Solid phase extraction of iron and lead in environmental matrices on amberlite xad-1180/pv

A solid phase extraction procedure using Amberlite XAD-1180/Pyrocatechol violet (PV) chelating resin for the determination of iron and lead ions in various environmental samples was established. The procedure is based on the sorption of lead(II) and iron(III) ions onto the resin at pH 9, followed by elution with 1 mol/L HNO3 and determination by flame atomic absorption spectrometry. The influence of alkaline, earth alkaline and some transition metals, as interferents, are discussed. The recoveries for the spiked analytes were greater than 95%. The detection limits for lead and iron by FAAS were 0.37 µg/L and 0.20 µg/L, respectively. Validation of the method described here was performed by using three certified reference materials (SRM 1515 Apple Leaves, SRM 2711 Montana Soil and NRCC-SLRS-4 Riverine Water). The procedure was successfully applied to natural waters and human hair.

Determinação simultânea de resíduos de cloranfenicol, tianfenicol e florfenicol em leite bovino por cromatografia eletrocinética micelar

A micellar electrokinetic chromatographic method (MEKC) is described for determining residues of amphenicols(chloramphenicol,thiamphenicol and florfenicol) in bovine milk. MEKC is conducted by using a separation buffer consisting of 20 mM Na2HPO4, 10 mM Na2B4O7, 50 mM SDS at pH 8.0; UV detection at 210 nm and 10 kV of voltage. The limit of detection ranged from 4.3-5.3 µg L-1. The MEKC method was applied for the simultaneous determination of amphenicols in milk samples spiked with amphenicols at three concentration levels: 10, 30 and 50 µg L-1. Recoveries ranging from 91-105% were obtained by following a simple extraction/preconcentration procedure.

Sistema aquoso bifásico: uma alternativa eficiente para extração de íons

Solvent extraction has been successfully applied to metal ion preconcentration and often meant the use of toxic organic diluents. However, regulatory pressure is increasingly focusing on the use and disposal of organic solvents, and thus the development of nonhazardous alternatives is important. In this review, we examine the application of aqueous biphasic systems (ABS) to extraction of ions, analyzing their potential and limitations and suggest that ABSs could be an efficient substitute for oil/water biphasic systems. ABSs are formed by mixing certain inorganic salts and water-soluble polymers, or by mixing two water-soluble polymers.

Pré-concentração de cádmio com Saccharomyces cerevisiae e determinação em águas fluviais usando espectrometria de emissão óptica com plasma indutivamente acoplado

A preconcentration method based on the use of Saccharomyces cerevisiae as sorbent material is proposed for the determination of Cd(II) in river water. The solid phase extraction was performed in batch mode and the determination of the analyte in the solid phase was easily carried out by introducing a slurry of the yeast (0.0625 g / 2.5 mL) directly into the ICP OES. A limit of detection of 0.11 µg L-1 and a sample throughput in the range of 4 - 54 sample h-1 were obtained. Determinations of cadmium in a certified sample and in real river water samples were in excellent agreement with the expected values.

Investigation of the occurrence of pesticide residues in rural wells and surface water following application to tobacco

In this work the exposure of wells and surface water to pesticides, commonly used for tobacco cropping, was assessed. Water consumption wells and surface water flows were sampled at different times. After a preconcentration step with solid phase extraction (SPE), the selected pesticides were determined by gas chromatography with electron capture detection (GC-ECD) or high performance liquid chromatography with diode array detection (HPLC-DAD). No pesticides were detected in the well water samples and surface water flow in the winter season. However, in the spring and summer higher concentrations of chlorpyrifos and imidacloprid were found in the water source samples. Atrazine, simazine and clomazone were also found. The occurrence of pesticides in collected water samples was related with the application to tobacco.

Cloud point extraction for the determination of copper in environmental samples by flame atomic absorption spectrometry

A simple cloud point extraction procedure is presented for the preconcentration of copper in various samples. After complexation by 4-hydroxy-2-mercapto-6-propylpyrimidine (PTU), copper ions are quantitatively extracted into the phase rich in Triton X-114 after centrifugation. Methanol acidified with 0.5 mol L-1 HNO3 was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). Analytical parameters including concentrations for PTU, Triton X-114 and HNO3, bath temperature, centrifugation rate and time were optimized. The influences of the matrix ions on the recoveries of copper ions were investigated. The detection limits (3SDb/m, n=4) of 1.6 ng mL-1 along with enrichment factors of 30 for Cu were achieved. The proposed procedure was applied to the analysis of environmental samples.

Microextração em fase líquida (LPME): fundamentos da técnica e aplicações na análise de fármacos em fluidos biológicos

The analysis of drugs and metabolites in biological fluids usually requires extraction procedures to achieve sample clean-up and analyte preconcentration. Commonly, extraction procedures are performed using liquid-liquid extraction or solid-phase extraction. Nevertheless, these extraction techniques are considered to be time-consuming and require a large amount of organic solvents. On this basis, microextraction techniques have been developed. Among them, liquid-phase microextraction has been standing out. This review describes the liquid-phase microextraction technique based on hollow fibers as a novel and promising alternative in sample preparation prior to chromatographic or electrophoretic analysis. The basic concepts related to this technique and its applicability in extraction of drugs are discussed.

Métodos de amostragem e análise para compostos reduzidos de enxofre atmosférico

This work presents a review of sampling and analytical methods that can be applied to atmospheric traces of reduced sulphur compounds (RSC) in the atmosphere. Sampling methodology involving discontinuous methods with preconcentration is mostly used. For the most part, adsorption on solids and cryogenic capture are applied as a procedure. The analysis of these compounds has been done mainly by gas chromatography with FPD, fluorescence and spectrophotometry. Advantages and disadvantages of the methodologies are also mentioned in this paper, aiming to guide the reader towards the most appropriate choice of a sampling and analytical method for RSCs.

Plasma polymerized acetaldehyde thin films for retention of volatile organic compounds

The aim of this work is the production and characterization of plasma polymerized acetaldehyde thin films. These films show highly polar species, are hydrophilic, organophilic and easily adsorb organic reactants with CO radicals but only allow permeation of reactants with OH radicals. The good step coverage of films deposited on aluminum trenches is useful for sensor development. Films deposited on hydrophobic substrates may result in a discontinued layer, which allows the use of preconcentration in sample pretreatment. Deposition on microchannels showed the possibility of chromatographic columns and/or retention system production to selectively detect or remove organic compounds from gas flows.

Estratégias de pré-concentração em eletroforese capilar (CE): parte 1. Manipulação da velocidade eletroforética do analito

Capillary electrophoresis has become a well-established and routine-based separation technique. It is based on the differences between charged analyte mobility in aqueous or organic electrolytes. Its major limitation is the sensitivity due to small sample injection volumes and the narrow diameter of the capillaries, especially when UV detection is used. There are a number of ways to increase the concentration sensitivity. This report shows some on-line preconcentration strategies to perform it in free solution capillary electrophoresis that are based on manipulation of the analyte electrophoretic velocity during the sample introduction (stacking, field amplification and transient isotachophoresis).

Estudo da adsorção de brometo de etídeo em resina XAD-7

The adsorption of ethidium bromide on XAD-7 resin was studied. The Freundlich model was the most representative isotherm model to describe the sorption behavior. A solid-liquid equilibrium model was proposed to explain the resin mass influence on the sorption. The equilibrium constant value estimated was 2.31. The results showed an ethidium bromide ion-pair physical adsorption, with adsorption enthalpy equals to -19.33 kJ/mol. A pK2 value equals to 4.69 ± 0.01 was estimated by two distinct methods. The results will be applied to the ethidium bromide preconcentration aiming its decomposition.

Emprego de sílica gel organicamente modificada e impressa ionicamente para pré-concentração seletiva on-line de íons cobre

The present work purposes the preparation of a silica gel sorbent organically modified with 2-aminoethyl-3-aminobutylmethyldimethoxysilane (AAMDMS) and imprinted with Cu2+ ions by means surface imprinting technique and its use for selective on-line sorbent preconcentration of Cu2+ ions with further UV-VIS spectrophotometric determination by flow injection analysis. The Cu2+-imprinted silica gel, when compared with non imprinted silica gel and silica gel, showed from the binary mixture of Cu2+/Ni2+ relative selectivity coefficient (k') of 6.84 and 5.43 and 6.64 and 19.83 for the mixture Cu2+/Pb2+, thus demonstrating higher selectivity of Cu2+-imprinted silica gel towards Cu2+ ions. Under optimized condition, the on-line preconcentration method provided detection limit of 3.4 μg L-1 and linear range ranging from 30.0 up to 300.0 μg L-1 (r = 0.995). The accuracy of method was successfully assessed by analyzing different kind of spiked water samples with recovery values ranging from 92.2 up to 103.0%.

Estratégias de pré-concentração em eletroforese capilar: parte 2. Manipulação da velocidade da fase dispersa/secundária

This work describes CE preconcentration strategies based on the effect of manipulation of the disperse/secondary velocity. Introduced by Terabe et al. in 1984, micellar electrokinetic chromatography is a powerful separation approach that increases the usage of electrokinetic phenomena for the separation of nonionic compounds. The main disadvantage of MEKC is the low concentration sensitivity associated with the limited optical path length for on-capillary photometric detection and the limited volume of sample solution that can be injected. This paper compiles on-line concentration strategies for neutral analytes by sample stacking and sweeping in micellar electrokinetic chromatography.

Estudo de sorção de herbicidas pelos argilominerais vermiculita e montmorilonita

The clay minerals montmorillonite (MT) and vermiculite (VT), previously treated with Ca2+, K+ and Na+, were employed in a sorption study with herbicides. The herbicides 2,4-D, diuron, alachlor and metolachlor showed no interaction with MT and VT. On the other hand, the triazines presented a good sorption process, close to 100% for ametrine removal and near to 56 and 69% for atrazine and simazine, respectively, by MT. These results suggest that the MT specie may be a good material for triazines removal from aqueous medium and an alternative phase to preconcentration process, besides to exhibit a good selectivity.

Pré-concentração de Cr(III) e análise de especiação de cromo empregando montmorilonita saturada com íons potássio

The clay mineral montmorillonite-K10 (MT), treated under acidic medium and saturated with potassium ions (MTK), was employed in sorption and desorption studies aiming the preconcentration of Cr(III) and the speciation analysis of chromium. The sorption process of Cr(III) was close to 100%, suggesting that MTK was a good material for Cr(III) preconcentration, although, the maximum recovery in HNO3 solution was near 89%. On the other hand, Cr(VI) practically was not retained in MTK, suggesting this material as an appropriate mineral phase to be used in speciation analysis of chromium in aqueous medium.