Espectrofotometría de absorción atómica con tubo en la llama: aplicación en la determinación total de cadmio, plomo y zinc en aguas frescas, agua de mar y sedimentos marinos

Thermospray flame furnace Atomic Absorption Spectrometry (TS-FF-AAS) was used for the total determination of Cd, Pb and Zn in fresh water and seawater samples at µg L-1 levels, and in marine sediment samples at µg g-1 levels. Using a sample loop of 50 µL and a peristaltic pump the samples were transported into the metallic tube placed over an air/acetylene flame, through a ceramic capillary (o.d. = 3.2 mm) containing two parallel internal orifices (i.d = 0.5 mm). The detection limits determined for Cd, Pb and Zn using a synthetic water matrix (2.5% m/v NaCl, 0.5% m/v MgCl2 and 0.8% m/v CaCl2) were 0.32 µg L-1; 2.6 µg L-1 and 0.21 µg L-1 respectively. The methodology by TS-FF-AAS was validated by determination of Cd, Pb and Zn in certified reference materials of water and marine sediment, and the t-test for differences between means was applied. No statistically significant differences were established in fresh water and seawater (p>0.05), whereas differences became apparent in marine sediment (p<0.03).

Análise de praguicidas organofosforados em água por extração em fase sólida (SPE) utilizando discos C18 e cromatografia em fase gasosa: avaliação da contaminação do reservatório de Furnas (MG-Brasil)

Solid phase extraction (SPE) in C18 disks has been optimized and validated for extraction of 5 organophosphorus (OP) pesticides in water. Extraction has been followed by separation and detection by gas chromatography/flame photometry. Excellent linearity was obtained for all compounds (r greater than 0.99), with CVs between 1.0-6.9%, recoveries between 73-95% and quantification limits between 2.5-5.0 µg L-1. Samples from Furnas dam were analyzed monthly during one year and 10% showed OP pesticide residues.

Síntese e caracterização de nanocompósitos Ni: SiO2 processados na forma de filmes finos

We have produced nanocomposite films of Ni:SiO2 by an alternative polymeric precursor route. Films, with thickness of ~ 1000 nm, were characterized by several techniques including X-ray diffraction, scanning electron microscopy, atomic force microscopy, flame absorption atomic spectrometry, and dc magnetization. Results from the microstructural characterizations indicated that metallic Ni-nanoparticles with average diameter of ~ 3 nm are homogeneously distributed in an amorphous SiO2 matrix. Magnetization measurements revealed a blocking temperature T B ~ 7 K for the most diluted sample and the absence of an exchange bias suggesting that Ni nanoparticles are free from an oxide layer.

Estudo do nitrogênio na combustão do gás natural

Nitrogen content in natural gas was studied in experimental and computational investigations to identify its influence on the emission level of exhaust gases from combustion facilities. Changes in natural gas composition with different N2 concentrations may result from introducing a new source gas into the system. An industrial burner fired at 75 kW, housed in a laboratory-scale furnace, was employed for runs where the natural gas/N2 proportion was varied. The exhaust and in-furnace measurements of temperature and gas concentrations were performed for different combustion scenarios, varying N2 content from 1-10 %v. Results have shown that the contamination of natural gas with nitrogen reduced the peak flame temperature, the concentration of unstable species, the NO X emission level and the heat transfer rate to the furnace walls, resulting from the recombination reactions.

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 de hidrocarbonetos voláteis e semi-voláteis na atmosfera

This paper focuses: (i) the development of a measurement technique for the determination of atmospheric C2-C6 hydrocarbons with sampling in canisters and analysis by gas chromatography/flame ionisation detector (GC/FID), (ii) the improvement of an existent adsorption-sampling technique with Tenax TA tubes for the determination of C6-C11 hydrocarbons and analysis by GC/FID after thermal desorption and cryogenic concentration, (iii) the identification of compounds present in ambient air by gas chromatography/mass spectrometry (GC/MS) for both canister and Tenax samples, (iv) a program of interlaboratorial comparison for quality control of C2-C11 analyses, and (v) the seasonal characterisation of ambient air C2-C11 hydrocarbons.

Desenvolvimento de um equipamento para avaliação do efeito do etanol na pressão de vapor e entalpia de vaporização em gasolinas automotivas

The quality of the gasoline utilized for fueling internal combustion engines with spark ignition is directly affected by the gasoline's properties. Thus, the fuel's properties must be in perfect equilibrium to allow the engine to perform optimally, not only insofar as fuel consumption is concerned, but also in order to reduce the emission of pollutants. Vapor pressure and vaporization enthalpy are important properties of a gasoline determining the fuel's behavior under different operating conditions in internal combustion engines. The study reported here involved the development of a device to determine the vapor pressure and the vaporization enthalpy of formulations containing volumes of 5, 15 and 25% of ethanol in four base gasolines (G1, G2, G3 and G4). The chemical composition of these gasolines was determined using a gas chromatographer equipped with a flame ionization detector (FID).

Determinação de contaminantes em óleos lubrificantes usados e em esgotos contaminados por esses lubrificantes

A simple and reliable ashing procedure is proposed for the preparation of used lubricating oil samples for the determination of Zn, Fe, Pb, Ni and Cu by the flame atomic absorption spectrometry technique. Sulphanilic acid was added to oil samples, the mixture coked and the coke ashed at 550 ºC. The solutions of the ash were analysed by flame AAS for these metals. The quantification limits were 38.250 µg g-1 for Zn, 4.550 µg g-1 for Fe, 1.562 µg g-1 for Pb, 1.450 µg g-1 for Ni, and 0.439 µg g-1 for Cu. The determinations, in lubricating oil, showed good precision and accuracy with recoveries between 90 and 110 %, indicating a negligible matrix effect in the experiments using addition of analyte, with relative standard deviation lower than 5%. The results for analysis of wastewater contamined by theses lubricants showed a very high relative standard deviation.

Validação em laboratório de método analítico para determinação do teor de adipato e ftalato de di-(2-etil-hexila) utilizados como plastificantes em filmes flexíveis de PVC

The validation of analytical methods was carried out for di-(ethylhexyl) phthalate (DEHP) and adipate (DEHA) the determination of in PVC films. The level of DEHP and DEHA in samples was determined by leaving the film in contact with n-heptane during 48 hours and analysis in a gas chromatograph (GC) equipped with a flame ionization detector and fused silica column with 5% phenylmethyl silicone in the dimensions 30 m x 0.53 mm x 2.65 mm. The results for detection and the quantification limits were smaller than the restriction limits. The recovery rates of DEHP and DEHA were, respectively, 69.10 and 75.30 %.

Avaliação da concentração de alguns íons metálicos em diferentes espécies de líquens do cerrado Sul-Mato-Grossense

Concentrations of Fe, Mn, Co, Cr, Zn and Cu were determinated using flame atomic absorption spectrometry in nine lichen species of the Sul-Mato-Grossense cerrado. The average metal ion concentrations varied in the following ranges: Fe, 248.41-1568.01; Mn, 98.50-397.33; Co, 10.08-24.81; Cr, 18.24-44.26; Zn, 14.62-34.79 and Cu, 3.23-7.57 mg kg-1. Statistical analysis (Pearson and Cluster) applied to the metal ion concentrations indicated that the accumulation of these ions can be due to several anthropogenic sources including agricultural activities, mineral exploration, biomass burning, soil mineral composition and leather tanning processes by chromium.

Urinary 2,5-hexanedione in workers exposed to n-hexane: influence of the sample treatment

The aim of the present study was to determine 2,5-hexanedione (2,5-HD), a metabolite of n-hexane, by gas chromatography/flame ionization detection in 31 workers exposed to n-hexane after two types of sample pretreatment, i.e., with (total 2,5-HD) and without (free 2,5-HD) acid hydrolysis. The mean urinary 2,5-HD was 0.52 mg/L (free) and 2.88 mg/L (total), this difference being significant (Student t-test, p < 0.05). The differences in the results according to the sample treatment support the need to modify the current Brazilian legislation, which proposes the analysis of 2,5-HD without indicating whether it is the free or total metabolite.

Butyltin speciation in sediments from Todos os Santos Bay (Bahia, Brazil) by GC-PFPD

Butyltin compounds were investigated in surface sediments from 17 stations in Todos os Santos Bay. Analytical conditions for organotin determination in marine sediments were optimized for GC with pulsed flame photometric detection. Detection limits were: 5.4 µg kg-1 for TBT; 0.2 µg kg-1 for DBT; and 2.1 µg kg-1 for MBT, using a 610-nm filter. In general, TBT concentrations were low and in the range of

Espectrometria de absorção atômica: o caminho para determinações multi-elementares

This paper present an overview of way covered for the spectrometry of atomic absorption (AAS), tracing a line of the historical events in its development and its establishment as a multielement technique. Additionally, the efforts carried by through several researchers in the search for the instrumental evolution, the advances, advantages, limitations, and trends of this approach are related. Several works focusing its analytical applications are cited employing simultaneous multielement determination by flame (FAAS) and/or graphite furnace (GF AAS), and fast sequential multielement determination using FAAS are reported in the present review.

Determinação de isotiocianato de benzila em Carica papaya utilizando cromatografia gasosa com detectores seletivos

In the present work, a method was developed and validated for the quantification of benzyl isothiocyanate (BITC) in the fruits of Carica papaya. The quantification of this compound was carried out by gas chromatography (GC) with selective detectors - nitrogen phosphorus detector (NPD) and flame photometric detector (FPD). The performance of these detectors showed a higher sensitivity of the NPD with a broader linear range of detection. The LOD/LOQ were 0.038/0.100 µg/mL for NPD and 5.78/19.29 µg/mL for FPD. The recovery of the method for BITC was 90,64%. An average value of BITC concentration in all the analyzed samples was 16,23 µg BITC/g.

Determinação de metil-etil-cetona em amostras de urina com amostragem por micro extração em fase sólida (MEFS) em headspace associada à cromatografia gasosa com detector de ionização de chama (CG-DIC)

Methyl ethyl ketone (MEK) is a solvent commonly used in chemical, paint and shoe industry. The aim of this study was to develop and validate a method for urinary quantification of MEK, employing headspace solid phase micro extraction sampling (SPME) coupled to gas chromatography with flame ionization detection (GC-FID). The calibration curve (y=4.6851x-0.0011) presented good linearity with r²=0.9993. Accuracy (94-109%), intra-assay precision (4.07-5.91%) and inter-assay precision (3.03-5.62%) were acceptable. The quantification limit was 0.19 mg/L. This low cost method can be used routinely in the biological monitoring of occupational exposure to MEK, according to the requirements of the Brazilian legislation.