A closed inline system for sample digestion using 70% hydrogen peroxide and UV radiation. Determination of lead in...

This paper proposes a closed inline system for decomposition of wine, aiming at the determination of lead using electrothermal atomization atomic absorption spectrometry (ETAAS). The system is built using a 0.8 mm diameter PTFE tube, which is wrapped around an 8 W UV lamp. The sample in the presence of 70% hydrogen peroxide is circulated on an 8 W UV lamp at the flow rate of 1 mL min^-1 for 45 min. Under these conditions, the carbon content varied from 10% to 2% for a red wine sample before and after digestion, respectively. The system has allowed the determination of lead in wine samples using the analytical line 283.306 nm in the presence of aluminum as the chemical modifier and pyrolysis and atomization temperatures of 800 and 1800 °C, respectively. Then, lead can be quantified employing the external calibration technique with limits of detection 0.27 and quantification 0.89 µg L^-1, and characteristics mass of 18 pg. The precision expressed by relative standard deviation (RSD%) was 2.13%, calculated using six replicates of a digested solution of a wine sample with the lead content of 16.35 µg L^-1. For evaluation of the accuracy method, two wine samples were analyzed simultaneously by the method proposed and also by inductively coupled plasma mass spectrometry (ICP-MS). A statistical test demonstrated no significant difference between the means obtained by these two techniques. Also, experiments involving addition/recovery tests confirmed the method's accuracy. The system was employed for digestion and determination of lead in four Brazilian wine samples. The lead content varied from 2.19 to 43.48 µg L^-1.