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A dispersive micro-solid phase extraction (DMSPE) with graphene as a solid adsorbent and ammonium pyrrolidinedithiocarbamate (APDC) as a chelating agent was proposed for speciation and detemination of inorganic selenium by the energy-dispersive X-ray fluorescence spectrometry (EDXRF). In developed DMSPE, graphene particles are dispersed throughout the analyzed solution, therefore reaction between...
Organotin compounds (OTCs) are heavily employed by industry for a wide variety of applications, including the production of plastics and as biocides. Reports of environmental prevalence, differential toxicity between OTCs, and poorly characterized human exposure have fueled the demand for sensitive, selective speciation methods. The objective of this investigation was to develop and validate a rapid,...
A new method based on dispersive liquid liquid microextraction (DLLME) combined with electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) was developed for the simultaneous speciation of inorganic arsenic (As), selenium (Se) and tellurium (Te) with sodium diethyldithiocarbamate (DDTC) as both chelating reagent and chemical modifier. As(III), Se(IV) and Te(IV) were...
Actinides determination in urine samples is part of the analyses performed to monitor internal contamination in case of an accident or a terrorist attack involving nuclear matter. Mineralisation is the first step of any of these analyses. It aims at reducing the sample volume and at destroying all organic compounds present. The mineralisation protocol is usually based on a wet ashing step, followed...
A selective separation method based on anion exchange cartridge was developed to determine antimony (Sb) speciation in biological matrices by graphite furnace atomic absorption spectrophotometry (GFAAS). The selectivity of the cartridge towards antimonite [SbIII] and antimonate [SbV] reversed in the presence of deionized (DI) water and 2mM citric acid. While SbV was retained by the cartridge in DI...
In this work, γ-mercaptopropyltrimethoxysilane (γ-MPTS) modified Fe3O4@SiO2 magnetic nanoparticles (MNPs) was successfully prepared, and characterized by Fourier transform infrared spectrometer (FT-IR), Transmission electron microscope (TEM) and Vibrating sample magnetometer (VSM). The sorption performance of the prepared Fe3O4@SiO2@γ-MPTS MNPs towards methylmercury (CH3Hg+) and inorganic mercury...
Speciation analysis of inorganic chromium in wastewater is of great significance for the monitoring of environmental pollution. In this work, N,N-bis(2-aminoethyl)ethane-1,2-diamine functionalized poly(chloromethyl styrene-co-styrene) was synthesized, characterized and used as the adsorbent to preconcentrate chromium species in environmental waters by on line solid-phase extraction (SPE). The trace...
A novel and environment friendly analytical method is reported for total chromium determination and chromium speciation in water samples, whereby tungsten coil atomic emission spectrometry (WCAES) is combined with in situ ionic liquid formation dispersive liquid–liquid microextraction (in situ IL-DLLME). A two stage multivariate optimization approach has been developed employing a Plackett–Burman...
The goal of this work is to emphasize the reliability of the thermal desorption technique in identifying mercury species. The analysis of mercury species in solids is essential for assessing the risk of disposal or re-use of mercury-contaminated materials. This study evaluates the accuracy and reliability of thermal desorption as a technique for identifying mercury species by means of different thermo-desorption...
Silver migration from a commercial baby feeding bottle and a food box containing AgNPs, as confirmed by SEM-EDX analysis, was evaluated using food simulant solutions [i.e., water, 3% (v/v) acetic acid, and 10% and 90% (v/v) ethanol]. Silver release was investigated at temperatures in the 20–70°C range using contact times of up to 10 days. Migration of silver from the food box was in all cases 2 to...
A highly sensitive and selective new procedure for the determination of silver in aqueous media was developed using a modified carbon paste electrode (MCPE) by differential pulse anodic stripping voltammetry (DPASV). The modified electrode was based on the incorporation of 2-hydroxybenzaldehyde benzoylhydrazone (2-HBBH) in the carbon paste electrode. Silver ions were preconcentrated on the modified...
Arsenic (As), Selenium (Se) and Mercury (Hg) are three trace elements that have been the subject of much analytical discussion and investigation over the last three decades. While Selenium (Se) is among the list of essential trace elements necessary for the regulation of metabolic processes and overall health, As and Hg are not, and have been the centre of various cases surrounding the contamination...
The presence of copper in wine is known to impact the reductive, oxidative and colloidal stability of wine, and techniques enabling measurement of different forms of copper in wine are of particular interest in understanding these spoilage processes. Electrochemical stripping techniques developed to date require significant pretreatment of wine, potentially disturbing the copper binding equilibria...
A rapid and effective suspended dispersive solid phase microextraction (SDSPME) was developed for the speciation of inorganic selenium using alumina nanoparticles functionalized with Aliquat-336. The target analytes were preconcentrated and determined by inductively coupled plasma optical emission spectrometry. Alumina nanoparticles were characterized using XRD, BET, SEM and EDX while the functionalized...
A new type of deep eutectic solvents (DESs) have been prepared and used as extraction solvents for ultrasound assisted-deep eutectic solvent based emulsification liquid phase microextraction method (UA-DES-ELPME) for the determination and speciation of total chromium, chromium(III) and chromium(VI). The chromium concentration in DES rich phase (extraction phase) was determined by using microsample...
A micro-solid phase extraction procedure for the separation and preconcentration of antimony based in the use of magnetic particles covered with silver nanoparticles functionalized with the sodium salt of 2-mercaptoethane-sulphonate (MESNa) is discussed. After separation by means of a magnetic field, the solid phase is directly introduced into an electrothermal atomizer for antimony determination...
High levels of vanadium have been reported in groundwater (<0.05–5300μgL−1 V) from different parts of Argentina, yet no detailed study of vanadium speciation has been performed. A highly selective strong anion exchange – solid phase extraction (SAX-SPE) method was used (in-situ) for vanadium speciation analysis of groundwater samples from La Pampa - LP (General San Martin and Eduardo Castex) and...
The speciation analysis of As in urine samples can provide important information for epidemiological studies. Considering that these studies involve hundreds or thousands of samples, a fast and reliable method using a simple LC system with short-length mixed bed ion exchange chromatographic column coupled to ICP-MS for As speciation in human urine samples was developed in this work. Separation of...
This work proposes the use of high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry (HPLC-ICP-MS) for simultaneous speciation of arsenic and chromium in iron supplements used for the treatment of anemia. The sample preparation procedure recommended for the total determination of arsenic and chromium was established using acid digestion in a microwave assisted...
A graphene oxide (GO) suspension was used to retain chromium (III) species in a neutral solution. The addition of Triton X-45 followed by heating resulted in a coacervate, to which the GO nanoparticles containing the analyte retained were transferred. Chromium was determined directly in the surfactant-rich phase by electrothermal atomic absorption spectrometry. The procedure was repeated using a second...
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