The use of samples from students quotidian can get their attention for teaching contents to be presented. We have already presented a series of simple experiments demonstrating the use of flame atomic emission spectrometry in the determination of cations in samples present in our day life. Here sodium is determined in cachaça (sugar cane spirit), a very popular Brazilian drink, to demonstrate de effect of matrix composition and its physico-chemical properties in the volume of sample nebulized in a flame photometer and consequently in analytical signals by using different ethanol:water solvent mixtures for calibration.

Determination of Cr(VI) and Cr(III) was studied in soil samples accidentally contaminated with sulphochromic solution. Molecular absorption spectrophotometry based on the diphenylcarbazide method was used for the determination of Cr(VI) after its alkaline extraction. The total chromium concentration was determined using ICP OES. The quantification of Cr(III) was accomplished by subtracting the Cr(VI) concentration from the total chromium concentration. Regardless of the known contamination of the soil samples by sulphochromic solution, concentrations of Cr(VI) were below the detection limit. Addition and recovery experiments for Cr(VI) in soil samples with and without organic matter indicated its influence on the reduction of Cr(VI) to Cr(III).

A decomposição de amostras que contêm elevados teores de Si, utilizando mistura com os ácidos nítrico e fluorídrico, pode provocar a precipitação de fluoretos de Al(III), Ca(II), Fe(III) e Mg(II) durante a digestão, impedindo a recuperação total desses elementos. Visando minimizar esse problema, foram testados quatro procedimentos aplicados a diferentes amostras de solos. O procedimento mais eficiente envolveu a decomposição assistida por radiação microondas, seguida pela separação do material sólido residual com elevado teor de Si do sobrenadante ácido. A fração residual foi solubilizada usando HF concentrado e, após complexação com ácido bórico, essa solução foi misturada à fase líquida do digerido. Os teores de metais nos digeridos foram determinados por espectrometria de emissão óptica em plasma induzido (ICP OES) e a exatidão foi demonstrada aplicando o procedimento proposto em amostras provenientes do programa colaborativo International Soil-Analytical Exchange (ISE, Wegening Agricultural University, Holanda) e em amostra certificada de solo proveniente do National Institute of Standard and Technology (NIST, SRM 2709), que apresentou respectivamente, os seguintes percentuais de recuperação: 100,0 ± 2,6; 99,5 ± 1,9; 108,5 ± 2,7; 94,6 ± 8,9; 92,2 ± 9,7; 95,7 ± 1,8; 96,7 ± 2,7; 95,2 ± 0,6; 103,6 ± 2,6 e 96,1 ± 1,6 para, Al, Ba, Ca, Cr, Cu, Fe, Mg, Mn, V e Zn.

The use of pre-mixed nitric and hydrofluoric acids for the decomposition of samples containing high amounts of Si can cause the precipitation of Al(III), Ca(II), Fe(III), and Mg(II) fluorides during digestion, reducing the total recovery of these elements. Four procedures were applied to certified soil samples in an attempt to circumvent this problem. The most efficient procedure was based on microwave-assisted acid digestion decomposition of the samples, followed by separation of the residual silicate compounds. This fraction was solubilized using concentrated HF and the remaining fluoride ions were complexed by adding boric acid. This solution was mixed with the liquid phase of the acid digest. Elemental analysis of the acid digests was performed by inductively coupled plasma optical emission spectrometry (ICP-OES). The accuracy of the procedure was confirmed by applying it to samples provided by the International Soil-Analytical Exchange (ISE- Wageningen Agricultural University, Netherlands) and to certified soil reference material from the National Institute of Standards & Technology (NIST, SRM 2709). The following elemental recovery (%) was obtained: 100.0 ± 2.6; 99.5 ± 1.9; 108.5 ± 2.7; 94.6 ± 8.9; 92.2 ± 9.7; 95.7 ± 1.8; 96.7 ± 2.7; 95.2 ± 0.6; 103.6 ± 2.6 and 96.1 ± 1.6 for Al, Ba, Ca, Cr, Cu, Fe, Mg, Mn, V, and Zn, respectively.