Neste trabalho, o desenvolvimento de um método limpo de preparo de amostras para a análise de fertilizantes inorgânicos baseado em extração assistida por ultrassom usando um banho de ultrassom é descrito. Amostras (70 mg) foram sonicadas por 5 min na presença de 2 mL de HNO 3 50% (v/v) dentro de tubos de vidro. A determinação de cobre, chumbo e cádmio nos extratos foi realizada empregando espectrometria de absorção atômica com chama (FAAS). É também demonstrada a possibilidade de empregar um agitador vortex como fonte de agitação mecânica para realizar a extração dos metais. O método proposto usando banho de ultrassom ou agitador vortex é simples, versátil e minimiza a geração de resíduos devido ao emprego de volumes reduzidos de ácido e amostra, contribuindo para o desenvolvimento de um método analítico limpo.In this work, the development of a "green" sample preparation procedure for the analysis of inorganic fertilizers based on ultrasound-assisted extraction using an ultrasonic bath is described. Samples (70 mg) were sonicated for 5 min in the presence of 2 mL of 50% (v/v) HNO 3 inside glass tubes. The determination of copper, lead and cadmium in the extracts were carried out by flame atomic absorption spectrometry (FAAS). It is also demonstrated the possibility of using of a vortex shaker as a mechanical agitation source to perform the metal extraction. The proposed extraction procedure using an ultrasonic bath or a vortex shaker is simple and versatile, and minimizes waste generation due to the employment of reduced volumes of acid and sample, contributing for the development of a clean analytical method.
Keywords: fertilizer, ultrasound, vortex, metals, extraction
IntroductionInorganic fertilizers are a major source of metals in agricultural soils. Special attention is given to metals such as cadmium and lead due to their high toxicity. These metals can be absorbed by plants in agricultural lands and can reach the aquatic ecosystem health. Through rivers and streams, the metals are transported in suspended sediments or as dissolved species in water. The most deleterious effects of metal pollution in the aquatic environment are caused by the presence of dissolved metal species in water. 1 In this way, the quality control of fertilizers is of capital importance to prevent environmental pollution by metals. The official method established by the Brazilian Ministry of Agriculture (Ministério de Agricultura, Pecuária e Abastecimento, MAPA) for the analysis of inorganic fertilizers involves a sample preparation step prior to atomic absorption spectrometric determinations of metals. 2 The sample preparation procedure consists of wet digestion with concentrated hydrochloric (10 mL) and nitric (2.5 mL) acids in hot plate in order to release the analytes from the sample matrix. 2 The procedure takes around 40 min and employs large volumes of acids and sample, and consequently generates large amount of chemical waste in a routine laboratory. Moreover, the procedure is not adequate for the determination of volatile ...