Abstract:The lead ingot sample was dissolved with nitric acid (1+3). The pH of sample solution was adjusted to about 3.1 with ammonia and nitric acid (1+3). After adding 10 mL of 100 g/L manganese nitrate solution, 10 mL of 10 g/L potassium permanganate solution was added into 0.47-0.70 mol/L nitric acid at 70 ℃under stirring. The separation of bismuth from matrix lead was realized by the co-precipitation characteristic between manganese dioxide and bismuth. The precipitate was dissolved with hydrochloric acid-hydrogen peroxide mixture (49+2). The determination method of bismuth in lead ingots by flame atomic absorption spectrometry (FAAS) was established using 10%-25% (V/V) as determination medium and 223.1 nm as determination wavelength. Under the selected optimal instrumental conditions, the concentration of bismuth in range of 0.50-5.00 μg/mL showed good linearity to its corresponding absorbance with correlation coefficient of r=0.999 8. The detection limit of bismuth in this method was 0.002 8 μg/mL. The interference tests showed that the residual lead and other elements in lead ingots had no interference with the determination of bismuth. The experimental method was applied to the determination of bismuth in four lead ingot standard samples with mass fraction of 0.000 39%-0.062%. The found results were basically consistent with the certified values. The relative standard deviations (RSD, n=11) were between 0.67% and 8.1%. The recoveries were between 98% and 102%.
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