convenient graphical user interface. (authors)

Effect of chromatographic separation on ASP system interface tension and the countermeasures

Directory of Open Access Journals (Sweden)

Jiawei REN

2016-06-01

Full Text Available Because of the existing chromatographic separation phenomenon, ASP flooding changes original nature of the system. Therefore, in laboratory ultra-low interfacial tension ASP system is preferred for sand packs flow experiment to research on the effect of chromatographic separation on ASP system interface tension. The two parameters of "breakthrough time" and "output difference" are used to describe the degree of chromatographic separation, and the produced fluid interfacial tensions at the outlet end at 120 min is measured. The research shows that there exists chromatographic separation between three chemicals of ASP system, with first polymer breakthrough and finally surfactant breakthrough; there is most serious chromatographic separation between surfactant and polymer, while minimum chromatographic separation between alkali and polymer; chromatographic separation makes ASP interfacial tension increase from 10^-3 magnitude to 10^-2 magnitude, affecting flooding effect of ASP system. Thus, reducing the loss of surfactant in the formation will be the main measure to reduce the degree of chromatographic separation. Using sophorolipid as sacrificial agent to replace part of the surfactant injected into formation before ASP system can effectively reduce the impact of chromatography separation and more effectively improve the ultimate recovery ratio.

On-chip DNA preconcentration in different media conductivities by electrodeless dielectrophoresis

KAUST Repository

Li, Shunbo

2015-09-01

© 2015 AIP Publishing LLC. Electrodeless dielectrophoresis is the best choice to achieve preconcentration of nanoparticles and biomolecules due to its simple, robust, and easy implementation. We designed a simple chip with microchannels and nano-slits in between and then studied the trapping of DNA in high conductive medium and low conductive medium, corresponding to positive and negative dielectrophoresis (DEP), respectively. It is very important to investigate the trapping in media with different conductivities since one always has to deal with the sample solutions with different conductivities. The trapping process was analyzed by the fluorescent intensity changes. The results showed that DNA could be trapped at the nano-slit in both high and low conductive media in a lower electric field strength (10 V/cm) compared to the existing methods. This is a significant improvement to suppress the Joule heating effect in DEP related experiments. Our work may give insight to researchers for DNA trapping by a simple and low cost device in the Lab-on-a-Chip system.

Production of chemically reactive radioactive ion beams through on-line separation; Production de faisceaux d'ions radioactifs chimiquement reactifs par separation en ligne

Energy Technology Data Exchange (ETDEWEB)

Joinet, A

2003-10-01

The ISOL (isotope separation on line) allows the production of secondary radioactive ion beams through spallation or fragmentation or fission reactions that take place in a thick target bombarded by a high intensity primary beam. The challenge is to increase the intensity and purity of the radioactive beam. The optimization of the system target/source requires the right choice of material for the target by taking into account the stability of the material, its reactivity and the ionization method used. The target is an essential part of the system because radioactive elements are generated in it and are released more or less quickly. Tests have been made in order to select the best fitted material for the release of S, Se, Te, Ge and Sn. Materials tested as target filling are: ZrO{sub 2}, Nb, Ti, V,TiO{sub 2}, CeO{sub x}, ThO{sub 2}, C, ZrC{sub 4} and VC). Other molecules such as: COSe, COS, SeS, COTe, GeS, SiS, SnS have been studied to ease the extraction of recoil nuclei (Se, S, Te, Ge and Sn) produced inside the target.

The low-ion QSO absorption-line systems

International Nuclear Information System (INIS)

Lanzetta, K.M.

1988-01-01

Various techniques are used to investigate the class of QSO absorption-line systems that exhibit low-ion absorption lines. Four separate investigations are conducted as follows: Spectroscopy of 32 QSOs at red wavelengths is presented and used to investigate intermediate-redshift MgII absorption. A total of 22 Mg II doublets are detected, from which properties of the Mg II absorbers are derived. Marginal evidence for intrinsic evolution of the number density of the Mg II absorbers with redshift is found. The data are combined with previous observations of C IV and C II seen in the same QSOs at blue wavelengths, and the properties of Mg II- and C IV-selected systems are compared. A sample is constructed of 129 QSOs for which are available published data suitable for detecting absorption-line systems that are optically thick to Lyman continuum radiation. A total of 53 such Lyman-limit systems are found, from which properties of the Lyman-limit systems are derived. It is found that the rate of incidence of the systems does not strongly evolved with redshift. This result is contrasted with the evolution found previously for systems selected on the basis of Mg II absorption. Spectroscopy at red wavelengths of eight QSOs with known damped Lyα absorption systems is presented. Spectroscopic and spectrophotometric observations aimed at detecting molecular hydrogen and dust in the z = 2.796 damped Lyα absorber toward Q1337 + 113 are presented

Solid-phase extraction and high-performance liquid chromatographic separation of pigments of red wines.

Science.gov (United States)

Csiktusnádi Kiss, G A; Forgács, E; Cserháti, T; Candeias, M; Vilas-Boas, L; Bronze, R; Spranger, I

2000-08-11

The adsorption and desorption capacities of 11 different solid-phase extraction sorbents were tested for the preconcenration of pigments of various Hungarian red wines. The concentrates were evaluated by multiwavelengh spectrophotometry combined with a spectral mapping technique (SPM) and by reversed-phase high-performance liquid chromatography. The highest (10-fold) concentration of pigments was achieved on octadecylsilica sorbent. It can be used five times without losing adsorption and desorption characteristics. SPM indicated that multiwavelength spectrophotometry can be employed for the differentiation of red wines. Comparison of the chromatograms of pigments with and without preconcentration showed that preconcentration makes possible the separation and detection of pigments present in low concentration in red wines.

An on-line monitoring system for navigation equipment

Science.gov (United States)

Wang, Bo; Yang, Ping; Liu, Jing; Yang, Zhengbo; Liang, Fei

2017-10-01

Civil air navigation equipment is the most important infrastructure of Civil Aviation, which is closely related to flight safety. In addition to regular flight inspection, navigation equipment's patrol measuring, maintenance measuring, running measuring under special weather conditions are the important means of ensuring aviation flight safety. According to the safety maintenance requirements of Civil Aviation Air Traffic Control navigation equipment, this paper developed one on-line monitoring system with independent intellectual property rights for navigation equipment, the system breakthroughs the key technologies of measuring navigation equipment on-line including Instrument Landing System (ILS) and VHF Omni-directional Range (VOR), which also meets the requirements of navigation equipment ground measurement set by the ICAO DOC 8071, it provides technical means of the ground on-line measurement for navigation equipment, improves the safety of navigation equipment operation, and reduces the impact of measuring navigation equipment on airport operation.

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.

Performance and stability of low-cost dye-sensitized solar cell based crude and pre-concentrated anthocyanins: Combined experimental and DFT/TDDFT study

Science.gov (United States)

Chaiamornnugool, Phrompak; Tontapha, Sarawut; Phatchana, Ratchanee; Ratchapolthavisin, Nattawat; Kanokmedhakul, Somdej; Sang-aroon, Wichien; Amornkitbamrung, Vittaya

2017-01-01

The low cost DSSCs utilized by crude and pre-concentrated anthocyanins extracted from six anthocyanin-rich samples including mangosteen pericarp, roselle, red cabbage, Thai berry, black rice and blue pea were fabricated. Their photo-to-current conversion efficiencies and stability were examined. Pre-concentrated extracts were obtained by solid phase extraction (SPE) using C18 cartridge. The results obviously showed that all pre-concentrated extracts performed on photovoltaic performances in DSSCs better than crude extracts except for mangosteen pericarp. The DSSC sensitized by pre-concentrated anthocyanin from roselle and red cabbage showed maximum current efficiency η = 0.71% while DSSC sensitized by crude anthocyanin from mangosteen pericarp reached maximum efficiency η = 0.97%. In addition, pre-concentrated extract based cells possess more stability than those of crude extract based cells. This indicates that pre-concentration of anthocyanin via SPE method is very effective for DSSCs based on good photovoltaic performance and stability. The DFT/TDDFT calculations of electronic and photoelectrochemical properties of the major anthocyanins found in the samples are employed to support the experimental results.

Separation and preconcentration of riboflavin from human plasma using polythionine coated magnetite/hydroxyapatite nanocomposite prior to analysis by surfactant-enhanced fluorimetry

Science.gov (United States)

Farzin, Leila; Shamsipur, Mojtaba

2017-09-01

The exploration of novel adsorption properties of conductive polymers based on hybridization with biocompatible nanomaterials receives an increasing interest. In this regard, hydroxyapatite (HA) bioceramic is of critical importance mainly owing to its facile synthesis, high surface area, economic and low toxicity in biological environments. In this work, we first prepared and characterized a magnetite/hydroxyapatite (Fe3O4/HA) nanocomposite using the bio-waste chicken eggshell via an attractive green way that involved low cost and irrespective of toxicity. Then, polythionine as a novel class of conductive polymers was in situ coated on the synthesized magnetic bioceramic for the separation and preconcentration of riboflavin (vitamin B2) in human plasma before its fluorimetric determination. Considering the putative role of riboflavin in protecting against cancer and cardiovascular diseases, it is essential to evaluate this vitamin in biological fluids. The described method possesses a linear range of 0.75-262.5 μg L- 1 (R2 = 0.9985) and a detection limit of 0.20 μg L- 1 (signal-to-noise ratio of 3). The relative standard deviations (RSDs) for single-sorbent repeatability and sorbent-to-sorbent reproducibility were less than 4.0% and 7.6% (n = 5), respectively. The respective enrichment factor and extraction recovery of the method found to be 35.7 and 98.4%. The analytical performance of method for riboflavin was characterized by good consistency of the results with those obtained by the enzyme-linked immunosorbent assay (ELISA) conventional method (p-value of < 0.05). The optimized protocol intended for control determinations of riboflavin in human subjects and is addressed to clinical laboratories.

In-Line Oil-Water Separation in Swirling Flow (USB stick)

NARCIS (Netherlands)

Slot, J.J.; van Campen, L.J.A.M.; Hoeijmakers, Hendrik Willem Marie; Mudde, R.F.; Johansen, S.T.

2011-01-01

An in-line oil-water separator has been designed and is investigated for single- and two-phase flow. Numerical single-phase flow results show an annular reversed flow region. This flow pattern agrees qualitatively with results from measurements. In the two-phase flow simulations two different drag

In-line near real time monitoring of fluid streams in separation processes for used nuclear fuel - 5146

International Nuclear Information System (INIS)

Nee, K.; Nilsson, M.

2015-01-01

Applying spectroscopic tools for chemical processes has been intensively studied in various industries owing to its rapid and non-destructive analysis for detecting chemical components and determine physical characteristic in a process stream. The general complexity of separation processes for used nuclear fuel, e.g., chemical speciation, temperature variations, and prominent process security and safety concerns, require a well-secured and robust monitoring system to provide precise information of the process streams at real time without interference. Multivariate analysis accompanied with spectral measurements is a powerful statistic technique that can be used to monitor this complex chemical system. In this work, chemometric models that respond to the chemical components in the fluid samples were calibrated and validated to establish an in-line near real time monitoring system. The models show good prediction accuracy using partial least square regression analysis on the spectral data obtained from UV/Vis/NIR spectroscopies. The models were tested on a solvent extraction process using a single stage centrifugal contactor in our laboratory to determine the performance of an in-line near real time monitoring system. (authors)

Determination of trace elements in ground water by two preconcentration methods using atomic absorption spectrometry

International Nuclear Information System (INIS)

Elhag, A. Y.

2004-01-01

This is a comparative study between two different methods of preconcentration done to separate the trace elements cadmium, nickel. chromium, manganese, copper, zinc, and lead in drinking (ground) water samples taken from different locations in Gezira State, central Sudan (the map); these methods are (coprecipitation) with aluminium hydroxide and by Ammonium Pyrrolidine Dithiocarbamate (APDC) using Methyl Isobutyl Ketone (MIBK) as an organic solvent; and subsequent analysis by Atomic Absorption Spectrometry (AAS) for both methods. The result of comparison showed the superiority of the (APDC) coprecipitation method over the aluminium hydroxide coprecipitation method in the total percentage recoveries of the studied trace elements in drinking (ground) water samples, such results confirm previous studies. This study also involves direct analysis of these water samples by atomic absorption spectrometry to determine the concentrations of trace elements Cadmium, Nickel, Chromium, Manganese, Copper, Zinc and Lead and compare it to the corresponding guide line values described by the World Health Organization and the maximum concentrations of trace elements in drinking water permitted by the Sudanese Standards and Metrology Organizations (SSMO), where the concentrations of some elements in some samples were found to be different than the described values by both of the organizations. The study includes a trial to throw light on the effect of the proximity of the water samples sources to the Blue Nile river on its trace elements concentrations; no relation was proved to exist in that respect.(Author)

UWIS isotope separator

Energy Technology Data Exchange (ETDEWEB)

Wojtasiewicz, A. [Warsaw Univ., Inst. of Experimental Physics, Nuclear Physics Div., Warsaw (Poland)

1997-12-31

Since 1995 the University of Warsaw Isotope Separator group has participated in the ISOL/IGISOL project at the Heavy Ion Cyclotron. This project consists in installation of an isotope separator (on line with cyclotron heavy ion beam) with a hot plasma ion source (ISOL system) and/or with an ion guide source (IGISOL system). In the report the short description of the present status of the project is presented. 2 figs, 10 refs.

Sea floor separation system; Havbunnsseparasjonssystem

Energy Technology Data Exchange (ETDEWEB)

Hatlo, Andreas; Skaranger, Jon

1998-07-01

This presentation describes work done by an alliance of Kongsberg Offshore a.s. (KOS) and Aker Maritime (AMA). The alliance comprises the development and delivery of seafloor separation systems. The alliance was established as an answer to the identified need of seafloor separation and processing in the oil industry. In several fields on the Norwegian shelf there is defined a potential need for seafloor separation and pumping. The same trend can be seen in international waters as well, especially on deeper waters. Calculation of the economic potential for the relevant applications is based on a large number of variables, including both OPEX and CAPEX assessments. In order to be able to identify and analyse this potential in a better way, KOS and AMA are developing a tool for cost-benefit evaluations of such a seafloor separation and pumping system. PROSERNAT (France) and ALSTOME (UK) are important subcontractors in the development of seafloor separation and pumping systems. PROSERNAT will supply the separation tank and internal arrangement, ALSTOME will supply the power electronics for the distribution of seafloor power distribution.

Flow injection analysis in inductively coupled plasma spectrometry

International Nuclear Information System (INIS)

Rosias, Maria F.G.G.

1995-10-01

The main features of flow injection analysis (FIA) as contribution to the inductively coupled plasma (Icp) spectrometry are described. A systematic review of researches using the combined FIA-Icp and the benefits of this association are presented. Flow systems were proposed to perform on-line Icp solution management for multielemental determination by atomic emission spectrometry (Icp-AES) or mass spectrometry. The inclusion of on-line ion exchangers in flow systems for matrix separation and/or analyte preconcentration are presented. Together with those applications the new advent of instruments with facilities for multielement detection on flow injection signals are described. (author). 75 refs., 19 figs

1-(2-Formamidoethyl)-3-phenylurea functionalized activated carbon for selective solid-phase extraction and preconcentration of metal ions

Energy Technology Data Exchange (ETDEWEB)

Tu Zhifeng; He Qun [Department of Chemistry, Lanzhou University, Lanzhou 730000 (China); Chang, Xijun, E-mail: tuzhf07@lzu.cn [Department of Chemistry, Lanzhou University, Lanzhou 730000 (China); Hu Zheng; Gao Ru; Zhang Lina; Li Zhenhua [Department of Chemistry, Lanzhou University, Lanzhou 730000 (China)

2009-09-07

A novel method that utilizes 1-(2-formamidoethyl)-3-phenylurea-modified activated carbon (AC-1-(2-formamidoethyl)-3-phenylurea) as a solid-phase extractant has been developed for simultaneous preconcentration of trace Cr(III), Cu(II), Fe(III) and Pb(II) prior to the measurement by inductively coupled plasma atomic emission spectrometry (ICP-AES). Experimental conditions for effective adsorption of trace levels of Cr(III), Cu(II), Fe(III) and Pb(II) were optimized using batch and column procedures in detail. The optimum pH value for the separation of metal ions simultaneously on the new sorbent was 4. And the adsorbed metal ions could be completely eluted by using 2.0 mL 2.0 mol L{sup -1} HCl solution. Common coexisting ions did not interfere with the separation and determination of target metal ions. The maximum static adsorption capacity of the sorbent at optimum conditions was found to be 39.8, 39.9, 77.8 and 17.3 mg g{sup -1} for Cr(III), Cu(II), Fe(III) and Pb(II), respectively. The detection limits of the method were found to be 0.15, 0.41, 0.27 and 0.36 ng mL{sup -1} for Cr(III), Cu(II), Fe(III) and Pb(II), respectively. The relative standard deviation (RSD) of the method was lower than 4.0% (n = 8). The method was successfully applied for the preconcentration of trace Cr(III), Cu(II), Fe(III) and Pb(II) in natural and certified samples with satisfactory results.

1-(2-Formamidoethyl)-3-phenylurea functionalized activated carbon for selective solid-phase extraction and preconcentration of metal ions.

Science.gov (United States)

Tu, Zhifeng; He, Qun; Chang, Xijun; Hu, Zheng; Gao, Ru; Zhang, Lina; Li, Zhenhua

2009-09-07

A novel method that utilizes 1-(2-formamidoethyl)-3-phenylurea-modified activated carbon (AC-1-(2-formamidoethyl)-3-phenylurea) as a solid-phase extractant has been developed for simultaneous preconcentration of trace Cr(III), Cu(II), Fe(III) and Pb(II) prior to the measurement by inductively coupled plasma atomic emission spectrometry (ICP-AES). Experimental conditions for effective adsorption of trace levels of Cr(III), Cu(II), Fe(III) and Pb(II) were optimized using batch and column procedures in detail. The optimum pH value for the separation of metal ions simultaneously on the new sorbent was 4. And the adsorbed metal ions could be completely eluted by using 2.0 mL 2.0 mol L(-1) HCl solution. Common coexisting ions did not interfere with the separation and determination of target metal ions. The maximum static adsorption capacity of the sorbent at optimum conditions was found to be 39.8, 39.9, 77.8 and 17.3 mg g(-1) for Cr(III), Cu(II), Fe(III) and Pb(II), respectively. The detection limits of the method were found to be 0.15, 0.41, 0.27 and 0.36 ng mL(-1) for Cr(III), Cu(II), Fe(III) and Pb(II), respectively. The relative standard deviation (RSD) of the method was lower than 4.0% (n=8). The method was successfully applied for the preconcentration of trace Cr(III), Cu(II), Fe(III) and Pb(II) in natural and certified samples with satisfactory results.

1-(2-Formamidoethyl)-3-phenylurea functionalized activated carbon for selective solid-phase extraction and preconcentration of metal ions

International Nuclear Information System (INIS)

Tu Zhifeng; He Qun; Chang, Xijun; Hu Zheng; Gao Ru; Zhang Lina; Li Zhenhua

2009-01-01

A novel method that utilizes 1-(2-formamidoethyl)-3-phenylurea-modified activated carbon (AC-1-(2-formamidoethyl)-3-phenylurea) as a solid-phase extractant has been developed for simultaneous preconcentration of trace Cr(III), Cu(II), Fe(III) and Pb(II) prior to the measurement by inductively coupled plasma atomic emission spectrometry (ICP-AES). Experimental conditions for effective adsorption of trace levels of Cr(III), Cu(II), Fe(III) and Pb(II) were optimized using batch and column procedures in detail. The optimum pH value for the separation of metal ions simultaneously on the new sorbent was 4. And the adsorbed metal ions could be completely eluted by using 2.0 mL 2.0 mol L -1 HCl solution. Common coexisting ions did not interfere with the separation and determination of target metal ions. The maximum static adsorption capacity of the sorbent at optimum conditions was found to be 39.8, 39.9, 77.8 and 17.3 mg g -1 for Cr(III), Cu(II), Fe(III) and Pb(II), respectively. The detection limits of the method were found to be 0.15, 0.41, 0.27 and 0.36 ng mL -1 for Cr(III), Cu(II), Fe(III) and Pb(II), respectively. The relative standard deviation (RSD) of the method was lower than 4.0% (n = 8). The method was successfully applied for the preconcentration of trace Cr(III), Cu(II), Fe(III) and Pb(II) in natural and certified samples with satisfactory results.

The on-line mass separator SIRIUS at the Strasbourg Reactor

International Nuclear Information System (INIS)

Zirnheld, J.P.; Schutz, L.

1979-01-01

The SIRIUS facility was developed to isolate short-lived neutron-rich nuclides far from the line of β stability. The installation, which consists of a helium-jet fission-product transport system, an ion source, an accelerator and a deviation magnet, is described. The main characteristics of the whole system can be summarized as: (1) the fission-product transmission to the ion source is about 90%: (2) the mass resolving power is of the order of 500: (3) the total transit time between production and detection is less than 1s : (4) the overall efficiency of the system is on the average better than 5x10 -5 . The nuclei available for nuclear spectroscopic studies have been examined. With a neutron flux of 5x10 11 /cm 2 .s and 730 mg for the uranium target, about 50 neutron-rich rare-earth isotopes (many of which had previously been unavailable) are available with sufficient activities for nuclear spectroscopic studies. (Auth.)

Study on decay of 118Xe and 119Xe by means of mass-separator on-line with a synchrocyclotron

International Nuclear Information System (INIS)

Berlovich, Eh.E.; Batist, L.Kh.; Blinnikov, Yu.S.

1976-01-01

The decay of sup(118, 119)Xe isotopes has been investigated. An experimental device involving a mass-separator operating in line with a synchrocyclotron is briefly outlined. The elements to be investigated were isolated from a proton-irradiated target by the 'on-beam-chemistry' methods and transferred into the mass-separator ion source. The Xe separated ions are transported to detectors in an experimental ha ll. The energies and relative γ ray intensities of 118 Xe → 118 J and of 119 Xe → 119 J decays ar presented. The error of the γ ray energy determination does not exceed 0.6 keV. Obtained are the periods of half-life: for 118 Xe - (3.8+-0.9) min, for 119 Xe - (5.8+-0.3) min. The decay scheme for 119 Xe is made up. The scheme of 119 Xe levels is well inscribed into the general systematics of the J odd isotope levels. On the basis of obtained and known data the spin values are described to the 119 J levels

Analysis of Trace Pharmaceuticals and Related Compounds in Municipal Wastewaters by Preconcentration, Chromatography, Derivatization, and Separation Methods

Directory of Open Access Journals (Sweden)

Petra Camilla Lindholm

2014-05-01

Full Text Available A significant portion of pharmaceuticals and other organic chemicals consumed by people and animals are released into municipal wastewater treatment plants. Most of them are degraded during the wastewater treatment processes, but some of them degrade only partially and may be widely transported and dispersed into the aquatic environment. This is why efficient and fast analytical methods are needed for detection of organic compounds in wastewaters at trace levels. Because wastewaters often consist of complex matrices and high-molecular mass materials, e.g., lignocellulosic biomass, which may bring challenges to the sample preparation procedures, efficient pre-concentration methods such as solid phase extraction (SPE solid phase microextraction (SPME, or single drop microextraction (SDME are needed. The most common analysis methods are gas chromatography (GC and liquid chromatography (LC coupled with tandem mass spectrometry (MS/MS. The aim of this review is to give an overview of chromatographic and spectroscopic methods when characterizing low- and medium-molecular weight organic pollutants, mainly focusing on pharmaceuticals, biocides, and personal care products in environmental matrices.

Determination of platinum group metals by ICP-AES in environmental samples after preconcentration

International Nuclear Information System (INIS)

Vlasankova, R.; Sommer, L.

1999-01-01

Platinum group metal (PGM) may have toxic properties and their presence in the environment represent danger for human health. With the introduction of automobile catalytic converters containing PGM, the emission of these noble metals into atmosphere has increased. Platinum, palladium and rhodium are used in this catalytic converters to decrease toxic emissions of carbon monoxide, unburnt hydrocarbons and nitrogen oxides in vehicles exhaust gases. These catalysts are mobile sources of PGM into the environment. Thus, increased platinum concentrations have been found in various objects of environment because of the massive introduction of such catalytic converters are present. The preconcentration and separation of PGM and their determination by ICP-AES in environmental samples are described

Penicillium digitatum immobilized on pumice stone as a new solid phase extractor for preconcentration and/or separation of trace metals in environmental samples

Energy Technology Data Exchange (ETDEWEB)

Baytak, Sitki [Department of Chemistry, Faculty of Science and Arts, Harran University, 63100 Sanliurfa (Turkey); Kenduezler, Erdal [Department of Primary Education, Faculty of Education, Ahi Evran University, 40100 Kirsehir (Turkey); Tuerker, Ali Rehber [Department of Chemistry, Faculty of Science and Arts, Gazi University, 06500 Ankara (Turkey)], E-mail: aturker@gazi.edu.tr; Goek, Nuray [Department of Environmental Engineering, Faculty of Engineering, Harran University, 63000 Sanliurfa (Turkey)

2008-05-30

This study presents a column solid phase extraction procedure based on column biosorption of Cu(II), Zn(II) and Pb(II) ions on Penicillium digitatum immobilized on pumice stone. The analytes were determined by flame atomic absorption spectrometry (FAAS). The optimum conditions such as: pH values, amount of solid phase, elution solution and flow rate of sample solution were evaluated for the quantitative recovery of the analytes. The effect of interfering ions on the recovery of the analytes has also been investigated. The recoveries of copper, zinc and lead under the optimum conditions were found to be 97 {+-} 2, 98 {+-} 2 and 98 {+-} 2%, respectively, at 95% confidence level. For the analytes, 50-fold preconcentration was obtained. The analytical detection limits for Cu(II), Zn(II) and Pb(II) were 1.8, 1.3 and 5.8 ng mL{sup -1}, respectively. The proposed procedure was applied for the determination of copper, zinc and lead in dam water, waste water, spring water, parsley and carrot. The accuracy of the procedure was checked by determining copper, zinc and lead in standard reference tea samples (GBW-07605)

Penicillium digitatum immobilized on pumice stone as a new solid phase extractor for preconcentration and/or separation of trace metals in environmental samples

International Nuclear Information System (INIS)

Baytak, Sitki; Kenduezler, Erdal; Tuerker, Ali Rehber; Goek, Nuray

2008-01-01

This study presents a column solid phase extraction procedure based on column biosorption of Cu(II), Zn(II) and Pb(II) ions on Penicillium digitatum immobilized on pumice stone. The analytes were determined by flame atomic absorption spectrometry (FAAS). The optimum conditions such as: pH values, amount of solid phase, elution solution and flow rate of sample solution were evaluated for the quantitative recovery of the analytes. The effect of interfering ions on the recovery of the analytes has also been investigated. The recoveries of copper, zinc and lead under the optimum conditions were found to be 97 ± 2, 98 ± 2 and 98 ± 2%, respectively, at 95% confidence level. For the analytes, 50-fold preconcentration was obtained. The analytical detection limits for Cu(II), Zn(II) and Pb(II) were 1.8, 1.3 and 5.8 ng mL -1 , respectively. The proposed procedure was applied for the determination of copper, zinc and lead in dam water, waste water, spring water, parsley and carrot. The accuracy of the procedure was checked by determining copper, zinc and lead in standard reference tea samples (GBW-07605)

Project development and commercialization of on-line analysis systems

International Nuclear Information System (INIS)

Watt, J.S.

1997-01-01

A project team first in the Australian Atomic Energy Commission (AAEC) and since 1982 in CSIRO has developed many on-line analysis systems for the mineral and energy industries. The development of these projects has followed a common pattern of laboratory R and D, field trials, commercialisation and technology transfer. This successful pattern is illustrated using examples of the development of systems for the on-line analysis of mineral slurries, for determination of the ash content of coal on conveyors, and for determination of the flow rates of oil, water and gas in pipelines. The first two systems are licensed to Australian companies, Amdel Ltd and Mineral Control Instrumentation Ltd. Both systems are used by industry worldwide, and are the market leaders for radioisotope gauges in their application field. The third system, the multiphase flow meter, was licensed in 1997 to Kvaerner FSSL Ltd of Aberdeen. This meter has even greater potential than the other two systems for economic benefit from its used and for numbers of installations. The on-line analysis systems have been developed to increase the productivity of the Australian mineral and energy industries, and to provide economic benefit to Australia. The economic benefit sought is predominantly improved process control based on use of the instrument, rather than from its sale. Sales of instruments are significant, however, with about A$80 million from the analysis systems and their derivatives since the 1970s. Some of the issues associated with the development of the on-line analysis system are outlined

Production of chemically reactive radioactive ion beams through on-line separation; Production de faisceaux d'ions radioactifs chimiquement reactifs par separation en ligne

Energy Technology Data Exchange (ETDEWEB)

Joinet, A

2003-10-01

The ISOL (isotope separation on line) allows the production of secondary radioactive ion beams through spallation or fragmentation or fission reactions that take place in a thick target bombarded by a high intensity primary beam. The challenge is to increase the intensity and purity of the radioactive beam. The optimization of the system target/source requires the right choice of material for the target by taking into account the stability of the material, its reactivity and the ionization method used. The target is an essential part of the system because radioactive elements are generated in it and are released more or less quickly. Tests have been made in order to select the best fitted material for the release of S, Se, Te, Ge and Sn. Materials tested as target filling are: ZrO{sub 2}, Nb, Ti, V,TiO{sub 2}, CeO{sub x}, ThO{sub 2}, C, ZrC{sub 4} and VC). Other molecules such as: COSe, COS, SeS, COTe, GeS, SiS, SnS have been studied to ease the extraction of recoil nuclei (Se, S, Te, Ge and Sn) produced inside the target.

A nanocomposite disk prepared from reduced graphene oxide and gold nanoparticles for the preconcentration of heterocyclic aromatic amines prior to their determination by HPLC

International Nuclear Information System (INIS)

Tan, Connieal; Wang, Yiru; Deng, Zhuo; Xu, Na; Song, Xinhong; Liu, Haihong; Rong, Mingcong; Chen, Xi

2014-01-01

We report on a preconcentration disk for the determination of trace amounts of heterocyclic aromatic amines (HAAs) in the groups of quinoline and quinoxaline congeners as possible human carcinogens. The disk is based on nanocomposite (NC) prepared from graphene oxide as the precursor and from gold nanoparticles that act as building blocks to form a three-dimensional NC. If deposited in the sampling valve of a HPLC system, the material displays excellent extraction capability for HAAs owing to its large surface and π-π stacking interaction. Following an optimization of the extraction parameters, the method was successfully applied to the simultaneous determination of polar HAAs in meat samples with detection limit of 0.09 to 0.16 ng g −1 and recoveries of 69.5 to 122.7 %. The disk was used in more than 150 subsequent preconcentration cycles without obvious loss of the absorption capability. The results reveal that this new NC represents an excellent sorbent for purposes of preconcentration. (author)

A versatile, refrigerant- and cryogen-free cryofocusing–thermodesorption unit for preconcentration of traces gases in air

Directory of Open Access Journals (Sweden)

F. Obersteiner

2016-10-01

Full Text Available We present a compact and versatile cryofocusing–thermodesorption unit, which we developed for quantitative analysis of halogenated trace gases in ambient air. Possible applications include aircraft-based in situ measurements, in situ monitoring and laboratory operation for the analysis of flask samples. Analytes are trapped on adsorptive material cooled by a Stirling cooler to low temperatures (e.g. −80 °C and subsequently desorbed by rapid heating of the adsorptive material (e.g. +200 °C. The set-up involves neither the exchange of adsorption tubes nor any further condensation or refocusing steps. No moving parts are used that would require vacuum insulation. This allows for a simple and robust design. Reliable operation is ensured by the Stirling cooler, which neither contains a liquid refrigerant nor requires refilling a cryogen. At the same time, it allows for significantly lower adsorption temperatures compared to commonly used Peltier elements. We use gas chromatography – mass spectrometry (GC–MS for separation and detection of the preconcentrated analytes after splitless injection. A substance boiling point range of approximately −80 to +150 °C and a substance mixing ratio range of less than 1 ppt (pmol mol−1 to more than 500 ppt in preconcentrated sample volumes of 0.1 to 10 L of ambient air is covered, depending on the application and its analytical demands. We present the instrumental design of the preconcentration unit and demonstrate capabilities and performance through the examination of analyte breakthrough during adsorption, repeatability of desorption and analyte residues in blank tests. Examples of application are taken from the analysis of flask samples collected at Mace Head Atmospheric Research Station in Ireland using our laboratory GC–MS instruments and by data obtained during a research flight with our in situ aircraft instrument GhOST-MS (Gas chromatograph for the Observation of Tracers �

Simultaneous preconcentration of Cu, Fe and Pb as methylthymol blue complexes on naphthalene adsorbent and flame atomic absorption determination

International Nuclear Information System (INIS)

Pourreza, Nahid; Hoveizavi, Reza

2005-01-01

A simultaneous preconcentration method was developed for determination of trace amounts of Cu, Fe and Pb by atomic absorption spectrometry. The method is based on the retention of their methylthymol blue complexes by naphthalene methyltrioctyl ammonium chloride adsorbent in a column. The adsorbed metal complexes were eluted from the column with nitric acid and Cu, Fe and Pb were determined by flame atomic absorption spectrometry. Several parameters such as pH of the sample solution, ligand concentration, volume of the sample and the amount of methyltrioctyl ammonium chloride loaded on naphthalene were evaluated. The effect of diverse ions on the preconcentration was also investigated. A preconcentration factor of up to 100 or more can easily be achieved depending on the volume of the sample taken. The calibration graphs were obtained in the range of 5-40, 10-100 and 10-200 ng ml -1 for Cu, Fe and Pb in the initial solution, respectively, when using 500 ml of the solution. The detection limit based on three standard deviations of the blank was 0.54, 3.1, and 4.5 ng ml -1 for Cu, Fe and Pb, respectively. The relative standard deviations (R.S.D.) of 0.62-1.4% for Cu, 1.9-3.4% for Fe and 1.0-2.2% for Pb were obtained. The method was applied to the determination of Cu, Fe and Pb in river and wastewater samples

Flotation-separation and ICP-AES determination of ultra trace amounts of copper, cadmium, nickel and cobalt using 2-aminocyclopentene-1-dithiocarboxylic acid.

Science.gov (United States)

Shamsipur, Mojtaba; Hashemi, Omid Reza; Safavi, Afsaneh

2005-09-01

A rapid flotation method for separation and enrichment of ultra trace amounts of copper(II), cadmium(II), nickel(II) and cobalt(II) ions from water samples is established. At pH 6.5 and with sodium dodecylsulfate used as a foaming reagent, Cu2+, Cd2+, Ni2+ and Co2+ were separated simultaneously with 2-aminocyclopentene-1-dithiocarboxylic acid (ACDA) added to 1 l of aqueous solution. The proposed procedure of preconcentration is applied prior to the determination of these four analytes using inductivity coupled plasma-atomic emission spectrometry (ICP-AES). The effects of pH, concentration of ACDA, applicability of different surfactants and foreign ions on the separation efficiency were investigated. The preconcentration factor of the method is 1000 and the detection limits of copper(II), cadmium(II), nickel(II) and cobalt(II) ions are 0.078, 0.075, 0.072 and 0.080 ng ml(-1), respectively.

SPHERE DAQ and off-line systems: implementation based on the qdpb system

International Nuclear Information System (INIS)

Isupov, A.Yu.

2003-01-01

Design of the on-line data acquisition (DAQ) system for the SPHERE setup (LHE, JINR) is described. SPHERE DAQ is based on the qdpb (Data Processing with Branchpoints) system and configurable experimental data and CAMAC hardware representations. Implementation of the DAQ and off-line program code, depending on the SPHERE setup's hardware layout and experimental data contents, is explained as well as software modules specific for such implementation

Binary electrokinetic separation of target DNA from background DNA primers.

Energy Technology Data Exchange (ETDEWEB)

James, Conrad D.; Derzon, Mark Steven

2005-10-01

This report contains the summary of LDRD project 91312, titled ''Binary Electrokinetic Separation of Target DNA from Background DNA Primers''. This work is the first product of a collaboration with Columbia University and the Northeast BioDefense Center of Excellence. In conjunction with Ian Lipkin's lab, we are developing a technique to reduce false positive events, due to the detection of unhybridized reporter molecules, in a sensitive and multiplexed detection scheme for nucleic acids developed by the Lipkin lab. This is the most significant problem in the operation of their capability. As they are developing the tools for rapidly detecting the entire panel of hemorrhagic fevers this technology will immediately serve an important national need. The goal of this work was to attempt to separate nucleic acid from a preprocessed sample. We demonstrated the preconcentration of kilobase-pair length double-stranded DNA targets, and observed little preconcentration of 60 base-pair length single-stranded DNA probes. These objectives were accomplished in microdevice formats that are compatible with larger detection systems for sample pre-processing. Combined with Columbia's expertise, this technology would enable a unique, fast, and potentially compact method for detecting/identifying genetically-modified organisms and multiplexed rapid nucleic acid identification. Another competing approach is the DARPA funded IRIS Pharmaceutical TIGER platform which requires many hours for operation, and an 800k$ piece of equipment that fills a room. The Columbia/SNL system could provide a result in 30 minutes, at the cost of a few thousand dollars for the platform, and would be the size of a shoebox or smaller.

Preconcentration and Extraction of Copper ion on Activated Carbon using α-Benzoinoxime and Pyrimidin 2-Thiole

International Nuclear Information System (INIS)

Ghaedi, M.; Mortazavi, K.; Janbezar, M.; Parham, H.

2006-01-01

Activated carbon modified methods were used for preconcentration and determination of copper in some real sample by flame atomic absorption spectrometry. The copper was adsorbed quantitatively on activated carbon due to their complexation with α-benzoinoxime and pyrimidin 2-thiole. The adsorbed copper on solid phase was eluted quantitatively using nitric acid. The important parameters such as pH, amount of carrier, flow rate, amount of activated carbon and type and concentration of eluting agent for obtaining maximum recovery was optimized. The methods based on α- benzoinoxime and pyrimidin 2-thiole at optimum conditions is linear over concentration range of 0.05-1.3 ug mL and 0.06-1.2 ug mL of copper with correlation coefficient of 0.9997 and 0.9994 and both detection limit of 1.2 ngmL, respectively. The preconcentration leads to enrichment factor of 200 and 240 and break through volume of 1200 mL for methods based on α- benzoinoxime and pyrimidin 2-thiole, respectively. The methods have good tolerance limit of interfering ion and selectivity that has been successfully applied for determination of copper content in real sample such as blood, wastewater and river sample. (author)

The determination of some heavy metals in food samples by flame atomic absorption spectrometry after their separation-preconcentration on bis salicyl aldehyde, 1,3 propan diimine (BSPDI) loaded on activated carbon

International Nuclear Information System (INIS)

Ghaedi, M.; Shokrollahi, A.; Kianfar, A.H.; Mirsadeghi, A.S.; Pourfarokhi, A.; Soylak, M.

2008-01-01

A sensitive and simple method for the simultaneous preconcentration of Cr 3+ , Fe 3+ , Cu 2+ , Ni 2+ , Co 2+ and Zn 2+ in real samples has been reported. The method is based on the adsorption of analytes on bis salicyl aldehyde, 1,3 propan diimine (BSPDI) loaded on activated carbon. The adsorbed metals on modified activated carbon were eluted using 8 mL of 2 mol L -1 nitric acid in acetone or 10 mL of 4 mol L -1 HNO 3 . The influences of the analytical parameters including pH and sample volume were investigated. The effects of matrix ions on the retentions of the analytes were also examined. The recoveries of analytes were generally quantitative. The method has been successfully applied for these metals content evaluation in some food samples

Enhancement of the conductivity detection signal in capillary electrophoresis systems using neutral cyclodextrins as sweeping agents.

Science.gov (United States)

Boublík, Milan; Riesová, Martina; Dubský, Pavel; Gaš, Bohuslav

2018-06-01

Conductivity detection is a universal detection technique often encountered in electrophoretic separation systems, especially in modern chip-electrophoresis based devices. On the other hand, it is sparsely combined with another contemporary trend of enhancing limits of detection by means of various preconcentration strategies. This can be attributed to the fact that a preconcentration experimental setup usually brings about disturbances in a conductivity baseline. Sweeping with a neutral sweeping agent seems a good candidate for overcoming this problem. A neutral sweeping agent does not hinder the conductivity detection while a charged analyte may preconcentrate on its boundary due to a decrease in its effective mobility. This study investigates such sweeping systems theoretically, by means of computer simulations, and experimentally. A formula is provided for the reliable estimation of the preconcentration factor. Additionally, it is demonstrated that the conductivity signal can significantly benefit from slowing down the analyte and thus the overall signal enhancement can easily overweight amplification caused solely by the sweeping process. The overall enhancement factor can be deduced a priori from the linearized theory of electrophoresis implemented in the PeakMaster freeware. Sweeping by neutral cyclodextrin is demonstrated on an amplification of a conductivity signal of flurbiprofen in a real drug sample. Finally, a possible formation of unexpected system peaks in systems with a neutral sweeping agent is revealed by the computer simulation and confirmed experimentally. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Chemically-modified activated carbon with ethylenediamine for selective solid-phase extraction and preconcentration of metal ions.

Science.gov (United States)

Li, Zhenhua; Chang, Xijun; Zou, Xiaojun; Zhu, Xiangbing; Nie, Rong; Hu, Zheng; Li, Ruijun

2009-01-26

A new method that utilizes ethylenediamine-modified activated carbon (AC-EDA) as a solid-phase extractant has been developed for simultaneous preconcentration of trace Cr(III), Fe(III), Hg(II) and Pb(II) prior to the measurement by inductively coupled plasma optical emission spectrometry (ICP-OES). The new sorbent was prepared by oxidative surface modification. Experimental conditions for effective adsorption of trace levels of Cr(III), Fe(III), Hg(II) and Pb(II) were optimized with respect to different experimental parameters using batch and column procedures in detail. The optimum pH value for the separation of metal ions simultaneously on the new sorbent was 4.0. Complete elution of absorbed metal ions from the sorbent surface was carried out using 3.0 mL of 2% (%w/w) thiourea and 0.5 mol L(-1) HCl solution. Common coexisting ions did not interfere with the separation and determination of target metal ions. The maximum static adsorption capacity of the sorbent at optimum conditions was found to be 39.4, 28.9, 60.5 and 49.9 mg g(-1) for Cr(III), Fe(III), Hg(II) and Pb(II), respectively. The time for 94% adsorption of target metal ions was less than 2 min. The detection limits of the method was found to be 0.28, 0.22, 0.09 and 0.17 ng mL(-1) for Cr(III), Fe(III), Hg(II) and Pb(II), respectively. The precision (R.S.D.) of the method was lower 4.0% (n=8). The prepared sorbent as solid-phase extractant was successfully applied for the preconcentration of trace Cr(III), Fe(III), Hg(II) and Pb(II) in natural and certified samples with satisfactory results.

Multi-Mode Operation for On-line Uninterruptible Power Supply System

DEFF Research Database (Denmark)

Lu, Jinghang; Savaghebi, Mehdi; Golestan, Saeed

2018-01-01

To enhance the robustness and disturbance rejection ability of an on-line uninterruptible power supply (UPS) system, an Internal Model Control (IMC)-based DC-link voltage regulation method is proposed in this paper. Furthermore, the multi-mode operations of the on-line UPS system are investigated...

An Improved CO2 Separation and Purification System Based on Cryogenic Separation and Distillation Theory

Directory of Open Access Journals (Sweden)

Gang Xu

2014-05-01

Full Text Available In this study, an improved CO2 separation and purification system is proposed based on in-depth analyses of cryogenic separation and distillation theory as well as the phase transition characteristics of gas mixtures containing CO2. Multi-stage compression, refrigeration, and separation are adopted to separate the majority of the CO2 from the gas mixture with relatively low energy penalty and high purity. Subsequently, the separated crude liquid CO2 is distilled under high pressure and near ambient temperature conditions so that low energy penalty purification is achieved. Simulation results indicate that the specific energy consumption for CO2 capture is only 0.425 MJ/kgCO2 with 99.9% CO2 purity for the product. Techno-economic analysis shows that the total plant investment is relatively low. Given its technical maturity and great potential in large-scale production, compared to conventional MEA and SelexolTM absorption methods, the cost of CO2 capture of the proposed system is reduced by 57.2% and 45.9%, respectively. The result of this study can serve as a novel approach to recovering CO2 from high CO2 concentration gas mixtures.

Parameter study on Japanese proposal of ITER hydrogen isotope separation system

International Nuclear Information System (INIS)

Yoshida, Hiroshi; Enoeda, Mikio; Tanaka, Shigeru; Ohokawa, Yoshinao; Ohara, Atsushi; Nagakura, Masaaki; Naito, Taisei; Nagashima, Kazuhiro.

1991-01-01

As part of Japanese design contribution in the ITER activity, conceptual design of an entire ITER tritium system and their safety analysis have been carried out through the three-year period since 1988. The tritium system includes the following subsystems; - Fuelling (gas puffing and pellet injection) subsystem, - Torus vacuum pumping subsystem, - Plasma exhaust gas purification subsystem, - Hydrogen isotope separation subsystem, - NBI gas processing subsystem, - Blanket tritium recovery subsystem, - Tritiated water processing subsystem, - Tritium safety subsystem. Hydrogen isotope separation system is a key subsystem in the ITER tritium system because it is connected to all above subsystems. This report describes an analytical study on the Japanese concept of hydrogen isotope separation system. (author)

On-line analyzers to distributed control system linking

Energy Technology Data Exchange (ETDEWEB)

Peterson, S.F.; Buchanan, B.R.; Sanders, M.A.

1990-01-01

The Analytical Development Section (ADS) of the Savannah River Laboratory is developing on-line analyzers to monitor various site processes. Data from some of the on-line analyzers (OLA's) will be used for process control by distributed control systems (DCS's) such as the Fisher PRoVOX. A problem in the past has been an efficient and cost effective way to get analyzer data onto the DCS data highway. ADS is developing a system to accomplish the linking of OLA's to PRoVOX DCS's. The system will be described, and results of operation in a research and development environment given. Plans for the installation in the production environment will be discussed.

The fire assay preconcentration of the platinum group elements for the neutron activation analysis of geological material

International Nuclear Information System (INIS)

Parry, S.J.

1994-01-01

This paper describes the work that has been carried out using neutron activation analysis (NAA) to develop a rapid and reliable method for the determination of the platinum group elements (PGE: Pt, Pd, Ir, Ru, Rh, and Os) and Au in geological, environmental and industrial samples. The method is based on the now established method of preconcentration with fire assay, followed by NAA of the separated PGE and Au. Recent developments have seen improvements in the technique to eliminate losses due to dissolution procedures, and complete recovery of the elements prior to analysis. The method is now being used to validate inductively coupled plasma-mass spectroscopy methods for analysis of the PGE

Magnetic separation in microfluidic systems

DEFF Research Database (Denmark)

Smistrup, Kristian

2007-01-01

to facilitate real-time monitoring of the experiments. The set-up and experimental protocol are described in detail. Results are presented for ’active’ magnetic bead separators, where on-chip microfabricated electromagnets supply the magnetic field and field gradients necessary for magnetic bead separation....... It is shown conceptually how such a system can be applied for parallel biochemical processing in a microfluidic system. ’Passive’ magnetic separators are presented, where on-chip soft magnetic elements are magnetized by an external magnetic field and create strong magnetic fields and gradients inside...

Electrochromatography on acrylate-based monolith in cyclic olefin copolymer microchip: a cost-effective and easy-to-use technology.

Science.gov (United States)

Ladner, Yoann; Crétier, Gérard; Faure, Karine

2012-10-01

This article shows that there is great interest in using an electrochromatographic microchip made of hexyl acrylate (HA) based porous monolith cast within the channel of a cyclic olefin copolymer (COC) device. The monolith is simultaneously in situ synthesized and anchored to the inner walls of the channel in less than 10 min. By appropriate choice of light intensity used during the synthesis, the separation efficiency obtained for nonpolar solutes such as polycyclic aromatic hydrocarbons (PAH) is increased up to 250 000 plates/m. The performance of this HA-filled COC microchip was investigated for a wide range of analytes of varying nature. The reversed-phase separation of four aflatoxins is obtained in less than 2 min. The baseline separation of a mixture of neurotransmitters including six amino acids and two catecholamines is possible thanks to the superimposition of the differences in electrophoretic mobility on the chromatographic process. The durability of the system at pH 13 allows the separation of five biogenic amines and the quantitative determination of two of them in numerous wine samples. The feasibility of on-line preconcentration is also demonstrated. Hydrophilic surface modification of COC channel via UV-photografting with poly(ethylene glycol) methacrylate (PEGMA) before in situ synthesis of HA, is necessary to reduce the adsorption of very hydrophobic solutes such as PAH during enrichment. The detection limit of fluoranthene is decreased down to less than 1 ppb with a preconcentration of 4.5 h on the HA-filled PEGMA functionalized COC microchip. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous determination of trace amounts of metals by high-performance liquid chromatography after preconcentration with adsorption on chlorotrifluoroethylene polymer as their hexamethylenedithiocarbamate complexes

International Nuclear Information System (INIS)

Shijo, Yoshio; Yoshida, Hideaki; Uehara, Nobuo; Kitamura, Teruo; Yoshimoto, Eiji.

1996-01-01

A method for the simultaneous determination of Bi, Cd, Cu, In, Ni and Pb by high-performance liquid chromatography is presented. These metals are preconcentrated on poly(chlorotrifluoroethylene) resin particles as their hexamethylenedithiocarbamate (HMDC) complexes, and eluted with dimethyl sulfoxide, followed by HPLC separation and determination using an ODS column. The conditions for the adsorption of metal-HMDC complexes, such as the pH, HMDC concentration, amount of the resin particles and elution times with dimethyl sulfoxide, are discussed. The resulting solution is suitable for injection into reversed-phase HPLC. The detection limits for the metals were found to be at sub μgl -1 levels. The application of this principle to the trace analysis of Bi, Cd, Cu, In, Ni and Pb in high-purity aluminum is demonstrated. (author)

A study of some neutron-rich isotopes of lanthanum, cerium and praseodymium by means of fast chemical on-line separation technique SISAK

International Nuclear Information System (INIS)

Skarnemark, G.

1977-01-01

The fast on-line chemical separation technique SISAK has been utilized to study the decay properties of neutron-rich isotopes of La, Ce and Pr. The results include partial decay schemes and γ-ray intensity data for 14 min 143 La, 42 s 144 La, 25 s 145 La, 9 s 146 La, 3 min 145 Ce, 14 min 146 Ce, 56 s 147 Ce, 50 s 148 Ce, 12 min 147 Pr, 2 min 148 Pr, 3 min 149 Pr and 6 s 150 Pr. Half-lives and γ-ray energies are reported for the previously unknown nuclides 147 La (Tsub(1/2) = 2.2 s), 148 La (Tsub(1/2) approximately 1 s), 149 Ce (Tsub(1/2) = 5.7 s) and 150 Ce (Tsub(1/2) = 4.1 s). The nuclides were formed in thermal neutron-induced fission of 235 U. The fission products were transferred to the SISAK system via a gas jet recoil transportation (GJRT) system. The combination of the GJRT system with SISAK is discussed, as well as the chemical separation systems used for the isolation of La, Ce and Pr. The appendices I - IX contain previously published material which is included in the thesis. (Auth.)

A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry.

Science.gov (United States)

Tuzen, Mustafa; Soylak, Mustafa; Citak, Demirhan; Ferreira, Hadla S; Korn, Maria G A; Bezerra, Marcos A

2009-03-15

A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L(-1) nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 microg L(-1), respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 microg L(-1). The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish.

A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Tuzen, Mustafa; Soylak, Mustafa; Citak, Demirhan; Ferreira, Hadla S.; Korn, Maria G.A.; Bezerra, Marcos A.

2009-01-01

A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L -1 nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 μg L -1 , respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 μg L -1 . The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish

R and D study on on-line criticality surveillance system (V)

International Nuclear Information System (INIS)

Yamada, Sumasu

2001-02-01

In view of necessity and importance of criticality surveillance systems for ensuring the safety of nuclear fuel manufacturing and reprocessing plants, 5-year basic studies and 4 year R and D studies on an on-line criticality surveillance system were carried out since 1991. This report is a summary of these series of studies. Noticing that the signal from a neutron detector is random in principle, these series of studies aimed to accumulate knowledge for developing an inexpensive criticality surveillance system with quick response based on the Auto-Regressive Moving Average (ARMA) model identification algorithm. During five-year basic studies on criticality surveillance system since 1991, we obtained knowledge required for developing a criticality surveillance system based on the ARMA model identification algorithm through 1) studies on recursive ARMA model identification algorithms most appropriate for estimating subcriticality form time series data under a steady state condition, 2) studies on pre-processing of signal from neutron detectors, 3) developing a new recursive ARMA model identification algorithm with small time delay to estimate time-dependent subcriticality, 4) proposing a basic concept for the elements required for an on-line criticality surveillance system, and 5) numerical analysis of data from the DCA experiments. During next four-year R and D studies on a criticality surveillance system since 1996, we 1) proposed modules required for a no-line criticality surveillance system, 2) revealed effectiveness of a adaptive digital filter (ADF) algorithm, as an important redundancy to the recursive ARMA model identification algorithm to be used in the signal processing module through numerical analysis of real data, 3) proposed a module of the Feynman-α method over γ ray signal and a fast signal processing module for γ ray signal, 4) developed a line-noise removal filter(Notch filter) and revealed its effectiveness for the DCA data corrupted with power-line

The Bochum on-line data acquisition system

International Nuclear Information System (INIS)

Paul, H.J.; Freiesleben, H.

1986-01-01

We describe an on-line data acquisition system based on a PDP 11 computer with CAMAC hardware. The software fully exploits the real-time features of the RSX-11M operating system. The basic characteristics of the program package, mainly written in FORTRAN 77, are: multitasking, shared common blocks, dynamical access to CAMAC hardware and data, and command orientated user interface. The system is particularly tailored for data acquisition in list mode of up to 64 parameters. (orig.)

The use of safeguards data for process monitoring in the Advanced Test Line for Actinide Separations

International Nuclear Information System (INIS)

Barnes, J.W.; Yarbro, S.L.

1987-01-01

Los Alamos is constructing an integrated process monitoring/materials control and accounting (PM/MC and A) system in the Advanced Testing Line for Actinide Separations (ATLAS) at the Los Alamos Plutonium Facility. The ATLAS will test and demonstrate new methods for aqueous processing of plutonium. The ATLAS will also develop, test, and demonstrate the concepts for integrated process monitoring/materials control and accounting. We describe how this integrated PM/MC and A system will function and provide benefits to both process research and materials accounting personnel

Development of a novel mixed hemimicelles dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene for the separation and preconcentration of fluoxetine in different matrices before its determination by fiber optic linear array spectrophotometry and mode-mismatched thermal lens spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Kazemi, Elahe; Haji Shabani, Ali Mohammad [Department of Chemistry, Yazd University, Safaieh, 89195-741, Yazd (Iran, Islamic Republic of); Dadfarnia, Shayessteh, E-mail: sdadfarnia@yazd.ac.ir [Department of Chemistry, Yazd University, Safaieh, 89195-741, Yazd (Iran, Islamic Republic of); Abbasi, Amir [Department of Physics, Yazd University, Safaieh, 89195-741, Yazd (Iran, Islamic Republic of); Rashidian Vaziri, Mohammad Reza [Laser and Optics Research School, 14155-1339, Tehran (Iran, Islamic Republic of); Behjat, Abbas [Department of Physics, Yazd University, Safaieh, 89195-741, Yazd (Iran, Islamic Republic of)

2016-01-28

This study aims at developing a novel, sensitive, fast, simple and convenient method for separation and preconcentration of trace amounts of fluoxetine before its spectrophotometric determination. The method is based on combination of magnetic mixed hemimicelles solid phase extraction and dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene as a sorbent. The magnetic graphene was synthesized by a simple coprecipitation method and characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). The retained analyte was eluted using a 100 μL mixture of methanol/acetic acid (9:1) and converted into fluoxetine-β-cyclodextrin inclusion complex. The analyte was then quantified by fiber optic linear array spectrophotometry as well as mode-mismatched thermal lens spectroscopy (TLS). The factors affecting the separation, preconcentration and determination of fluoxetine were investigated and optimized. With a 50 mL sample and under optimized conditions using the spectrophotometry technique, the method exhibited a linear dynamic range of 0.4–60.0 μg L{sup −1}, a detection limit of 0.21 μg L{sup −1}, an enrichment factor of 167, and a relative standard deviation of 2.1% and 3.8% (n = 6) at 60 μg L{sup −1} level of fluoxetine for intra- and inter-day analyses, respectively. However, with thermal lens spectrometry and a sample volume of 10 mL, the method exhibited a linear dynamic range of 0.05–300 μg L{sup −1}, a detection limit of 0.016 μg L{sup −1} and a relative standard deviation of 3.8% and 5.6% (n = 6) at 60 μg L{sup −1} level of fluoxetine for intra- and inter-day analyses, respectively. The method was successfully applied to determine fluoxetine in pharmaceutical formulation, human urine and environmental water samples. - Graphical abstract: A novel, sensitive, fast, simple and convenient mixed hemimicelles

Development of a novel mixed hemimicelles dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene for the separation and preconcentration of fluoxetine in different matrices before its determination by fiber optic linear array spectrophotometry and mode-mismatched thermal lens spectroscopy

International Nuclear Information System (INIS)

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

2016-01-01

This study aims at developing a novel, sensitive, fast, simple and convenient method for separation and preconcentration of trace amounts of fluoxetine before its spectrophotometric determination. The method is based on combination of magnetic mixed hemimicelles solid phase extraction and dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene as a sorbent. The magnetic graphene was synthesized by a simple coprecipitation method and characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). The retained analyte was eluted using a 100 μL mixture of methanol/acetic acid (9:1) and converted into fluoxetine-β-cyclodextrin inclusion complex. The analyte was then quantified by fiber optic linear array spectrophotometry as well as mode-mismatched thermal lens spectroscopy (TLS). The factors affecting the separation, preconcentration and determination of fluoxetine were investigated and optimized. With a 50 mL sample and under optimized conditions using the spectrophotometry technique, the method exhibited a linear dynamic range of 0.4–60.0 μg L"−"1, a detection limit of 0.21 μg L"−"1, an enrichment factor of 167, and a relative standard deviation of 2.1% and 3.8% (n = 6) at 60 μg L"−"1 level of fluoxetine for intra- and inter-day analyses, respectively. However, with thermal lens spectrometry and a sample volume of 10 mL, the method exhibited a linear dynamic range of 0.05–300 μg L"−"1, a detection limit of 0.016 μg L"−"1 and a relative standard deviation of 3.8% and 5.6% (n = 6) at 60 μg L"−"1 level of fluoxetine for intra- and inter-day analyses, respectively. The method was successfully applied to determine fluoxetine in pharmaceutical formulation, human urine and environmental water samples. - Graphical abstract: A novel, sensitive, fast, simple and convenient mixed hemimicelles dispersive micro solid

Development of a relatively cheap and simple automated separation system for a routine separation procedure based on extraction chromatography

International Nuclear Information System (INIS)

Petro Zoriy; Reinhold Flucht; Mechthild Burow; Peter Ostapczuk; Reinhard Lennartz; Myroslav Zoriy

2010-01-01

A robust analytical method has been developed in our laboratory for the separation of radionuclides by means of extraction chromatography using an automated separation system. The proposed method is both cheap and simple and provides the advantageous, rapid and accurate separation of the element of interest. The automated separation system enables a shorter separation time by maintaining a constant flow rate of solution and by avoiding clogging or bubbling in the chromatographic column. The present separation method was tested with two types of samples (water and urine) using UTEVA-, TRU- and Sr-specific resins for the separation of U, Th, Am, Pu and Sr. The total separation time for one radionuclide ranged from 60 to 100 min with the separation yield ranging from 68 to 98% depending on the elements separated. We used ICP-QMS, multi-low-level counter and alpha spectroscopy to measure the corresponding elements. (author)

Separation and Preconcentration of Ag(1) in Aqueous Samples by Flotation as an Ion-Associate Using Iodide and Ferroin Followed the Determination by Flame Atomic Absorption Spectrometry

International Nuclear Information System (INIS)

Hosseini, M.S.; Kardan-Moghaddam, G.; Hashemi-Moghaddam, M.

2007-01-01

A simple method for separation/preconcentration and determination of Ag (1) in aqueous samples is described. The method is based on formation of an ion-associate between Ag (1)-iodide complex and ferroin, which can be floated at the interface of the aqueous/n-heptane phases. The flotation process was carried out using 500-ml aliquot of the aqueous solution and the floated layer was dissolved in 5 ml of 1 M HNO 3 containing methanol (50% v/v) as the solvent. The Ag (1) content was then determined by flame atomic absorption spectrometry (FAAS). The method so could be considered as an enrichment process, was achieved to a quantitative feature, when the pH of the solution was adjusted to 4 and the concentrations of iodide and ferroin were about 3.2x10 -4 M and 6.25x10 -5 M, respectively. The LOD and RSD (n=7) were obtained 1.0x10 -8 M and 2.4%, respectively. It was found that a large number of cations and anions even at high considerably foreign ion/Ag(1) ratios were not interfered. The method was applied satisfactorily to recovery of Ag(I) from different aqueous samples

Ni(II) ion-imprinted solid-phase extraction and preconcentration in aqueous solutions by packed-bed columns

International Nuclear Information System (INIS)

Ersoez, Arzu; Say, Ridvan; Denizli, Adil

2004-01-01

Solid-phase extraction (SPE) columns packed with materials based on molecularly imprinted polymers (MIPs) were used to develop selective separation and preconcentration for Ni(II) ion from aqueous solutions. SPE is more rapid, simple and economical method than the traditional liquid-liquid extraction. MIPs were used as column sorbent to increase the grade of selectivity in SPE columns. In this study, we have developed a polymer obtained by imprinting with Ni(II) ion as a ion-imprinted SPE sorbent. For this purpose, NI(II)-methacryloylhistidinedihydrate (MAH/Ni(II)) complex monomer was synthesized and polymerized with cross-linking ethyleneglycoldimethacrylate to obtain [poly(EGDMA-MAH/Ni(II))]. Then, Ni(II) ions were removed from the polymer getting Ni(II) ion-imprinted sorbent. The MIP-SPE preconcentration procedure showed a linear calibration curve within concentration range from 0.3 to 25 ng/ml and the detection limit was 0.3 ng/ml (3 s) for flame atomic absorption spectrometry (FAAS). Ni(II) ion-imprinted microbeads can be used several times without considerable loss of adsorption capacity. When the adsorption capacity of nickel imprinted microbeads were compared with non-imprinted microbeads, nickel imprinted microbeads have higher adsorption capacity. The K d (distribution coefficient) values for the Ni(II)-imprinted microbeads show increase in K d for Ni(II) with respect to both K d values of Zn(II), Cu(II) and Co(II) ions and non-imprinted polymer. During that time K d decreases for Zn(II), Cu(II) and Co(II) ions and the k' (relative selectivity coefficient) values which are greater than 1 for imprinted microbeads of Ni(II)/Cu(II), Ni(II)/Zn(II) and Ni(II)/Co(II) are 57.3, 53.9, and 17.3, respectively. Determination of Ni(II) ion in sea water showed that the interfering matrix had been almost removed during preconcentration. The column was good enough for Ni determination in matrixes containing similar ionic radii ions such as Cu(II), Zn(II) and Co(II)

Booth Library On-Line Circulation System (BLOC

Directory of Open Access Journals (Sweden)

Paladugu V. Rao

1971-06-01

Full Text Available An on-line circulation system developed at a relatively small university library demonstrates that academic libraries with limited funds can develop automated systems utilizing parent institution's computer facilities in a time-sharing mode. In operation since September 1968, using an IBM 360/50 computer and associated peripheral equipment, it provides control over all stack books.

Preconcentration of plutonium and americium using the Actinide-CUTM Resin for human tissue analysis

International Nuclear Information System (INIS)

Qu, H.; Stuit, D.; Glover, S.E.; Love, S.F.; Filby, R.H.; Washington State Univ., Pullman, WA

1998-01-01

A method for the preconcentration of Am and Pu from human tissue solutions (liver, lung, bone etc) using the Actinide-CU Resin (EIChroM Industries) has been developed for their alpha-spectrometric determination. With near 100% recoveries were obtained by preconcentration, subsequent decomposition methods for eluent were developed. Good agreement for Pu and Am determination with the USTUR anion-exchange/solvent extraction method was demonstrated using previously analyzed human tissue solutions and NIST SRMs. The advantages of the preconcentration method applied to human tissue analysis are simplicity of operation, shorter analysis time compared to anion exchange/solvent extraction methods, and capacity to analyze large tissue samples (up to 15 g bone ash per analysis and 500 g soft tissue). (author)

Determination of silver in fresh water by atomic absorption spectrometry following flotation preconcentration by iron(III) collectors

Energy Technology Data Exchange (ETDEWEB)

Cundeva, K.; Stafilov, T. [Institute of Chemistry, Faculty of Science, St. Cyril and Methodius University, Skopje (Yugoslavia)

1997-08-01

Colloid precipitate flotation of silver from fresh water is applied for preconcentration and separation. Optimal conditions using hydrated iron(III) oxide and iron(III) tetramethylenedithiocarbamate as collectors were investigated. Various factors affecting the silver recovery, including collector mass, nature of the supporting electrolyte, pH of the working medium, electrokinetic potential of the collector particle surfaces, type of surfactant, induction time etc., were checked. Within the optimal pH range (5.5-6.5) silver was separated quantitatively (94.9- 100.0%) with 30 mg Fe(III) as collector. The content of silver was determined by electrothermal atomic absorption spectrometry and compared to that from inductively coupled plasma-atomic emission spectrometry. The detection limit of silver by the method described is 0.01 {mu}g/L. (orig.) With 2 figs., 3 tabs.

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

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.

On-line monitoring system for I-131 manufacturing labs

International Nuclear Information System (INIS)

Osovizky, A.; Malamud, Y.; Paran, Y.; Tal, N.; Turgeman, S.; Weinstein, M.

1997-01-01

An on-line monitoring and safety system has been installed in a lab for manufacturing 1-131 capsules for nuclear medicine use. Production of up to 100mCi batches is performed in shielded glove boxes. The safety system is based on a unique, 'Medi SMARTS' system (Medical Survey Mapping Automatic Radiation Tracing System), that collects continuously the radiation measurements for processing, display, and storage for future retrieval. Radiation is measured by GM tubes, data is transferred to a data processing unit, and then via a RS-485 communication line to a computer. In addition to the operational advantages and radiation levels storage, the system is being evaluated for the purpose of identifying risky stages in the process. (authors)

Development of a centrifugal in-line separator for oil-water flows

NARCIS (Netherlands)

Slot, J.J.

2013-01-01

The world energy consumption will increase in the next decades. However, many aging oil fields are showing a steady decline in oil production. And they are producing increasing amounts of water, making the separation of the oil from the oil-water mixture an important processing step. In-line

Recent approaches for enhancing sensitivity in enantioseparations by CE.

Science.gov (United States)

Sánchez-Hernández, Laura; García-Ruiz, Carmen; Luisa Marina, María; Luis Crego, Antonio

2010-01-01

This article reviews the latest methodological and instrumental improvements for enhancing sensitivity in chiral analysis by CE. The review covers literature from March 2007 until May 2009, that is, the works published after the appearance of the latest review article on the same topic by Sánchez-Hernández et al. [Electrophoresis 2008, 29, 237-251]. Off-line and on-line sample treatment techniques, on-line sample preconcentration strategies based on electrophoretic and chromatographic principles, and alternative detection systems to the widely employed UV/Vis detection in CE are the most relevant approaches discussed for improving sensitivity. Microchip technologies are also included since they can open up great possibilities to achieve sensitive and fast enantiomeric separations.

Preparation of Modified Magnetic Nanocomposites Dithiooxamide/Fe3O4 for Preconcentration and Determination of Trace Amounts of Cobalt Ions in Food and Natural Water Samples

Directory of Open Access Journals (Sweden)

Ali Mirabi

2016-09-01

Full Text Available The first study on the high efficiency of nanometer-sized magnetic nanoparticles (Fe3O4 coated with sodium dodecyl sulfate (SDS and dithiooxamide as a new sorbent solid phase extraction has been reported. Modified magnetic nanicomposites was used to preconcentrate and separate Co (II ions in food and environmental water samples. Magnetic nanoparticles were prepared by chemical precipitation of Fe (II and Fe (III salts from aqueous solution by ammonia solution. These magnetic nanoparticles and nanocomposites were characterized by scanning electron microscopy (SEM, transmission electron microscopy (TEM, thermo gravimetric analysis (TGA and elemental analysis CHNS. A micro sample introduction system was employed for the nebulization micro-volume of diluted solution into flame atomic absorption spectrometry (FAAS. The extraction conditions were optimized by selecting the appropriate extraction parameters including the amount of nanosorbent, pH value, volume of dithiooxamide and condition of eluting solution. The detection limit of this method for Co (II ions was 1.21 ng ml-1 and the R.S.D. was 0.9% (n=6. The advantages of this new method include rapidity, easy preparation of nanosorbents and a high preconcentration factor. The proposed method has been applied to the determination of Co (II ions at trace levels in real samples such as, kiwi, orange, cucumber, apple, green pepper, honey, potato, tap water, river water and sea water with satisfactory results.

Optimization of temperature-programmed GC separations. II. Off-line simplex optimization and column selection

NARCIS (Netherlands)

Snijders, H.M.J.; Janssen, J.G.M.; Cramers, C.A.M.G.; Sandra, P; Bertsch, W.; Sandra, P.; Devos, G.

1996-01-01

In this work a method is described which allows off-line optimization of temperature programmed GC separations. Recently, we described a new numerical method to predict off-line retention times and peak widths of a mixture containing components with known identities in capillary GC. In the present

Lead preconcentration in synthetic samples with triton x-114 in the cloud point extraction and analysis by atomic absorption (EAAF)

International Nuclear Information System (INIS)

Zegarra Pisconti, Marixa; Cjuno Huanca, Jesus

2015-01-01

A methodology was developed about lead preconcentration in water samples that were added dithizone as complexing agent, previously dissolved in the nonionic surfactant Triton X-114, until the formation of the critical micelle concentration and the cloud point temperature. The centrifuged system gave a precipitate with high concentrations of Pb (II) that was measured by atomic absorption spectroscopy with flame (EAAF). The method has proved feasible to be implemented as a method of preconcentration and analysis of Pb in aqueous samples with concentrations less than 1 ppm. Several parameters were evaluated to obtain a percentage recovery of 89.8%. (author)

Determination and preconcentration of natural and radio-cesium from aqueous solution

International Nuclear Information System (INIS)

Gueclue, K.; Apak, R.; Tuetem, E.; Atun, G.

2004-01-01

A modified atomic emission spectrometric (AES) method to determine cesium(I), based on the measurement of emission intensity at 455.5 nm with a limit of quantitation (LOQ) of 5.5 mg/l and a linear range up to 100 mg/l is reported. In order to increase the sensitivity and lower the detection limits, potential sorbents were investigated for preconcentrating Cs from natural waters. Among the various ion-exchange materials synthesized, potassium hexanitrocobaltate (PHNCo) yielded the highest capacity for 137 Cs tagged Cs + solutions as measured by gamma-spectrometry with a HPGe detector, showing the potential of a cesium preconcentration sorbent. As an alternative to AES determination, the PHNCo sorbent may be used for Cs + collection from radiocesium tagged solutions and the retained activity in the dry solid exchanger be determined by gamma-spectrometry. (author)

Determination of tungsten and tin ions after preconcentration by flotation

International Nuclear Information System (INIS)

Dietze, U.; Kunze, S.

1990-01-01

A highly sensitive and selective combined method of flotation followed by spectrophotometry/d.c. polarography for the determination of tungsten and tin ions in acid and alkaline waste waters and hydrometallurgical solutions is presented here. Both kinds of ions are coprecipitated in the analyte solution with zirconium hydroxide after addition of ZrOCl 2 solution and ammonia. Afterwards, the collector precipitate is separated from the aqueous phase and preconcentrated by flotation for which sodium oleate and a frother are added. The precipitate is dissolved in a small amount of acid, with the organic reagents being destroyed by oxidation. The enrichment factor of the proposed technique is 100, with variations possible. Recovery is 94 % for tungsten and 99 % for tin. Spectrophotometry of the thiocyanate complex and d.c. polarography are applied as determination techniques for tungsten and tin, respectively. Detection limits attainable by this technique are 6 ng.ml -1 for tungsten and 5 ng.ml -1 for tin for the initial sample. (Authors)

Heated uranium tetrafluoride target system to release non-rare gas fission products for the TRISTAN isotope separator

International Nuclear Information System (INIS)

Gill, R.L.

1977-10-01

Off-line experiments indicated that fluorides of As, Se, Br, Kr, Zr, Nb, Mo, Tc, Ru, Sb, Te, I and Xe could be volatilized, but except for Br, Kr, I and Xe, none of these elements were observed after mass separation in the on-line experiments. The results of the on-line experiments indicated a very low level of hydride contamination at ambient temperature and consequently, uranium tetrafluoride replaced uranyl stearate as the primary gaseous fission product target. Possible reasons for the failure of the heated target system to yield non-rare gas activities are discussed and suggestions for designing a new heated target system are presented

Activated carbon modified with 4-(8-hydroxyquinoline-azo)benzamidine for selective solid-phase extraction and preconcentration of trace lead from environmental samples

International Nuclear Information System (INIS)

Tian, H.; Chang, X.; Hu, Z.; Yang, K.; He, Q.; Zhang, L.; Tu, Z.

2010-01-01

Activated carbon was chemically modified with 4-(8-hydroxyquinoline-azo)benzamidine and used for separation and preconcentration of trace amounts of Pb(II) in environmental samples by solid-phase extraction prior to the measurement by inductively coupled plasma atomic emission spectrometry. The effects of pH, shaking time, eluent concentration and volume, sample flow rate and potential interfering ions were studied. Under the optimum conditions, the enrichment factor was 100, the detection limits is 0. 43 ng mL -1 , and the relative standard deviations are <2. 1% (n = 8). The adsorption capacity of the sorbent is 53. 58 mg of lead(II) per gram of the material. The sorbent was successfully applied to the preconcentration of trace Pb(II) in the reference materials GBW 08301 (river sediment) and GBW 08302 (Tibet soil). The recovery of lead(II) from Yellow river water, Huangshui water, and tap water is in range of 99. 3-101. 6%. (author)

Characterizing chemical systems with on-line computers and graphics

International Nuclear Information System (INIS)

Frazer, J.W.; Rigdon, L.P.; Brand, H.R.; Pomernacki, C.L.

1979-01-01

Incorporating computers and graphics on-line to chemical experiments and processes opens up new opportunities for the study and control of complex systems. Systems having many variables can be characterized even when the variable interactions are nonlinear, and the system cannot a priori be represented by numerical methods and models. That is, large sets of accurate data can be rapidly acquired, then modeling and graphic techniques can be used to obtain partial interpretation plus design of further experimentation. The experimenter can thus comparatively quickly iterate between experimentation and modeling to obtain a final solution. We have designed and characterized a versatile computer-controlled apparatus for chemical research, which incorporates on-line instrumentation and graphics. It can be used to determine the mechanism of enzyme-induced reactions or to optimize analytical methods. The apparatus can also be operated as a pilot plant to design control strategies. On-line graphics were used to display conventional plots used by biochemists and three-dimensional response-surface plots

A modular multi-microcomputer system for on-line vibration diagnostics

International Nuclear Information System (INIS)

Saedtler, E.

1988-01-01

A new modular multi-microprocessor system for on-line vibration monitoring and diagnostics of PWRs is described. The aim of the system is to make feasible an early detection of increasing failures in relevant regions of a reactor plant, to verify the mechanical integrity of the investigated components, and to improve therefore the operational safety of the plant. After a discussion of the implemented surveillance methods and algorithms, which are based on hierarchical structured identification (estimation) and statistical pattern recognition tools, the system architecture (software and hardware) is portrayed. The classification scheme itself works sequential so that samples (or features) can arrive on-line. This on-line classification is important in order to take necessary actions in time. Furthermore, the system has learning capabilities, which means it is adaptable to different, varying states and plant conditions. The main features of the system are presented and its contribution to an automation of complex surveillance and monitoring tasks is shown. (author)

Comparison of ultra-violet and inductively coupled plasma-atomic emission spectrometry for the on-line quantification of selenium species after their separation by reversed-phase liquid chromatography

International Nuclear Information System (INIS)

Tsopelas, Fotios N.; Ochsenkuehn-Petropoulou, Maria Th.; Mergias, Ioannis G.; Tsakanika, Lambrini V.

2005-01-01

An analytical approach for selenium speciation using liquid chromatography (LC) coupled with ultra-violet (UV) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) was developed. The separation of the investigated selenium species, selenites, selenates, selenomethionine, selenocystine, selenocystamine and dimethyldiselenide was accomplished in less than 6 min on a BIO Wide Pore RP-18 column using sodium salt of n-octanesulfonic acid as ion-pairing modifier. The on-line detection of the separated selenium species was performed using UV spectrometry at the optimum wavelength of 192 nm, obtained by the UV spectra of the investigated individual selenium species. ICP-AES was also used as element specific on-line detector, after its coupling with the chromatographic system. The UV and ICP-AES detectors were compared for their suitability, including sensitivity and detection limits, for the on-line quantification of the six selenium species. The developed LC-UV as well as LC-ICP-AES techniques were successfully applied to a selenized yeast candidate reference material, after its enzymatic extraction with protease XIV. It was found that the described LC-UV technique is suitable for the determination of selenomethionine, the main selenium compound in the yeast, with an accuracy of 5%, although the UV detector is not element specific and it is rarely used for selenium speciation. This finding can prove valuable for routine laboratories to perform selenium speciation in such materials

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

Science.gov (United States)

Werner, Justyna

2018-05-15

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

26 CFR 1.414(r)-1 - Requirements applicable to qualified separate lines of business.

Science.gov (United States)

2010-04-01

... lines of business. 1.414(r)-1 Section 1.414(r)-1 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT... Plans, Etc. § 1.414(r)-1 Requirements applicable to qualified separate lines of business. (a) In general. Section 414(r) prescribes the conditions under which an employer is treated as operating qualified...

Environmentally safe separation and pre-concentration of rhodium and ruthenium from spent nuclear fuel using mixed-micelle cloud point extraction and determination by ICP-MS

International Nuclear Information System (INIS)

Ranjit, M.; Meeravali, N.N.; Kumar, S.J.

2010-01-01

Full text: Recently, spend nuclear fuel waste of thermal and fast reactors are emerging as an alternative valuable resource for Rh, Ru and Pd. In addition, its presence causes the difficulty in the vitrification process. Hence, its safe extraction from these wastes has to be carried out by using the environmental friendly extraction procedure. In this study, we have reported the simple mixed-micelle cloud point extraction (MM-CPE) procedure for separation as well as pre-concentration of Rh, Ru and Pd. This MM-CPE is carried out preliminarily from aqueous chloride medium with Aliquat-336/Triton X-114 mixed-micelles in the absence and presence of tin(II) chloride. In presence of chloride medium alone, only Pd get extracted quantitatively, while extraction of Rh and Ru are negligible. In presence of tin chloride, the extraction of Rh and Ru increases and becomes quantitative, without affecting the extraction of Pd. The MM-CPE conditions are optimized under influence of variables such as HCI, Aliquat-336, Triton X-114 and tin chloride concentrations and incubation time and temperature. Under the optimized conditions, the accuracy of the procedure is verified by using recovery study carried out from real water samples. This work is under progress to apply real nuclear fuel waste samples

Determinação de mercúrio em águas por CVAAS empregando sílica modificada por 2-aminotiazol

OpenAIRE

Silva, F. A. [UNESP; Alcântara, I. L. de [UNESP; Roldan, P. S. [UNESP; Padilha, C. C. F. [UNESP; Araújo, A. B. de [UNESP; Valente, J. P. S. [UNESP; Florentino, A. O. [UNESP; Padilha, P. M. [UNESP

2005-01-01

This paper discusses a rapid and sensitive method developed to determine trace levels of mercury in natural water samples by cold vapor atomic absorption spectrometry using a preconcentration system composed by mini-column packed with 100 mg of 2-aminothiazol modified silica gel (SiAT) coupled on-line with the spectrometer's cold vapor generator system. The optimum preconcentration conditions are also described here. The preconcentrated Hg(II) ions were eluted directly from the column to the ...

A novel homocystine-agarose adsorbent for separation and preconcentration of nickel in table salt and baking soda using factorial design optimization of the experimental conditions.

Science.gov (United States)

Hashemi, Payman; Rahmani, Zohreh

2006-02-28

Homocystine was for the first time, chemically linked to a highly cross-linked agarose support (Novarose) to be employed as a chelating adsorbent for preconcentration and AAS determination of nickel in table salt and baking soda. Nickel is quantitatively adsorbed on a small column packed with 0.25ml of the adsorbent, in a pH range of 5.5-6.5 and simply eluted with 5ml of a 1moll(-1) hydrochloric acid solution. A factorial design was used for optimization of the effects of five different variables on the recovery of nickel. The results indicated that the factors of flow rate and column length, and the interactions between pH and sample volume are significant. In the optimized conditions, the column could tolerate salt concentrations up to 0.5moll(-1) and sample volumes beyond 500ml. Matrix ions of Mg(2+) and Ca(2+), with a concentration of 200mgl(-1), and potentially interfering ions of Cd(2+), Cu(2+), Zn(2+) and Mn(2+), with a concentration of 10mgl(-1), did not have significant effect on the analyte's signal. Preconcentration factors up to 100 and a detection limit of 0.49mugl(-1), corresponding to an enrichment volume of 500ml, were obtained for the determination of the analyte by flame AAS. Application of the method to the determination of natural and spiked nickel in table salt and baking soda solutions resulted in quantitative recoveries. Direct ETAAS determination of nickel in the same samples was not possible because of a high background observed.

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

Speciation analysis of mercury in sediments, zoobenthos and river water samples by high-performance liquid chromatography hyphenated to atomic fluorescence spectrometry following preconcentration by solid phase extraction

International Nuclear Information System (INIS)

Margetinova, Jana; Houserova-Pelcova, Pavlina; Kuban, Vlastimil

2008-01-01

A high-pressure microwave digestion was applied for microwave-assisted extraction (MAE) of mercury species from sediments and zoobenthos samples. A mixture containing 3 mol L -1 HCl, 50% aqueous methanol and 0.2 mol L -1 citric acid (for masking co-extracted Fe 3+ ) was selected as the most suitable extraction agent. The efficiency of proposed extraction method was better than 95% with R.S.D. below 6%. A preconcentration method utilizing a 'homemade' C18 solid phase extraction (SPE) microcolumns was developed to enhance sensitivity of the mercury species determination using on-column complex formation of mercury-2-mercaptophenol complexes. Methanol was chosen for counter-current elution of the retained mercury complexes achieving a preconcentration factor as much as 1000. The preconcentration method was applied for the speciation analysis of mercury in river water samples. The high-performance liquid chromatography-cold vapour atomic fluorescence spectrometric (HPLC/CV-AFS) method was used for the speciation analysis of mercury. The complete separation of four mercury species was achieved by an isocratic elution of aqueous methanol (65%/35%) on a Zorbax SB-C18 column (4.6 mm x 150 mm, 5 μm) using the same complexation reagent (2-mercaptophenol). The limits of detection were 4.3 μg L -1 for methylmercury (MeHg + ), 1.4 μg L -1 for ethylmercury (EtHg + ), 0.8 μg L -1 for inorganic mercury (Hg 2+ ), 0.8 μg L -1 for phenylmercury (PhHg + )

Application of chitosan and its N-heterocyclic derivatives for preconcentration of noble metal ions and their determination using atomic absorption spectrometry.

Science.gov (United States)

Azarova, Yu A; Pestov, A V; Ustinov, A Yu; Bratskaya, S Yu

2015-12-10

Chitosan and its N-heterocyclic derivatives N-2-(2-pyridyl)ethylchitosan (2-PEC), N-2-(4-pyridyl) ethylchitosan (4-PEC), and N-(5-methyl-4-imidazolyl) methylchitosan (IMC) have been applied in group preconcentration of gold, platinum, and palladium for subsequent determination by atomic absorption spectroscopy (AAS) in solutions with high background concentrations of iron and sodium ions. It has been shown that the sorption mechanism, which was elucidated by XPS, significantly influences the sorption capacity of materials, the efficiency of metal ions elution after preconcentration, and, as a result, the accuracy of metal determination by AAS. We have shown that native chitosan was not suitable for preconcentration of Au(III), if the elution step was used as a part of the analysis scheme. The group preconcentration of Au(III), Pd(II), and Pt(IV) with subsequent quantitative elution using 0.1M HCl/1M thiourea solution was possible only on IMC and 4-PEC. Application of IMC for analysis of the national standard quartz ore sample proved that gold could be accurately determined after preconcentration/elution with the recovery above 80%. Copyright © 2015 Elsevier Ltd. All rights reserved.

On-line detection of small radioactive ions by capillary electrophoresis

International Nuclear Information System (INIS)

Klunder, G.L.; Andrews, J.E. Jr.; Russo, R.E.

1994-01-01

Worldwide environmental interests have placed a great demand on developing techniques for rapid characterization of contaminated soil and groundwater. Detection of radioactive contaminants is necessary for monitoring effluents from nuclear processes or to assure proper long term storage of radioactive waste. The authors have been investigating the chemistry required to separate representative radioactive small cations and anions by capillary electrophoresis. In order to evaluate the separation chemistry, detection of stable isotopes of the representative ions was achieved by indirect absorption for cations and direct absorption for anions. Several buffer systems which have been considered in the optimization of the separations will be discussed. The authors have designed and tested two on-line radioactivity detectors for capillary electrophoresis. An on-line solid state CdTe detector was constructed for this study and a scintillation detector has been designed using a high gain photodiode light sensor. Different scintillation materials have been tested. Comparison of the detectors, design considerations, efficiency and limits of detection will be presented

Determination of lead, iron and nickel in water and vegetable samples after preconcentration with aspergillus niger loaded on silica gel

Energy Technology Data Exchange (ETDEWEB)

Baytak, Sitki [Harran University, Arts and Science Faculty, Department of Chemistry, Sanliurfa (Turkey); Kocyigit, Abdurrahim [Harran University, Faculty of Medicine, Department of Biochemistry, Sanliurfa (Turkey); Rehber Tuerker, Ali [Gazi University, Arts and Science Faculty, Department of Chemistry, Ankara (Turkey)

2007-12-15

A method for the determination of Fe(III), Pb(II), and Ni(II) by flame atomic absorption spectrometry (FAAS) after preconcentrating on a column containing Aspergillus niger loaded on silica gel 60 (Biosorbent) is described. The effect of experimental parameters such as pH, flow rate of sample solution, and volume of sample solution were investigated on the recovery of the analytes. The effect of interfering ions on the recovery of the analytes has also been investigated. Recoveries of Fe(III), Pb(II), and Ni(II) were (98 {+-} 2), (98 {+-} 3), (99 {+-} 2)% at the 95% confidence level, respectively. For the analytes, 50-fold preconcentration was obtained. The analytical detection limits for Fe(III), Pb(II), and Ni(II) were 1.7, 5.2, and 1.6 ng/mL, respectively. The proposed method was applied to the determination of trace metals in various water and vegetable samples. The analytes have been determined with relative error lower than 7%. (Abstract Copyright [2007], Wiley Periodicals, Inc.)

Preconcentration and determination of uranium on to polyurethane foam functionalized with salicylate

International Nuclear Information System (INIS)

Sousa, Alvaro S.F. de; Ferreira, Elizabeth de M.M.; Cassella, Ricardo J.

2009-01-01

Salicylate was covalently linking with a commercial polyurethane foam (PUF) through -N=N-group generating a stable chelating sorbent (PUFS). The synthesized sorbent was characterized by Infrared Spectrometry (IR) measurement. Good stability towards various solvents was noticed. The pH influence and equilibration shaking time adsorption onto foam functionalized was studied as factors influencing the extraction process of the uranium ion solution. Extraction of uranium was accomplished in 10 minutes. Uranium at ppb level was absorbed as the salicylate complex on powered PUFS at pH about 8.0. Uranium could be achieved in 85 % from a 500 mL uranium solution (0.1 μgmL -1 ) which shows the suitability of salicylate foam for preconcentration analysis. (author)

A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Tuzen, Mustafa [Department of Chemistry, Gaziosmanpasa University, 60250 Tokat (Turkey); Soylak, Mustafa [Department of Chemistry, Erciyes University, 38039 Kayseri (Turkey)], E-mail: soylak@erciyes.edu.tr; Citak, Demirhan [Department of Chemistry, Gaziosmanpasa University, 60250 Tokat (Turkey); Ferreira, Hadla S.; Korn, Maria G.A. [Universidade Federal da Bahia, Instituto de Quimica, 40170-290 Salvador (Brazil); Bezerra, Marcos A. [Universidade Estadual do Sudoeste da Bahia, 45200-190 Jequie (Brazil)

2009-03-15

A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L{sup -1} nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 {mu}g L{sup -1}, respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 {mu}g L{sup -1}. The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish.

Rapid assessment of mycotoxins in wine by on-line SPE-UHPLC-FLD

Directory of Open Access Journals (Sweden)

Nistor Alina-Mihaela

2017-01-01

Full Text Available According to the latest statistics, grapes are one of the largest fruit crops worldwide. In this regard, it is important to consider all factors influencing quality of grapes and wine. In the last years, scientist focused on the study of mycotoxins that can influence the quality of wine. It is considered that toxins produced by moulds, causing significant economic losses, affect approximately one quarter of the world grape production. If the selective sorting of infected grapes is not done adequately, wine will present a major risk to consumers, mycotoxins being considered by the “International Agency for Cancer Research” a carcinogenic compound. The main mycotoxins monitored in this study come from Aspergillus sp., and are represented by aflatoxins B1, B2, G1, G2 and ochratoxin A. This study purpose is to develop a faster method for the analysis of mycotoxins, in order to increase rapidity and efficiency for the evaluation of the degree of infestation in wine. The purposed method is using an on-line large volume injection coupled to pre-concentration of sample (SPE which is directly transfer to the ultra-high-pressure liquid chromatography (UHPLC column for separation and the detection by means of the fluorescence detector (FLD. As the maximum tolerated level for mycotoxins in wines is 2 ppm, this method is able to detect under this limits of quantification with RSD below 2%.

Pre-concentration and determination of tartrazine dye from aqueous solutions using modified cellulose nanosponges.

Science.gov (United States)

Shiralipour, Roohollah; Larki, Arash

2017-01-01

In this study, a new absorbent based on cellulose nanosponges modified with methyltrioctylammonium chloride (aliquat 336) was prepared and used for pre-concentration, removal and determination of tartrazine dye, using UV-vis spectrophotometry. This adsorbent was fully characterized using various instrumental techniques such as SEM, FTIR and XRD spectra. The pre-concentration and removal procedures were studied in column and batch modes, respectively. The effects of parameters such as pH of the aqueous medium, methyltrioctylammounium chloride dose, adsorbent amount, desorbing conditions and interfering ions on the adsorption of tartrazine were investigated and optimized. The fitting experimental data with conventional isotherm models revealed that the adsorption followed the Brunauer-Emmett-Teller (BET) model and the maximum adsorption capacity for tartrazine was 180mg/g with modified nanosponges. Under the optimized conditions, the calibration curve was linear over the range of 2-300ng/mL and the limit of detection was 0.15ng/mL. The relative standard deviation (RSD) for 20 and 100ng/mL of tartrazine were 3.1% and 1.5%, respectively. The proposed method was applied for pre-concentration and determination of tartrazine dye in different water samples. Copyright © 2016 Elsevier Inc. All rights reserved.

A new electrostatic on-line collection-system

International Nuclear Information System (INIS)

Dufour, J.P.; Del Moral, R.; Fleury, A.

1981-06-01

The working conditions of a new on-line electrostatic collection system are presented. The main charactersitics are high efficiency (reaching 20%) and short delay time (down to the millisecond). The salient features of specific devices for measurements of absolute cross sections, recoil range distributions and angular distributions are given

Extraction chromatographic separation of Sr, Pu and Am in environmental samples

Energy Technology Data Exchange (ETDEWEB)

Sidhu, Rajdeep

2004-04-01

An accurate determination of radionuclides from various sources in the environment is essential for assessment of the potential hazards and suitable countermeasures both in case of an authorised release, accidents and routine surveillance. Due to the short range of alpha and beta radiation, the accurate determination of pure alpha and beta emitters must always include radiochemical separations to separate the analytes from the matrix and from other interfering stable and radioactive nuclides. Hence, the procedures used for their determination are usually tedious and involve several preconcentration and separation steps. This work deals with the determination of {sup 90}Sr, {sup 241}Am, {sup 238}Pu, {sup 239,240}Pu and {sup 244}Cm, whic some of the most important artificial radionuclides. Due to either absence or low yield of gamma radiation, a secure determination of low concentrations of all these nuclides requires a dedicated chemistry. Selective extraction chromatographic resins (TRU- and Sr-Resin) have been utilised to develop new procedures for the analyses of Pu, Am and Cm isotopes in seawater and both these and {sup 90}Sr in soil, sediment, urine and low-level liquid radioactive effluents. The proposed method for the analyses of Pu and Am in seawater offers a quick and secure mode for the determination of these radionuclides in marine waters. Combined pre-concentration of actinides and strontium (oxalate or phosphate precipitation) followed by dual column separation on TRU- and Sr-Resin significantly reduces the through put time and costs compared to traditional ion exchange and precipitation methods. The greatest gain in productivity and environmental friendliness is achieved in Sr separations using Sr-Resin instead of precipitations involving fuming nitric acid and oxalate, hydroxide, chromate and carbonate precipitations. (author)

Preconcentration of trace uranium from seawater with solid phase extraction followed by differential pulse polarographic determination in chloroform eluate

International Nuclear Information System (INIS)

Dojozan, Dj.; Pournaghi-Azar, M.H.; Toutounchi-Asr, J.

1998-01-01

In the present study, an effective method is presented for the separation and preconcentration of uranium (VI) by solid phase extraction (SPE). For this purpose, U(VI) oxinate is formed by the reaction of U(VI) with 8-hydroxyquinoline and adsorbed onto the octylsilane (C-8) SPE cartridge. The analyte is completely eluted with chloroform and determined by differential pulse polarography. The SPE conditions were optimized by evaluating the effective factors such as pH, oxine concentration, type and concentration of buffer and masking agent. By the proposed method a preconcentration factor of more than 100 was achieved. The average recovery of uranium (VI) oxinate (0.1 mg l -1 ) was 99.8%. The relative standard deviation was 1.6% for seven replicate determinations of uranyl ion in the solution with a concentration 20 μg l -1 . Some concomitant ions such as Ca +2 , Mg +2 and Fe +3 which interfere in extraction or determination process of uranium were masked with EDTA in aqueous phase during the extraction process. The proposed method was successfully used for the determination of uranium in Caspian Sea and Persian Gulf water samples

R and D of On-line Reprocessing Technology for Molten-Salt Reactor Systems

International Nuclear Information System (INIS)

Uhlir, Jan; Tulackova, Radka; Chuchvalcova Bimova, Karolina

2006-01-01

The Molten Salt Reactor (MSR) represents one of promising future nuclear reactor concept included in the Generation IV reactors family. The reactor can be operated as the thorium breeder or as the actinide transmuter. However, the future deployment of Molten-Salt Reactors will be significantly dependent on the successful mastering of advanced reprocessing technologies dedicated to their fuel cycle. Here the on-line reprocessing technology connected with the fuel circuit of MSR is of special importance because the reactor cannot be operated for a long run without the fuel salt clean-up. Generally, main MSR reprocessing technologies are pyrochemical, majority of them are fluoride technologies. The proposed flow-sheets of MSR on-line reprocessing are based on a combination of molten-salt / liquid metal extraction and electro-separation processes, which can be added to the gas extraction process already verified during the MSRE project in ORNL. The crucial separation method proposed for partitioning of actinides from fission products is based on successive Anodic dissolution and Cathodic deposition processes in molten fluoride media. (authors)

On-line determination of anions in pulp mills by capillary electrophoresis (CE); Tehdasoloissa tapahtuva anionien kapillaarielektroforeettinen on-line maeaeritys ja sen hyoedyntaeminen prosessivalvonnassa - MPKY 02

Energy Technology Data Exchange (ETDEWEB)

Kokkonen, R.; Holmberg, M.; Vainikka, V. [Finnish Pulp and Paper Research Institute, Espoo (Finland)

1998-12-31

The aim of the study was to set-up a process control system for on-line measurement of certain anions. Typical anions which forms precipitates in pulp and paper mills are oxalate, carbonate and sulphate. Thus it is important to develop a continuous process analyzing system to control concentration levels of this anions. For the preliminary tests of continuous determinations of chloride and sulphate anions in tap water a simple on-line system was build in KCL (The Finnish Pulp and Paper Research Institute) and connected to a capillary electroforesis apparatus. In the preliminary tests a chromate buffer (ph = 7.6) was used. Separation of chloride and sulphate was excellent but the stability of buffer was not good enough and it was usable only for few hours. After experimental studies VTT developed a stable capillary electrophoresis method based on mixed amine buffer and this was selected for an on-line method for determination of anions in process waters of the pulp and paper industry. In the preliminary on-line test (r = 20) repeatabilities of migration times of sulphate and chloride with the chromate buffer were < 5 % (RSD) and peak heights < 15 % (RSD). With the mixed amine buffer repeatabilities were better. The preliminary tests showed that it is possible to connect a capillary electrophoresis system to on-line measurements. For the moment no commercial on-line CE apparatus is available. (orig.)

On-line determination of anions in pulp mills by capillary electrophoresis (CE); Tehdasoloissa tapahtuva anionien kapillaarielektroforeettinen on-line maeaeritys ja sen hyoedyntaeminen prosessivalvonnassa - MPKY 02

Energy Technology Data Exchange (ETDEWEB)

Kokkonen, R; Holmberg, M; Vainikka, V [Finnish Pulp and Paper Research Institute, Espoo (Finland)

1999-12-31

The aim of the study was to set-up a process control system for on-line measurement of certain anions. Typical anions which forms precipitates in pulp and paper mills are oxalate, carbonate and sulphate. Thus it is important to develop a continuous process analyzing system to control concentration levels of this anions. For the preliminary tests of continuous determinations of chloride and sulphate anions in tap water a simple on-line system was build in KCL (The Finnish Pulp and Paper Research Institute) and connected to a capillary electroforesis apparatus. In the preliminary tests a chromate buffer (ph = 7.6) was used. Separation of chloride and sulphate was excellent but the stability of buffer was not good enough and it was usable only for few hours. After experimental studies VTT developed a stable capillary electrophoresis method based on mixed amine buffer and this was selected for an on-line method for determination of anions in process waters of the pulp and paper industry. In the preliminary on-line test (r = 20) repeatabilities of migration times of sulphate and chloride with the chromate buffer were < 5 % (RSD) and peak heights < 15 % (RSD). With the mixed amine buffer repeatabilities were better. The preliminary tests showed that it is possible to connect a capillary electrophoresis system to on-line measurements. For the moment no commercial on-line CE apparatus is available. (orig.)

A new electrostatic on-line collection-system

International Nuclear Information System (INIS)

Dufour, J.P.; Del Moral, R.; Fleury, A.; Hubert, F.; Llabador, Y.; Mauhourat, M.B.; Bimbot, R.; Gardes, D.; Rivet, M.F.

1981-01-01

The working conditions of a new on-line electrostatic collection system are presented. The main characteristics are high efficiency (reaching 20%) and short delay time (down to the millisecond). The salient features of specific devices for measurements of absolute cross sections, recoil range distributions and angular distributions are given. (orig.)

26 CFR 1.414(r)-7 - Determination of the employees of an employer's qualified separate lines of business.

Science.gov (United States)

2010-04-01

... same department, or at the same location, to the same qualified separate line of business would be an... qualified separate lines of business. 1.414(r)-7 Section 1.414(r)-7 Internal Revenue INTERNAL REVENUE...-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-7 Determination of the employees of an employer's qualified...

ORION - the OMEGA Remote Interactive On-line System

CERN Document Server

Russell, R D; Krieger, M

1973-01-01

ORION is a system which permits the manipulation of files, records and characters, remote job submittal and retrieval of output files including the direct loading of remote on-line computers. The system uses the computer hardware of the OMEGA project at CERN, and is designed to assist researchers in development and debugging of their programs.

State of technology, system and solution supporting on-line maintenance - company's activities and products

International Nuclear Information System (INIS)

Nishitani, Junichi; Shimizu, Shunichi; Higasa, Hisakazu

2010-01-01

The new inspection system based on operator's maintenance and monitoring program of nuclear power plants was introduced in Japan more than one year ago and recommended on-line maintenance (maintenance during operation) will be carried out to increase capacity factor with safe and reliable operation of the plant. In this feature article, nine experts described the state of technology, system and solution supporting on-line maintenance - company's activities and products. These were titled as 'MHI's technology supporting on-line maintenance'. 'Technology supporting on-line maintenance - Toshiba's activities to upgrade monitoring and diagnostic service and maintenance management', 'AsahiKASEI's activities of on-line maintenance', 'Importance of information sharing of on-line maintenance and its ideal method-function of impact plan of IBM Maximo Asset Management for Nuclear', 'US's on-line maintenance and information systems', 'SmartProcedures realizing safe operation of nuclear power plant - proposal of computerized procedures', 'Ultrasonic leak detection system SDT170', 'Application of infrared thermography for equipment maintenance in nuclear power plant' and 'On-line condition monitoring system - condition eye'. (T. Tanaka)

Relativistic and separable classical hamiltonian particle dynamics

International Nuclear Information System (INIS)

Sazdjian, H.

1981-01-01

We show within the Hamiltonian formalism the existence of classical relativistic mechanics of N scalar particles interacting at a distance which satisfies the requirements of Poincare invariance, separability, world-line invariance and Einstein causality. The line of approach which is adopted here uses the methods of the theory of systems with constraints applied to manifestly covariant systems of particles. The study is limited to the case of scalar interactions remaining weak in the whole phase space and vanishing at large space-like separation distances of the particles. Poincare invariance requires the inclusion of many-body, up to N-body, potentials. Separability requires the use of individual or two-body variables and the construction of the total interaction from basic two-body interactions. Position variables of the particles are constructed in terms of the canonical variables of the theory according to the world-line invariance condition and the subsidiary conditions of the non-relativistic limit and separability. Positivity constraints on the interaction masses squared of the particles ensure that the velocities of the latter remain always smaller than the velocity of light

Graphene for separation and preconcentration of trace amounts of cobalt in water samples prior to flame atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Yukun Wang

2016-09-01

Full Text Available A new sensitive and simple method was developed for the preconcentration of trace amounts of cobalt (Co using 1-(2-pyridylazo-2-naphthol (PAN as chelating reagent prior to its determination by flame atomic absorption spectrometry. The proposed method is based on the utilization of a column packed with graphene as sorbent. Several effective parameters on the extraction and complex formation were selected and optimized. Under optimum conditions, the calibration graph was linear in the concentration range of 5.0–240.0 μg L−1 with a detection limit of 0.36 μg L−1. The relative standard deviation for ten replicate measurements of 20.0 and 100.0 μg L−1 of Co were 3.45 and 3.18%, respectively. Comparative studies showed that graphene is superior to other adsorbents including C18 silica, graphitic carbon, and single- and multi-walled carbon nanotubes for the extraction of Co. The proposed method was successfully applied in the analysis of four real environmental water samples. Good spiked recoveries over the range of 95.8–102.6% were obtained.

On-line corrosion monitoring in district heating systems

DEFF Research Database (Denmark)

Richter, Sonja; Thorarinsdottir, R.I.; Hilbert, Lisbeth Rischel

2004-01-01

), Electrochemical Noise (EN) and Zero Resistance Ammetry (ZRA). Electrochemical Resistance (ER) has also been used to measure corrosion. The method traditionally only measures corrosion off-line but with newly developed high-sensitive ER technique developed by MetriCorr in Denmark, on-line monitoring is possible...... complicates the chemistry of the environment. Hydrogen sulphide is present in geothermal systems and can be formed as a by-product of sulphate-reducing-bacteria (SRB). The application of electrochemical methods makes on-line monitoring possible. These methods include: Linear Polarization Resistance (LPR....... In order to assess both general corrosion and localized corrosion, it is necessary to apply more than one monitoring technique simultaneously, ZRA or EN for measuring localized corrosion and LPR or ER for measuring general corrosion rate. The advantage of monitoring localized corrosion is indisputable...

A study on neutron activation analysis for the determination of the contents of impurities in reactor materials

International Nuclear Information System (INIS)

Kim, N.B.

1983-01-01

In determining the contents of impurity elements in reactor materials using neutron activation analysis, methods for preconcentration and radiochemical separtion have been studied. Before applying neutron irradiation, impurities in uranium dioxide have been preconcentrated by an anion exchange separtion method and boron impurity has been preconcentrated by a cation exchange separation method or an ashing method. After neutron irradiation the radiochemical separation method for the determination of 27 elements is based on a group separation using ion-exchange resin and material exchanger. The method has imployed mineral acid or organic mixture of the acid, excluding hydrofluoric acid, as the media and common glass wares as the apparatus. This separation method was applied to the reactor materials such as aluminum, steel, graphite and uranium dioxide. The single comparator method was used for determining the content of each element separated radiochemically and analytical results gave the statistical and systematic errors of less than 10% and 6.1%, respectively. A prompt gamma-ray measurement method has been used for determining the content of preconcentrated boron and the analytical results gave the statistical and systematic errors of 5.4% and 3.3%, respectively. (Author)

ORION-the Omega Remote Interactive On-line System

CERN Document Server

Russell, R D; Levratt, B; Lipps, H; Sparrman, P

1974-01-01

ORION is a system which permits the manipulation of files, records and characters, remote job submittal and retrieval of output files including the direct loading of remote on-line computers. The system uses the computer hardware of the OMEGA project at CERN and is designed to assist researchers in development and debugging of their programs. (10 refs).

NAA using Cf-252 after preconcentration

International Nuclear Information System (INIS)

Panyo, O.; Moebius, S.; Keller, C.

1988-01-01

Neutron activation analysis (NAA) with thermal neutron using Cf-252 sources was applied to elemental analysis of elements in water samples. A high-resolution Ge(Li) detector was employed for gamma-radiation detection. Both suspended particulate matter and liquid fraction were investigated after filtration. Preconcentration method by co-precipitation using iron (III) hydroxide and oxine were chosen for use. Elements which were considered to be able to detect in the present study are Al, As, Cl, K, Mg, Mn, Na, Sr, Ti, U, V and Zn

The beam diagnostic instruments in Beijing radioactive ion-beam facilities isotope separator on-line

International Nuclear Information System (INIS)

Ma, Y.; Cui, B.; Ma, R.; Tang, B.; Chen, L.; Huang, Q.; Jiang, W.

2014-01-01

The beam diagnostic instruments for Beijing Radioactive Ion-beam Facilities Isotope Separator On-Line are introduced [B. Q. Cui, Z. H. Peng, Y. J. Ma, R. G. Ma, B. Tang, T. Zhang, and W. S. Jiang, Nucl. Instrum. Methods 266, 4113 (2008); T. J. Zhang, X. L. Guan, and B. Q. Cui, in Proceedings of APAC 2004, Gyeongju, Korea, 2004, http://www.jacow.org , p. 267]. For low intensity ion beam [30–300 keV/1 pA–10 μA], the beam profile monitor, the emittance measurement unit, and the analyzing slit will be installed. For the primary proton beam [100 MeV/200 μA], the beam profile scanner will be installed. For identification of the nuclide, a beam identification unit will be installed. The details of prototype of the beam diagnostic units and some experiment results will be described in this article

Basic studies of a gas-jet-coupled ion source for on-line isotope separation

International Nuclear Information System (INIS)

Anderl, R.A.; Novick, V.J.; Greenwood, R.C.

1980-01-01

A hollow-cathode ion source was used in a gas-jet-coupled configuration to produce ion beams of fission products transported to it from a 252 Cf fission source. Solid aerosols of NaCl and Ag were used effectively as activity carriers in the gas-jet system. Flat-plate skimmers provided an effective coupling of the ion source to the gas jet. Ge(Li) spectrometric measurements of the activity deposited on an ion-beam collector relative to that deposited on a pre-skimmer collector were used to obtain separation efficiencies ranging from 0.1% to > 1% for Sr, Y, Tc, Te, Cs, Ba, Ce, Pr, Nd and Sm. The use of CCl 4 as a support gas resulted in a significant enhancement of the alkaline-earth and rare-earth separation efficiencies

Study for reactive power on distribution system line B RSG-GAS

International Nuclear Information System (INIS)

Yan Bony Marsahala

2010-01-01

Study for reactive power on distribution system line B RSG-GA is already done. The study intended to evaluate how much inductive load need the reactive power (positive), how much power factor, and what will be done to increase the power factor. The reactive power is the losses power, can't be changed into energy, but it is need for transmission process and it is cause the energy losses. The loads on distribution system line B consist of induction motors which are used for primary cooling system and secondary cooling system, lift, blower on cooling tower, and air condition system. Due to the motors using, the power factor are falling down to low. By the calculation results give that the inductive loads on distribution line B are 850 KVA and these loads caused the low power factor 0.80. If we want to increase the power factor up to 0.95, it is need to install the reactive loads likes capacitor bank 250 KVAR. (author)

Removal of power line interference of space bearing vibration signal based on the morphological filter and blind source separation

Science.gov (United States)

Dong, Shaojiang; Sun, Dihua; Xu, Xiangyang; Tang, Baoping

2017-06-01

Aiming at the problem that it is difficult to extract the feature information from the space bearing vibration signal because of different noise, for example the running trend information, high-frequency noise and especially the existence of lot of power line interference (50Hz) and its octave ingredients of the running space simulated equipment in the ground. This article proposed a combination method to eliminate them. Firstly, the EMD is used to remove the running trend item information of the signal, the running trend that affect the signal processing accuracy is eliminated. Then the morphological filter is used to eliminate high-frequency noise. Finally, the components and characteristics of the power line interference are researched, based on the characteristics of the interference, the revised blind source separation model is used to remove the power line interferences. Through analysis of simulation and practical application, results suggest that the proposed method can effectively eliminate those noise.

Laser systems for on-line laser ion sources

International Nuclear Information System (INIS)

Geppert, Christopher

2008-01-01

Since its initiation in the middle of the 1980s, the resonant ionization laser ion source has been established as a reliable and efficient on-line ion source for radioactive ion beams. In comparison to other on-line ion sources it comprises the advantages of high versatility for the elements to be ionized and of high selectivity and purity for the ion beam generated by resonant laser radiation. Dye laser systems have been the predominant and pioneering working horses for laser ion source applications up to recently, but the development of all-solid-state titanium:sapphire laser systems has nowadays initiated a significant evolution within this field. In this paper an overview of the ongoing developments will be given, which have contributed to the establishment of a number of new laser ion source facilities worldwide during the last five years.

Project development and commercialisation of on-line analysis systems

International Nuclear Information System (INIS)

Watt, J.S.

2000-01-01

A project team first in the Australian Atomic Energy Commission (AAEC) and since 1982 in CSIRO has developed many on-line analysis systems for the mineral and energy industries. The development of these projects, usually lasting 7-10 years, has followed a common pattern of laboratory R and D, field trials, commercialisation and technology transfer. This successful pattern is illustrated using examples of the development of systems for the on-line analysis of mineral slurries, for determination of the ash content of coal on conveyors, and for determination of the flow rates of oil, water and gas in pipelines. The first two systems, licensed to Australian companies, are used world-wide. They are now the market leaders for radioisotope gauges in their application field. The third, the multiphase flow meter, was licensed in 1997 to an international company. This meter has even greater potential than the other two systems for economic benefit from its use and for numbers of installations. (author)

A metal-organic framework nanocomposite made from functionalized magnetite nanoparticles and HKUST-1 (MOF-199) for preconcentration of Cd(II), Pb(II), and Ni(II)

International Nuclear Information System (INIS)

Ghorbani-Kalhor, Ebrahim

2016-01-01

The author describes the preparation of a magnetic metal organic framework of type MOF-199 containing magnetite (Fe 3 O 4 ) nanoparticles carrying covalently immobilized 4-(thiazolylazo) resorcinol (Fe 3 O 4 -TAR). This material is shown to represent a viable sorbent for separation and preconcentration of Cd(II), Pb(II), and Ni(II) ions. Box-Behnken design was applied to optimize the parameters affecting preconcentration. Following elution with 0.6 mol L −1 EDTA, the ions were quantified by FAAS. The capacity of the sorbent ranged between 185 and 210 mg g −1 . The limits of detection are 0.15, 0.40, and 0.8 ng mL −1 for Cd(II), Ni(II), and Pb(II) ions, respectively. The relative standard deviations are <8.5 %. The method was successfully applied to the rapid extraction of trace amounts of these ions from sea food and agri food. (author)

Estimation of Separation Buffers for Wind-Prediction Error in an Airborne Separation Assistance System

Science.gov (United States)

Consiglio, Maria C.; Hoadley, Sherwood T.; Allen, B. Danette

2009-01-01

Wind prediction errors are known to affect the performance of automated air traffic management tools that rely on aircraft trajectory predictions. In particular, automated separation assurance tools, planned as part of the NextGen concept of operations, must be designed to account and compensate for the impact of wind prediction errors and other system uncertainties. In this paper we describe a high fidelity batch simulation study designed to estimate the separation distance required to compensate for the effects of wind-prediction errors throughout increasing traffic density on an airborne separation assistance system. These experimental runs are part of the Safety Performance of Airborne Separation experiment suite that examines the safety implications of prediction errors and system uncertainties on airborne separation assurance systems. In this experiment, wind-prediction errors were varied between zero and forty knots while traffic density was increased several times current traffic levels. In order to accurately measure the full unmitigated impact of wind-prediction errors, no uncertainty buffers were added to the separation minima. The goal of the study was to measure the impact of wind-prediction errors in order to estimate the additional separation buffers necessary to preserve separation and to provide a baseline for future analyses. Buffer estimations from this study will be used and verified in upcoming safety evaluation experiments under similar simulation conditions. Results suggest that the strategic airborne separation functions exercised in this experiment can sustain wind prediction errors up to 40kts at current day air traffic density with no additional separation distance buffer and at eight times the current day with no more than a 60% increase in separation distance buffer.

UNISOR on-line nuclear orientation facility (UNISOR/NOF)

International Nuclear Information System (INIS)

Girit, I.C.; Alton, G.D.; Bingham, C.R.; Carter, H.K.; Simpson, M.L.; Cole, J.D.; Croft, W.L.; Hamilton, J.H.; Jones, E.F.; Gore, P.M.; Kormicki, J.; Xie, H.; Kern, B.D.; Krane, K.S.; Xu, Y.S.; Mantica, P.F. Jr.; Zimmermann, B.E.; Nettles, W.G.; Zganjar, E.F.; Kortelahti, M.O.; Newbolt, W.B.

1988-01-01

The UNISOR on-line nuclear orientation facility (UNISOR/NOF) consists of a 3 He- 4 He dilution refrigerator on line to the isotope separator. Nuclei are implanted directly into a target foil which is soldered to the bottom accessed cold finger of the refrigerator. A 1.5 T superconducting magnet polarizes the ferromagnetic target foils and determines the axis of symmetry. Up to eight gamma detectors can be positioned around the refrigerator, each 9 cm from the target. A unique feature of this system is that the k=4 term in the directional distribution function can be directly and unambigously deduced so that a single solution for the mixing ratio can be found. The first on-line experiment at this facility reported here was a study of the decay of the 191 Hg and 193 Hg isotopes. (orig.)

On-line test of power distribution prediction system for boiling water reactors

International Nuclear Information System (INIS)

Nishizawa, Y.; Kiguchi, T.; Kobayashi, S.; Takumi, K.; Tanaka, H.; Tsutsumi, R.; Yokomi, M.

1982-01-01

A power distribution prediction system for boiling water reactors has been developed and its on-line performance test has proceeded at an operating commercial reactor. This system predicts the power distribution or thermal margin in advance of control rod operations and core flow rate change. This system consists of an on-line computer system, an operator's console with a color cathode-ray tube, and plant data input devices. The main functions of this system are present power distribution monitoring, power distribution prediction, and power-up trajectory prediction. The calculation method is based on a simplified nuclear thermal-hydraulic calculation, which is combined with a method of model identification to the actual reactor core state. It has been ascertained by the on-line test that the predicted power distribution (readings of traversing in-core probe) agrees with the measured data within 6% root-mean-square. The computing time required for one prediction calculation step is less than or equal to 1.5 min by an HIDIC-80 on-line computer

REQUIREMENTS AND GUIDELINES FOR NSLS EXPERIMENTAL BEAM LINE VACUUM SYSTEMS-REVISION B

International Nuclear Information System (INIS)

FOERSTER, C.

1999-01-01

Typical beam lines are comprised of an assembly of vacuum valves and shutters referred to as a ''front end'', optical elements to monochromatize, focus and split the photon beam, and an experimental area where a target sample is placed into the photon beam and data from the interaction is detected and recorded. Windows are used to separate sections of beam lines that are not compatible with storage ring ultra high vacuum. Some experimental beam lines share a common vacuum with storage rings. Sections of beam lines are only allowed to vent up to atmospheric pressure using pure nitrogen gas after a vacuum barrier is established to protect ring vacuum. The front end may only be bled up when there is no current in the machine. This is especially true on the VUV storage ring where for most experiments, windows are not used. For the shorter wavelength, more energetic photons of the x-ray ring, beryllium windows are used at various beam line locations so that the monochromator, mirror box or sample chamber may be used in a helium atmosphere or rough vacuum. The window separates ring vacuum from the environment of the downstream beam line components. The stored beam lifetime in the storage rings and the maintenance of desirable reflection properties of optical surfaces depend upon hydrocarbon-free, ultra-high vacuum systems. Storage ring vacuum systems will operate at pressures of ∼ 1 x 10 -10 Torr without beam and ∼ 1 x 10 -9 Torr with beam. Systems are free of hydrocarbons in the sense that no pumps, valves, etc. containing organics are used. Components are all-metal, chemically cleaned and bakeable. To the extent that beam lines share a common vacuum with the storage ring, the same criteria will hold for beam line components. The design philosophy for NSLS beam lines is to use all-metal, hydrocarbon-free front end components and recommend that experimenters use this approach for common vacuum hardware downstream of front ends. O-ring-sealed valves, if used, are not

Preconcentration and extraction of copper(II on activated carbon using ethyl-2-quinolyl-β (p-carboxyphenyl hydrazonedioxo propionate

Directory of Open Access Journals (Sweden)

Mehrorang Ghaedi

2008-12-01

Full Text Available Activated carbon modified method was used for the preconcentration and determination of copper content in real samples such as tap water, wastewater and a synthetic water sample by flame atomic absorption spectrometry. The copper(II was adsorbed quantitatively on activated carbon due to its complexation with ethyl-2-quinolyl-β(p-carboxyphenyl hydrazonedioxo propionate (EQCPDP. The adsorbed copper(II ion on solid phase was eluted quantitatively by using nitric acid. The important parameters such as pH, amount of carrier, flow rate, amount of activated carbon and type and concentration of eluting agent for obtaining maximum recovery were optimized. The method at optimum conditions gives linear concentration range of 0.05-1.0 μg mL-1 of copper(II with correlation coefficient of 0.9994 and the detection limit of 0.99 ng mL-1. The preconcentration leads to enrichment factor of 175 and break through volume of 1750 mL. The method has good tolerance limit of interfering ions and selectivity and it has been successfully applied for determination of copper content in real sample such as blood, wastewater and river sample.

Preconcentration and determination of heavy metals in water, sediment and biological samples

Directory of Open Access Journals (Sweden)

Shirkhanloo Hamid

2011-01-01

Full Text Available In this study, a simple, sensitive and accurate column preconcentration method was developed for the determination of Cd, Cu and Pb ions in river water, urine and sediment samples by flame atomic absorption spectrometry. The procedure is based on the retention of the analytes on a mixed cellulose ester membrane (MCEM column from buffered sample solutions and then their elution from the column with nitric acid. Several parameters, such as pH of the sample solution, volume of the sample and eluent and flow rates of the sample were evaluated. The effects of diverse ions on the preconcentration were also investigated. The recoveries were >95 %. The developed method was applied to the determination of trace metal ions in river water, urine and sediment samples, with satisfactory results. The 3δ detection limits for Cu, Pb and Cd were found to be 2, 3 and 0.2 μg dm−3, respectively. The presented procedure was successfully applied for determination of the copper, lead and cadmium contents in real samples, i.e., river water and biological samples.

Chemically modified activated carbon with 1-acylthiosemicarbazide for selective solid-phase extraction and preconcentration of trace Cu(II), Hg(II) and Pb(II) from water samples.

Science.gov (United States)

Gao, Ru; Hu, Zheng; Chang, Xijun; He, Qun; Zhang, Lijun; Tu, Zhifeng; Shi, Jianping

2009-12-15

A new sorbent 1-acylthiosemicarbazide-modified activated carbon (AC-ATSC) was prepared as a solid-phase extractant and applied for removing of trace Cu(II), Hg(II) and Pb(II) prior to their determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The separation/preconcentration conditions of analytes were investigated, including effects of pH, the shaking time, the sample flow rate and volume, the elution condition and the interfering ions. At pH 3, the maximum static adsorption capacity of Cu(II), Hg(II) and Pb(II) onto the AC-ATSC were 78.20, 67.80 and 48.56 mg g(-1), respectively. The adsorbed metal ions were quantitatively eluted by 3.0 mL of 2% CS(NH2)2 and 2.0 mol L(-1) HCl solution. Common coexisting ions did not interfere with the separation. According to the definition of IUPAC, the detection limits (3sigma) of this method for Cu(II), Hg(II) and Pb(II) were 0.20, 0.12 and 0.45 ng mL(-1), respectively. The relative standard deviation under optimum conditions is less than 4.0% (n=8). The prepared sorbent was applied for the preconcentration of trace Cu(II), Hg(II) and Pb(II) in certified and water samples with satisfactory results.

FCC riser quick separation system: a review

Directory of Open Access Journals (Sweden)

Zhi Li

2016-10-01

Full Text Available Abstract The riser reactor is the key unit in the fluid catalytic cracking (FCC process. As the FCC feedstocks become heavier, the product mixture of oil, gas and catalysts must be separated immediately at the outlet of the riser to avoid excessive coking. The quick separation system is the core equipment in the FCC unit. China University of Petroleum (Beijing has developed many kinds of separation system including the fender-stripping cyclone and circulating-stripping cyclone systems, which can increase the separation efficiency and reduce the pressure drop remarkably. For the inner riser system, a vortex quick separation system has been developed. It contains a vortex quick separator and an isolated shell. In order to reduce the separation time, a new type of separator called the short residence time separator system was developed. It can further reduce the separation time to less than 1 s. In this paper, the corresponding design principles, structure and industrial application of these different kinds of separation systems are reviewed. A system that can simultaneously realize quick oil gas separation, quick oil gas extraction and quick pre-stripping of catalysts at the end of the riser is the trend in the future.

Micelle-mediated methodology for the preconcentration of uranium prior to its determination by flow injection

Energy Technology Data Exchange (ETDEWEB)

Fernandez Laespada, M E; Perez Pavon, J L; Moreno Cordero, B [Univ. de Salamanca (Spain). Dept. de Quimica Analitica, Nutricion y Bromatologia

1993-02-01

Cloud point extraction has been used for the preconcentration of uranium, prior to its determination by flow injection. The non-ionic surfactant employed was Triton X-114 and the reagent chosen to form a hydrophobic chelate of uranium was 1-(2-pyridylazo)-2-naphthol. The optimum conditions for the preconcentration and determination of uranium have been studied. This methodology has been applied to the determination of trace amounts of uranium in tap and river waters from Salamanca. (Author).

Slantingly cross loading sample system enables simultaneous performance of separation and mixture to detect molecular interactions on thin-layer chromatography.

Science.gov (United States)

Shimizu-Yumoto, Hiroko; Hayashi, Nobuyuki; Ichimura, Kazuo; Nakayama, Masayoshi

2012-07-06

Anthocyanins are major flower pigments that can be affected by copigments, colorless compounds that can modify anthocyanin coloration to more intense and bluer. Thin-layer chromatography (TLC) is an available technique to separate and analyze anthocyanins and copigments. To easily and comprehensively detect copigments, we added function of mixture of compounds to TLC; by slantingly cross loading samples on TLC, compounds are symmetrically developed at various angle lines from the upper origin to individual R(f) values and cross each other in an orderly fashion, where mixture is simultaneously performed with separation. Occurrence of copigments can be detected as a coloration change on the developed line of anthocyanin. Pink sweet pea (Lathyrus odoratus L.) petals were analyzed by the cross-TLC and a more intense spot and a paler spot on the anthocyanin line were detected. As each spot overlapped with an ultraviolet absorbance line, each of these ultraviolet absorption compounds was purified and identified as kaempferol 3-rhamnoside and 2-cyanoethyl-isoxazolin-5-one, respectively. Whereas kaempferol 3-rhamnoside is a flavonoid and had a general copigment effect of more intense and bluer coloration change, 2-cyanoethyl-isoxazolin-5-one is a compound whose structure is outside of conventional categories of copigments and had a novel effect to change anthocyanin coloration paler while maintaining color tone. We determined that the search for copigments should be carried out without pre-existing prediction of structures and effects. We have shown that slantingly cross loading samples system on plate-type chromatography is an effective technique for such comprehensive analysis of molecular interaction. Crown Copyright © 2012. Published by Elsevier B.V. All rights reserved.

Study on on-Line Measurement and Controlling System of the Foundation Trench-Leveling Machine

International Nuclear Information System (INIS)

Yi, J G; Jiang, H Y; Xing, Y Z; Chen, J; Liu, J T

2006-01-01

Research the system software and hardware composing, the control mode, the online measurement and control principle based on the laser receiver and the inclination sensor as the signal source. After the laser receiver accepts the laser signal, the laser signal is carried through the light filter treatment so as to reduce the sunlight interference, and then amplified and modulated, last transmitted to the control unit. The inclination sensor adapts XWQJ02-01S, measure the slope angle the x and y verticality direction. The error adjusting range is ±0.05 0 . The separate time treatment avoids simultaneously adjusting the laser and inclination signal to each other interfere. The on-line measurement and control system realizes the parts to work on the plane that parallels with the datum plane of the laser beam scan. The trench-leveling machine must retain ±0.05 0 with the datum plane. Adapting the least square method to fit the linear curve, the movement trend of the work parts on the work plane is judged through the slope number. The test result shows that thought the combination measurement and control of the laser and slope angle the leveling precision are ±5mm/100. Its can satisfy with the construction criterion request

LED-Based High-Voltage Lines Warning System

Directory of Open Access Journals (Sweden)

Eldar MUSA

2013-04-01

Full Text Available LED-based system, running with the current of high-voltage lines and converting the current flowing through the line into the light by using a toroid transformer, has been developed. The transformer’s primary winding is constituted by the high voltage power line. Toroidal core consists of two equal parts and the secondary windings are evenly placed on these two parts. The system is mounted on the high-voltage lines as a clamp. The secondary winding ends are connected in series by the connector on the clamp. LEDs are supplied by the voltage at the ends of secondary. Current flowing through highvoltage transmission lines is converted to voltage by the toroidal transformer and the light emitting LEDs are supplied with this voltage. The theory of the conversion of the current flowing through the line into the light is given. The system, running with the current of the line and converting the current into the light, has been developed. System has many application areas such as warning high voltage lines (warning winches to not hinder the high-voltage lines when working under the lines, warning planes to not touch the high-voltage lines, remote measurement of high-voltage line currents, and local illumination of the line area

Recent developments in automated determinations of trace level concentrations of elements and on-line fractionations schemes exploiting the micro-sequential injection - lab-on-valve approach

DEFF Research Database (Denmark)

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

2006-01-01

The determination of trace level concentrations of elements, such as metal species, in complex matrices by atomic absorption or emission spectrometric methods often require appropriate pretreatments comprising separation of the analyte from interfering constituents and analyte preconcentration...... are presented as based on the exploitation of micro-sequential injection (μSI-LOV) using hydrophobic as well as hydrophilic bead materials. The examples given comprise the presentation of a universal approach for SPE-assays, front-end speciation of Cr(III) and Cr(VI) in a fully automated and enclosed set...

Selective Flow Injection Analysis of Ultra-trace Amounts of Cr(VI), Preconcentration of It by Solvent Extraction, and Determination by Electrothermal Atomic Absorption Spectrometry (ETAAS)

DEFF Research Database (Denmark)

Nielsen, Steffen; Sturup, Stefan; Spliid, Henrik

1999-01-01

(IBMK). The Cr(VI) is complexed by reaction with ammonium pyrrolidine dithiocarbamate (APDC), and the non-charged Cr(VI)-PDC chelate formed is extracted into IBMK in a knotted reactor made from PTFE tubing. The organic extractant is separated from the aqueous phase by a gravity phase separator......(VI) was achieved after preconcentration for 99 s at a sample flow rate of 5.5 ml min-1, as compared to direct introduction of 55 mul of sample, yielding a detection limit (3sigma) of 3.3 ng l-1. The sampling frequency was 24.2 samples h-1. The proposed method was successfully evaluated by analyzing a NIST Cr...

Thin-layer chromatography - liquid chromatography, an ideal supplement demonstrated by the separation of lanthanoids

International Nuclear Information System (INIS)

Specker, H.; Hufnagel, A.

1984-01-01

All lanthanoids have been separated by thin-layer chromatography (TLC) with short retention times by using a mixture of ether/tetrahydrofurane (THF)/bis-(2-ethylhexyl)-phosphate (HDEHP)/nitric acid. The eluent was empirically tested by synergistic effects. The results have been transferred to high-performance liquid chromatography /HPLC). It was possible to use the same eluent in TLC and HPLC both for the analytical separation of all lanthanoids and for the separation of fission products. The experimental experience gained in HPLC could be applied to the pre-concentration of isotopes in TLC. Both methods excellently supplemented each other in the separation of lanthanoids. (orig.) [de

Development of Hplc Techniques for the Analysis of Trace Metal Species in the Primary Coolant of a Pressurised Water Reactor.

Science.gov (United States)

Barron, Keiron Robert Philip

Available from UMI in association with The British Library. The need to monitor corrosion products in the primary circuit of a pressurised water reactor (PWR), at a concentration of 10pg ml^{-1} is discussed. A review of trace and ultra-trace metal analysis, relevant to the specific requirements imposed by primary coolant chemistry, indicated that high performance liquid chromatography (HPLC), coupled with preconcentration of sample was an ideal technique. A HPLC system was developed to determine trace metal species in simulated PWR primary coolant. In order to achieve the desired detection limit an on-line preconcentration system had to be developed. Separations were performed on Aminex A9 and Benson BC-X10 analytical columns. Detection was by post column reaction with Eriochrome Black T and Calmagite Linear calibrations of 2.5-100ng of cobalt (the main species of interest), were achieved using up to 200ml samples. The detection limit for a 200ml sample was 10pg ml^{-1}. In order to achieve the desired aim of on-line collection of species at 300^circ C, the use of inorganic ion-exchangers is essential. A novel application, utilising the attractive features of the inorganic ion-exchangers titanium dioxide, zirconium dioxide, zirconium arsenophosphate and pore controlled glass beads, was developed for the preconcentration of trace metal species at temperature and pressure. The performance of these exchangers, at ambient and 300^ circC was assessed by their inclusion in the developed analytical system and by the use of radioisotopes. The particular emphasis during the development has been upon accuracy, reproducibility of recovery, stability of reagents and system contamination, studied by the use of radioisotopes and response to post column reagents. This study in conjunction with work carried out at Winfrith, resulted in a monitoring system that could follow changes in coolant chemistry, on deposition and release of metal species in simulated PWR water loops. On

Preconcentration of trace elements from high-purity thorium and uranium on Chelex-100 and determination by graphite furnace atomic absorption spectrometry with Zeeman-effect background correction

International Nuclear Information System (INIS)

Raje, Naina; Kayasth, Satish; Asari, T.P.S.; Gangadharan, S.

1994-01-01

Preconcentration of trace impurities from large-sized samples of uranium metal and thorium oxide using a small column of Chelex-100 followed by their determination using graphite furnace atomic absorption spectrometry (GFAAS) is reported. A 0.5-10-g amount of the sample (uranium metal or thorium oxide) was dissolved, complexed with ammonium carbonate and subjected to the ion-exchange procedure. The retained analytes were eluted with 2-4 M nitric acid and brought to a small volume for a final dilution to 10-25 ml for their determination using GFAAS. The validity of the separation procedure and recoveries at μg kg -1 levels was checked by standard addition; the recoveries were >95%

Radionuclide Sensors for Environmental Monitoring: From Flow Injection Solid-Phase Absorptiometry to Equilibration-Based Preconcentrating Minicolumn Sensors with Radiometric Detection

International Nuclear Information System (INIS)

Grate, Jay W.; Egorov, Oleg B.; O'Hara, Matthew J.; Devol, Timothy A.

2008-01-01

The development of in situ sensors for ultratrace detection applications in process control and environmental monitoring remains a significant challenge. Such sensors must meet difficult detection limit requirements while selectively detecting the analyte of interest in complex or otherwise challenging sample matrixes. Nowhere are these requirements more daunting than in the field of radionuclide sensing. The detection limit requirements can be extremely low. Nevertheless, a promising approach to radionuclide sensing based on preconcentrating minicolumn sensors has been developed. In addition, a method of operating such sensors, which we call equilibration-based sensing, has been developed that provides substantial preconcentration and a signal that is proportional to analyte concentration, while eliminating the need for reagents to regenerate the sorbent medium following each measurement. While this equilibration-based sensing method was developed for radionuclide sensing, it can be applied to nonradioactive species as well, given a suitable on-column detection system. By replacing costly sampling and laboratory analysis procedures, in situ sensors could have a significant impact on monitoring and long term stewardship applications. The aim of this review is to cover radionuclide sensors that combine some form of selective sorption with a radiometric detection method, and, as a primary aim, to comprehensively review preconcentrating minicolumn sensors for radionuclide detection. As a secondary aim, we will cover radionuclide sensors that combine sorption and scintillation in formats other than minicolumn sensors. We are particularly concerned with the detection of alpha- and beta-emitting radionuclides, which present particular challenges for measurements in liquid media

Magnetic separation technique for groundwater by five HTS melt-processed bulk magnets arranged in a line

International Nuclear Information System (INIS)