Use of constrained mixture design for optimization of method for determination of zinc and manganese in tea leaves employing slurry sampling Original Research Article

A slurry suspension sampling technique has been developed for manganese and zinc determination in tea leaves by using flame atomic absorption spectrometry. The proportions of liquid-phase of the slurries composed by HCl, HNO3 and Triton X-100 solutions have been optimized applying a constrained mixture design. The optimized conditions were 200 mg of sample ground in a tungsten carbide balls mill (particle size < 100 μm), dilution in a liquid-phase composed by 2.0 mol L−1 nitric, 2.0 mol L−1 hydrochloric acid and 2.5% Triton X-100 solutions (in the proportions of 50%, 12% and 38% respectively), sonication time of 10 min and final slurry volume of 50.0 mL. This method allowed the determination of manganese and zinc by FAAS, with detection limits of 0.46 and 0.66 μg g−1, respectively. The precisions, expressed as relative standard deviation (RSD), are 6.9 and 5.5% (n = 10), for concentrations of manganese and zinc of 20 and 40 μg g−1, respectively. The accuracy of the method was confirmed by analysis of the certified apple leaves (NIST 1515) and spinach leaves (NIST 1570a). The proposed method was applied for the determination of manganese and zinc in tea leaves used for the preparation of infusions. The obtained concentrations varied between 42 and 118 μg g−1 and 18.6 and 90 μg g−1, respectively, for manganese and zinc. The results were compared with those obtained by an acid digestion procedure and determination of the elements by FAAS. There was no significant difference between the results obtained by the two methods based on a paired t-test (at 95% confidence level).