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A study was undertaken to ascertain the analytical capabilities of combined ICP–OES with ultrasonic nebulization to perform on-line preconcentration and speciation of inorganic V species in urine samples using a micro-column packed with l-methionine immobilized on controlled pore glass (CPG) as solid phase extractant. At pH 5.0, l-methionine is selective only towards V(V) while, total vanadium was...
The properties and behaviour of Hg depend on both the oxidation state and the chemical form: the bioavailability, toxicity, persistence and accumulation of mercury in the food web are strongly influenced by chemical speciation. The present work aims to determine the chemical forms of mercury present in soil and to evaluate the fraction of mercury in soil solution available to plants. In order to do...
This review summarizes and discusses the research carried out on the determination of antimony and its predominant chemical species in atmospheric aerosols. Environmental matrices such as airborne particulate matter, fly ash and volcanic ash present a number of complex analytical challenges as very sensitive analytical techniques and highly selective separation methodologies for speciation studies...
Isotopic exchange based approaches have for many years been applied in soil and solute research. However, acquiring and elaboration of experimental data were not always straightforward and complete. A strict and correct use of combined isotopic exchange-compartmental analysis may widen the knowledge database and provide information not available as yet. The experiments were carried out with arsenic...
This paper focuses on the analytical performance improvement of the coupled technique HPLC–ICPMS using on-line collision/reaction cell technology for selenium elemental and speciation analyses at the ng (Se) l −1 level in aquatic environment. Collision/reaction cell operating parameters were optimised, resulting in selected conditions of 5.5mlmin −1 H 2 and 0.5mlmin −1...
Thermodynamic and Raman spectroscopic speciation was used to define the operating conditions for an innovative cleaning treatment of the decayed carbonate-based stones using ion exchange technology. The conditioning process of the Lewatit OC1071 anion exchanger with EDTA (Y) was monitored by ionic chromatography. Characterisation of the initial (R–Cl) and the final (R 2 –H 2 Y) forms...
In this paper we report a comparison on the sequestering ability of some polycarboxylic ligands towards dioxouranium(VI) (UO 22+ , uranyl). Ligands taken into account are mono- (acetate), di- (oxalate, malonate, succinate and azelate), tri- (1,2,3-propanetricarboxylate) and hexa-carboxylate (1,2,3,4,5,6-benzenehexacarboxylate). The sequestering ability of polycarboxylic ligands towards...
Time-resolved synchrotron X-ray absorption near edge structure (XANES) spectroscopy was used to study changes of chromium speciation in soils upon soil–water interaction. The time resolution was 30–45min. In a flow-column apparatus operated near the synchrotron beamline, two different types of soil were treated with potassium-dichromate solution, and soil samples were taken and directly analysed by...
In this work, the reactions of various copper ions with 1,3,3-trimethyl-2-[5-(1,3,3-trimethyl-1,3-dihydro-indol-2-ylidene)-penta-1,3-dienyl]-3H-indolium – more commonly known as dimethylindodicarbocyanine polymethyne dye (DIDC) – as well as the application of the results obtained for the development of a spectrophotometric method for the determination of Cu(I), Cu(II) and Cu(III) are described. Cu(I)...
An on-line inorganic and organomercury species separation, preconcentration and determination system consisting of cold vapor atomic absorption spectrometry (CV-AAS or CV-ETAAS) coupled to a flow injection (FI) method was studied. The inorganic mercury species was retained on a column (i.d., 3mm; length 3cm) packed to a height of 0.7cm with a chelating resin aminopropyl-controlled pore glass (550Å)...
An isotope dilution method has been developed for the speciation analysis of chromium in natural waters which accounts for species interconversions without the requirement of a separation instrument connected to the mass spectrometer. The method involves (i) in-situ spiking of the sample with isotopically enriched chromium species; (ii) separation of chromium species by precipitation with iron hydroxide;...
Several solvent mixtures and techniques for the extraction of arsenic (As) species from rice flour samples prior to their analysis by HPLC–ICP-MS were investigated. Microwave-assisted extraction using water at 80°C for 30min provided the highest extraction efficiency. Total recoveries of extracted As species were in good agreement with the total As concentrations determined by ICP-MS after microwave-assisted...
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