Search results for: Preconcentration
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 7

Search results for: Preconcentration

7 Extraction of Polystyrene from Styrofoam Waste: Synthesis of Novel Chelating Resin for the Enrichment and Speciation of Cr(III)/Cr(VI) Ions in Industrial Effluents

Authors: Ali N. Siyal, Saima Q. Memon, Latif Elçi, Aydan Elçi

Abstract:

Polystyrene (PS) was extracted from Styrofoam (expanded polystyrene foam) waste, so called white pollutant. The PS was functionalized with N,N- Bis(2-aminobenzylidene)benzene-1,2-diamine (ABA) ligand through an azo spacer. The resin was characterized by FT-IR spectroscopy and elemental analysis. The PS-N=N-ABA resin was used for the enrichment and speciation of Cr(III)/Cr(VI) ions and total Cr determination in aqueous samples by flame atomic absorption spectrometry (FAAS). The separation of Cr(III)/Cr(VI) ions was achieved at pH 2. The recovery of Cr(VI) ions was achieved ≥ 95.0% at optimum parameters: pH 2; resin amount 300mg; flow rates 2.0mL min-1 of solution and 2.0mL min-1 of eluent (2.0mol L-1 HNO3). Total Cr was determined by oxidation of Cr(III) to Cr(VI) ions using H2O2. The limit of detection (LOD) and quantification (LOQ) of Cr(VI) were found to be 0.40 and 1.20μg L-1, respectively with preconcentration factor of 250. Total saturation and breakthrough capacitates of the resin for Cr(IV) ions were found to be 0.181 and 0.531mmol g-1, respectively. The proposed method was successfully applied for the preconcentration/speciation of Cr(III)/Cr(VI) ions and determination of total Cr in industrial effluents.

Keywords: Styrofoam waste, Polymeric resin, Preconcentration, Speciation, Cr(III)/Cr(VI) ions, FAAS.

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6 Speciation, Preconcentration, and Determination of Iron(II) and (III) Using 1,10-Phenanthroline Immobilized on Alumina-Coated Magnetite Nanoparticles as a Solid Phase Extraction Sorbent in Pharmaceutical Products

Authors: Hossein Tavallali, Mohammad Ali Karimi, Gohar Deilamy-Rad

Abstract:

The proposed method for speciation, preconcentration and determination of Fe(II) and Fe(III) in pharmaceutical products was developed using of alumina-coated magnetite nanoparticles (Fe3O4/Al2O3 NPs) as solid phase extraction (SPE) sorbent in magnetic mixed hemimicell solid phase extraction (MMHSPE) technique followed by flame atomic absorption spectrometry analysis. The procedure is based on complexation of Fe(II) with 1, 10-phenanthroline (OP) as complexing reagent for Fe(II) that immobilized on the modified Fe3O4/Al2O3 NPs. The extraction and concentration process for pharmaceutical sample was carried out in a single step by mixing the extraction solvent, magnetic adsorbents under ultrasonic action. Then, the adsorbents were isolated from the complicated matrix easily with an external magnetic field. Fe(III) ions determined after facility reduced to Fe(II) by added a proper reduction agent to sample solutions. Compared with traditional methods, the MMHSPE method simplified the operation procedure and reduced the analysis time. Various influencing parameters on the speciation and preconcentration of trace iron, such as pH, sample volume, amount of sorbent, type and concentration of eluent, were studied. Under the optimized operating conditions, the preconcentration factor of the modified nano magnetite for Fe(II) 167 sample was obtained. The detection limits and linear range of this method for iron were 1.0 and 9.0 - 175 ng.mL−1, respectively. Also the relative standard deviation for five replicate determinations of 30.00 ng.mL-1 Fe2+ was 2.3%.

Keywords: Alumina-coated magnetite nanoparticles, magnetic mixed hemimicell solid-phase extraction, Fe(ΙΙ) and Fe(ΙΙΙ), pharmaceutical sample.

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5 Interaction of Electroosmotic Flow on Isotachophoretic Transport of Ions

Authors: S. Bhattacharyya, Partha P. Gopmandal

Abstract:

A numerical study on the influence of electroosmotic flow on analyte preconcentration by isotachophoresis ( ITP) is made. We consider that the double layer induced electroosmotic flow ( EOF) counterbalance the electrophoretic velocity and a stationary ITP stacked zones results. We solve the Navier-Stokes equations coupled with the Nernst-Planck equations to determine the local convective velocity and the preconcentration dynamics of ions. Our numerical algorithm is based on a finite volume method along with a secondorder upwind scheme. The present numerical algorithm can capture the the sharp boundaries of step-changes ( plateau mode) or zones of steep gradients ( peak mode) accurately. The convection of ions due to EOF reduces the resolution of the ITP transition zones and produces a dispersion in analyte zones. The role of the electrokinetic parameters which induces dispersion is analyzed. A one-dimensional model for the area-averaged concentrations based on the Taylor-Aristype effective diffusivity is found to be in good agreement with the computed solutions.

Keywords: Interfaces, Electroosmotic flow, QUICK Scheme, Dispersion, Effective Diffusivity.

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4 Supercritical Fluid Extraction of Lutein Esters from Marigold Flowers and their Hydrolysis by Improved Saponification and Enzyme Biocatalysis

Authors: A. Peter Amala Sujith, T.V. Hymavathi, P. Yasoda Devi

Abstract:

Lutein is a dietary oxycarotenoid which is found to reduce the risks of Age-related Macular Degeneration (AMD). Supercritical fluid extraction of lutein esters from marigold petals was carried out and was found to be much effective than conventional solvent extraction. The saponification of pre-concentrated lutein esters to produce free lutein was studied which showed a composition of about 88% total carotenoids (UV-VIS spectrophotometry) and 90.7% lutein (HPLC). The lipase catalyzed hydrolysis of lutein esters in conventional medium was investigated. The optimal temperature, pH, enzyme concentration and water activity were found to be 50°C, 7, 15% and 0.33 respectively and the activity loss of lipase was about 25% after 8 times re-use in at 50°C for 12 days. However, the lipase catalyzed hydrolysis of lutein esters in conventional media resulted in poor conversions (16.4%).

Keywords: lutein, preconcentration, saponification, lipase

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3 Amberlite XAD-4 Functionalized with 1-amino-2-naphthole for Determination and Preconcentration of Copper (II) in Aqueous Solution by Flame Atomic Absorption Spectrometry

Authors: Elham Moniri, Homayon Ahmad Panahi, Mahshid Nikpour Nezhati, Faranak Mahmoudi, Meghdad Karimi

Abstract:

A new chelating resin is prepared by coupling Amberlite XAD-4 with 1-amino-2-naphthole through an azo spacer. The resulting sorbent has been characterized by FT-IR, elemental analysis and thermogravimetric analysis (TGA) and studied for preconcentrating of Cu (II) using flame atomic absorption spectrometry (FAAS) for metal monitoring. The optimum pH value for sorption of the copper ions was 6.5. The resin was subjected to evaluation through batch binding of mentioned metal ion. Quantitative desorption occurs instantaneously with 0.5 M HNO3. The sorption capacity was found 4.8 mmol.g-1 of resin for Cu (II) in the aqueous solution. The chelating resin can be reused for 10 cycles of sorption-desorption without any significant change in sorption capacity. A recovery of 99% was obtained the metal ions with 0.5 M HNO3 as eluting agent. The method was applied for metal ions determination from industrial waste water sample.

Keywords: Amberlite XAD-4; Copper (II); Flame atomicabsorption; Chelator; 1-amino-2- naphthole

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2 Determination and Preconcentration of Iron (II) in Aqueous Solution with Amberlite XAD-4 Functionalized with 1-amino-2-naphthole by Flame Atomic Absorption Spectrometry

Authors: Homayon Ahmad Panahi, Mahshid Nikpour Nezhati, Faranak Mahmoudi, Elham Moniri, Meghdad Karimi

Abstract:

A new chelating resin is prepared by coupling Amberlite XAD-4 with 1-amino-2-naphthole through an azo spacer. The resulting sorbent has been characterized by FT-IR, elemental analysis and thermogravimetric analysis (TGA) and studied for preconcentrating of Fe (II) using flame atomic absorption spectrometry (FAAS) for metal monitoring. The optimum pH value for sorption of the iron ions was 6.5. The resin was subjected to evaluation through batch binding of mentioned metal ion. Quantitative desorption occurs instantaneously with 0.5 M HNO3. The sorption capacity was found 4.1 mmol.g-1 of resin for Fe (II) in the aqueous solution. The chelating resin can be reused for 10 cycles of sorption-desorption without any significant change in sorption capacity. A recovery of 97% was obtained the metal ions with 0.5 M HNO3 as eluting agent. The method was applied for metal ions determination from industrial waste water sample.

Keywords: Amberlite XAD-4, Iron (II), Flame atomic absorption, Chelator, 1-amino-2- naphthole

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1 Preconcentration and Determination of Cyproheptadine in Biological Samples by Hollow Fiber Liquid Phase Microextraction Coupled with High Performance Liquid Chromatography

Authors: Najari Moghadam Sh., Qomi M., Raofie F., Khadiv J.

Abstract:

In this study, a liquid phase microextraction by hollow fiber (HF-LPME) combined with high performance liquid chromatography-UV detector was applied to preconcentrate and determine trace levels of Cyproheptadine in human urine and plasma samples. Cyproheptadine was extracted from 10 mL alkaline aqueous solution (pH: 9.81) into an organic solvent (n-octnol) which was immobilized in the wall pores of a hollow fiber. Then was back-extracted into an acidified aqueous solution (pH: 2.59) located inside the lumen of the hollow fiber. This method is simple, efficient and cost-effective. It is based on pH gradient and differences between two aqueous phases. In order to optimize the HF-LPME some affecting parameters including the pH of donor and acceptor phases, the type of organic solvent, ionic strength, stirring rate, extraction time and temperature were studied and optimized. Under optimal conditions enrichment factor, limit of detection (LOD) and relative standard deviation (RSD(%), n=3) were up to 112, 15 μg.L−1 and 2.7, respectively.

Keywords: Biological samples, Cyproheptadine, hollow fiber, liquid phase microextraction.

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