Evaluation of sample preparation methods for cereal digestion for subsequent As, Cd, Hg and Pb determination by AAS-based techniques.

Sample preparation methodsforcereal digestion were evaluated for the first time for subsequent As, Cd, Hg, and Pb determination by atomic absorption spectroscopy techniques. Microwave-assisted digestion (MW-AD) under high and medium pressure and microwave-induced combustion (MIC) were evaluated. The use of MIC made it possible to digest 700 mg of samples, and agreements of 97, 96, 100 and 92% were obtained for As, Cd, Hg and Pb, respectively, when 7 mol L-1 HNO3 was used as the absorbing solution. It was not necessary to dilute the digests obtained to avoid interferences in the quantification of As, Cd, Hg, and Pb. Although high pressure MW-AD was efficient for cereal digestion, interferences were observed on analyte determination. Limits of quantification obtained by MIC were 0.034 (As), 0.015 (Cd), 0.021 (Hg) and 0.105 (Pb) µg g-1, which are suitable to attain the maximum levels recommended by international agencies in cereal samples.

Determination of elemental impurities in poly(vinyl chloride) by inductively coupled plasma optical emission spectrometry.

In this work, a method for poly(vinyl chloride) (PVC) analysis by inductively coupled plasma optical emission spectrometry (ICP-OES) was developed. Samples were digested by microwave-induced combustion (MIC) and thirteen elements (Ba, Cd, Co, Cu, Fe, Mg, Mn, Mo, Ni, Pb, Sr, V and Zn) were determined by ICP-OES. Operational conditions of MIC were investigated allowing quantitative determination of all the analytes and suitable results were achieved using a 3 mol L(-1) HNO3 solution. Microwave-assisted wet digestion (MAWD) using closed quartz vessels and a single reaction chamber microwave digestion system (MAWD-SRC), were also evaluated for PVC digestion for results comparison. All the evaluated sample preparation methods were considered suitable for PVC digestion but MIC was preferable due to the possibility of using diluted HNO3 instead of concentrated reagents and due to the better digestion efficiency. The residual carbon content (RCC) in digests obtained by MIC was significantly lower in comparison with the values obtained after MAWD and by MAWD-SRC. Accuracy for the proposed method was better than 94% for all analytes by comparison of results with those obtained by neutron activation analysis (NAA). Using MIC, it was possible to digest a relatively high sample mass (500 mg) and up to 8 samples in less time (25 min) in comparison with MAWD and MAWD-SRC (about 60 min for both methods). The efficiency of digestion by MIC was higher 99% and lower limits of detection (as low as 0.1 µg g(-1)) were obtained avoiding the use of concentrated acids that is of great concern according to the current green chemistry recommendations.