Alterations in morphometric and organosomatic indices and histopathological analyses indicative of environmental contamination in Mullet, Mugil liza, from Southeastern Brazil.

Mullet (Mugil liza) were sampled in five different areas along the Guanabara Bay, southeastern Brazil, classified as non-contaminated, moderately contaminated and contaminated. Morphometric (Fulton condition factor, relative condition factor and weight to length scaling coefficient) and organosomatic (hepatosomatic index) indices of environmental stress were analysed. Fish from the differentially contaminated areas show statistically different Fulton and relative condition factors and hepatosomatic indices, but not the weight to length scaling coefficient. The Kn and the FCF followed the same trend, with fish from São Gonçalo (1.07 ± 0.04 and 0.89 ± 0.03), Itaipu (0.84 ± 0.01 and 0.86 ± 0.01) and the Rodrigo de Freitas Lagoon (1.03 ± 0.01 and 0.87 ± 0.20) showing higher FCFs than fish from Magé (0.96 ± 0.01 and 0.81 ± 0.01). Fish from Itaipu showed significantly higher HSI values than the other sampling sites (1.68 ± 0.07), with fish from Olaria and Ipiranga showing the lowest (1.56 ± 0.12 and 1.60 ± 0.07, respectively).

On-line mercury and methylmercury pre-concentration by adsorption of their dithiophosphoric acid diacyl ester chelates on a C18 column and cold-vapor atomic-absorption detection.

The pre-concentration of mercury(II) and methylmercury by adsorption of their dithiophosphoric acid diacyl ester (DDTP) chelates on a C18 column, then detection with cold-vapor atomic-absorption spectrometry was investigated. Conditions such as sample pH, reductant and chelating agent flow and concentration, and eluent and carrier gas flow were optimized. Optimization was performed by use of evolutionary operation with a proper factorial design. At a sample flow of 5.3 mL min(-1) and a loading time of 4.5 min, column adsorption efficiency ranged from 88 to 93% for both species. Detection limits down to 10 ng L(-1) were obtained at a sample throughput of 12 h(-1). There was good agreement between found and certified values in the analysis of certified reference materials after their microwave-assisted mineralization with HNO3 and H2O2.

Fourier transform infrared spectrometric determination of Ziram.

A procedure has been developed for vapour-phase Fourier transform infrared determination of Ziram, a dithiocarbamate pesticide. The method is based on the evolution of CS(2), after decomposition of the dithiocarbamate with diluted H(2)SO(4) at 50 degrees C. The CS(2) evolved was swept by a carrier flow of nitrogen to a laboratory-made infrared gas cell of 39 mm pathlength and 490 mul volume. The signals were registered as a function of time. The area of peaks obtained from absorbance measurement in the wavenumber range between 1600 and 1450 cm(-1) were interpolated in a calibration line established from Ziram standards treated in the same way as samples. The method provided an absolute limit of detection of 0.055 mg, a variation coefficient of the order of 6% for an analyte mass of 50 mg, and an analysis time of 3.5 min.

Flow injection-FTIR determination of dithiocarbamate pesticides.

A flow injection Fourier transform infrared spectrometric procedure has been developed for the determination the dithiocarbamate pesticides Ziram and Thiram in solid samples. All the operations involved, such as extraction, filtration and measurement, were integrated in the experimental set-up in order to avoid excessive manipulation of samples and standards. Ultrasonic assisted and mechanical extraction were evaluated for the solubilization of the analytes and, additionally, the effect of carrier flow rate, sample loop volume and the ratio between sample mass and volume of solvent employed were studied. Quantitative extractions with chloroform were obtained for both Ziram and Thiram, after 5 and 2 min, respectively, of mechanical shaking of sample slurries. Absorbance measurement, in the wavenumber range of 1600-1460 cm-1 for Ziram and 1400-1315 cm-1 for Thiram, was carried out, and the area values of the peaks obtained, as a function of time, were interpolated in external calibration lines prepared from standard solutions of Ziram and Thiram in chloroform. Analyses of commercial formulations and spiked soil samples incubated two weeks were in a good agreement with values found by other methodologies. Absolute detection limits of 400 micrograms for Ziram and 785 micrograms for Thiram and variation coefficients of 6.4% and 2.5% were obtained by use of the aforementioned methodology.

Fourier transform infrared determination of CO2 evolved from carbonate in carbonated apatites.

A quantitative method based on FTIR has been developed to determine carbonate in synthetic apatites. The method measures the evolved CO2 after reaction of 50 mg apatite with 2 mL of hydrochloric acid (0.5 M) in a reaction vessel, heated to 40 degrees C. The CO2 evolved was swept by a carrier of nitrogen to a laboratory-made infrared gas cell of 39 mm pathlength and 490 microL volume. The signals were recorded as a function of time and the areas of the chemigram peaks obtained from the measurements in the wavenumber range of 2,500-2,150 cm(-1), were interpolated using a calibration curve. The method can be used to study apatites with carbonate contents below 0.2% with a sampling frequency of 8 h(-1).

Determination of cadmium in whole blood and urine electrothermal atomic absorption spectrometry using palladium-based modifiers and in situ decontamination.

The determination of Cd in whole blood and urine by electrothermal atomic absorption spectrometry using Pd-based modifiers and in situ decontamination was studied. The performance of Pd, Pd + NH4NO3, and Pd + Mg(NO3)2 as modifiers were compared with respect to maximum pyrolysis and atomization temperatures, background attenuation, linear calibration range and matrix interference. Samples were diluted (1 + 4) with 0.1% Triton X-100 (blood) or 0.2% HNO3 (urine), and introduced onto the graphite tube platform already containing the in situ dried and decontaminated modifier. The influence of modifier volume and concentration, as well as that of the dilution ratio was investigated. The proposed procedure involves the use of Pd(NO3)2 + (Mg(NO3)2 as modifier, a pyrolysis temperature of 700 degree C and an in situ decontamination step of 1200 degrees C. The atomization temperature was 1700 degrees C. The detection limit (n = 10, k = 3) was 0.22 micrograms l-1 for both samples. Typical relative standard deviation values (n = 3) were below 3%. Using matrix-matched standards, good agreement was observed between experimental and reference values in the analysis of certified reference materials. Interlaboratory comparison data have confirmed the validity of the proposed analytical procedure.