Interference of salts on the determination of lead by electrothermal atomic absorption spectrometry. Ion chromatographic study

The influence of various salts on the atomization signal of lead has been examined by using a transverse heated atomic absorption spectrometer. To get more information about interference mechanisms, volatilization of salts has been studied by ion chromatographic analysis of the residue left on the furnace after drying or charring. The use of a Pd/Mg chemical modifier in these model solutions has also been examined. In 0.1 M chloride medium, NaCl, MgCl2 and CaCl2 do not interfere significantly. However, their different behaviour in the furnace, and particularly hydrolysis of MgCl2 influence greatly the charring curves of Pb. The use of a Pd/Mg modifier appears interesting only in the case of NaCl. Indeed, Pd stabilizes Pb sufficiently to permit the removal of NaCl by charring. In the case of MgCl2, Pb is not sufficiently stabilized to remove chloride through hydrolysis of MgCl2 or volatilization of MgCl2. In the presence of CaCl2, the Pb signal is delayed and coincides with the background absorption signal of CaCl2; the stabilization effect is not sufficient to eliminate CaCl2 by charring before atomization. At 0.1 M nitrate concentration, the presence of NaNO3, Mg(NO3)(2), and particularly Ca(NO3)(2), greatly modifies the atomization signal shape of Pb. Pb is more stabilized in nitrate medium, but losses are observed at the decomposition step of nitrate salts. In this medium, the stabilization effect of Pd leads to a single peak signal and permits elimination of nitrate decomposition products before atomization. Interference effects are more important in the presence of 0.1 M sulphate salts and increase with the acidity of the medium. Na2SO4, which is reduced to Na2S on the graphite, does not interfere significantly. However, the decomposition products of MgSO4 and CaSO4 induce an important interference effect on the determination of Pb which is stabilized in the furnace. In the case of Na2SO4, the use of the Pd/Mg modifier delays the atomization signal which coincides with the background absorption signal, leading to an important interference effect which cannot be eliminated by charring. In the presence of MgSO4 and CaSO4, the stabilizing effect of Pd permits the elimination of decomposition products of sulphate salts before atomization and suppresses the chemical interference effect.