Search results for: speciation.

Authors: Karel Borovec, Jerzy Gorecki, Tadeas Ochodek

Abstract:

Combustion of solid fuels is one of the main sources of mercury in the environment. To reduce the amount of mercury emitted to the atmosphere, it is necessary to modify or optimize old purification technologies or introduce the new ones. Effective reduction of mercury level in the flue gas requires the use of speciation systems for mercury form determination. This paper describes tests and provides comparison of two industrial portable and continuous systems for mercury speciation in the flue gas: Durag HM-1400 TRX with a speciation module and the Portable Continuous Mercury Speciation System based on the SGM-8 mercury speciation set, made by Nippon Instruments Corporation. Additionally, the paper describes a few analytical problems that were encountered during a two-year period of using the systems.

Keywords: Mercury determination, speciation, continuous measurement, flue gas.

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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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Authors: Magdalena Jabłońska-Czapla

Abstract:

The work allowed gaining knowledge about redox and speciation changes of As, Cr and Sb ionic forms in Klodnica River water. This kind of studies never has been conducted in this region of Poland. In study optimized and validated previously HPLC-ICP-MS methods for determination of As, Sb and Cr was used. Separation step was done using high-performance liquid chromatograph equipped with ion-exchange column followed by ICP-MS spectrometer detector. Preliminary studies included determination of the total concentration of As, Sb and Cr, pH, Eh, temperature and conductivity of the water samples. The study was conducted monthly from March to August 2014, at six points on the Klodnica River. The results indicate that exceeded at acceptable concentration of total Cr and Sb was observed in Klodnica River and we should qualify Klodnica River waters below the second purity class. In Klodnica River waters dominates oxidized antimony and arsenic forms, as well as the two forms of chromium Cr(VI) and Cr(III). Studies have also shown the methyl derivative of arsenic's presence.

Keywords: Antimony, arsenic, chromium, HPLC-ICP-MS, river water, speciation.

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Authors: Mikko Mäkelä, Risto Pöykiö, Gary Watkins, Hannu Nurmesniemi, Olli Dahl

Abstract:

Trace element speciation of an integrated soil amendment matrix was studied with a modified BCR sequential extraction procedure. The analysis included pseudo-total concentration determinations according to USEPA 3051A and relevant physicochemical properties by standardized methods. Based on the results, the soil amendment matrix possessed neutralization capacity comparable to commercial fertilizers. Additionally, the pseudo-total concentrations of all trace elements included in the Finnish regulation for agricultural fertilizers were lower than the respective statutory limit values. According to chemical speciation, the lability of trace elements increased in the following order: Hg < Cr < Co < Cu < As < Zn < Ni < Pb < Cd < V < Mo < Ba. The validity of the BCR approach as a tool for chemical speciation was confirmed by the additional acid digestion phase. Recovery of trace elements during the procedure assured the validity of the approach and indicated good quality of the analytical work.

Keywords: BCR, bioavailability, trace element, industrialresidue, sequential extraction

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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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Authors: Michael P. Herring, Lavrent Khachatryan, Barry Dellinger

Abstract:

Low Temperature Matrix Isolation - Electron Paramagnetic Resonance (LTMI-EPR) Spectroscopy was utilized to identify the species of iron oxide nanoparticles generated during the oxidative pyrolysis of 1-methylnaphthalene (1-MN). The otherwise gas-phase reactions of 1--MN were impacted by a polypropylenimine tetra-hexacontaamine dendrimer complexed with iron (III) nitrate nonahydrate diluted in air under atmospheric conditions. The EPR fine structure of Fe (III)2O3 nanoparticles clusters, characterized by gfactors of 2.00, 2.28, 3.76 and 4.37 were detected on a cold finger maintained at 77 K after accumulation over a multitude of experiments. Additionally, a high valence Fe (IV) paramagnetic intermediate and superoxide anion-radicals, O2•- adsorbed on nanoparticle surfaces in the form of Fe (IV) --- O2•- were detected from the quenching area of Zone 1 in the gas-phase.

Keywords: Cryogenic trapping, EPFRs, dendrimer, Fe2O3 doped silica, soot.

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Authors: K. Benhabib, X. Pierens, V-D Nguyen, G. Mimanne

Abstract:

The main hypothesis of the dynamics of solid phase microextraction (SPME) is that steady-state mass transfer is respected throughout the SPME extraction process. It considers steady-state diffusion is established in the two phases and fast exchange of the analyte at the solid phase film/water interface. An improved model is proposed in this paper to handle with the situation when the analyte (atrazine) is in contact with colloid suspensions (carboxylate latex in aqueous solution). A mathematical solution is obtained by substituting the diffusion coefficient by the mean of diffusion coefficient between analyte and carboxylate latex, and also thickness layer by the mean thickness in aqueous solution. This solution provides an equation relating the extracted amount of the analyte to the extraction a little more complicated than previous models. It also gives a better description of experimental observations. Moreover, the rate constant of analyte obtained is in satisfactory agreement with that obtained from the initial curve fitting.

Keywords: Pesticide, SPME methods, polyacrylate, steady state.

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Authors: S. B. Otieno, T. S. Jayne, M. Muyanga

Abstract:

Selenium is an-antioxidant which is important for human health enters food chain through crops. In Kenya Zea mays is consumed by 96% of population hence is a cheap and convenient method to provide selenium to large number of population. Several soil factors are known to have antagonistic effects on selenium speciation hence the uptake by Zea mays. There are no studies in Kenya that has been done to determine the effects of soil characteristics (pH, Tcarbon, CEC, Eh) affect accumulation of selenium in Zea mays grains in Maize Belt in Kenya. About 100 Zea mays grain samples together with 100 soil samples were collected from the study site put in separate labeled Ziplocs and were transported to laboratories at room temperature for analysis. Maize grains were analyzed for selenium while soil samples were analyzed for pH, Cat Ion Exchange Capacity, total carbon, and electrical conductivity. The mean selenium in Zea mays grains varied from 1.82 ± 0.76 mg/Kg to 11±0.86 mg/Kg. There was no significant difference between selenium levels between different grain batches {χ (Df =76) = 26.04 P= 1.00} The pH levels varied from 5.43± 0.58 to 5.85± 0.32. No significant correlations between selenium in grains and soil pH (Pearson’s correlations = - 0.143), and between selenium levels in grains and the four (pH, Tcarbon, CEC, Eh) soil chemical characteristics {F (4,91) = 0.721 p = 0.579} was observed. It can be concluded that the soil chemical characteristics in the study site did not significantly affect the accumulation of native selenium in Zea mays grains.

Keywords: Maize, native, soil, selenium.

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