Electrothermal atomic absorption spectrometric determination of lead in high-purity reagents with flow-injection on-line microcolumn preconcentration and separation using a macrocycle immobilized silica gel sorbent

摘要

A fully automated procedure for the determination of ng l~(-1) amounts of lead has been developed using flow injection (FI) online column preeoncentration coupled with electrothermal atomic absorption spectrometry (ETAAS). The proposed FI manifold andits operation make possible the introduction of the total eluate volume into the graphite atomizer, avoiding the necessity for optimization of subsampling the eluate. The interference of other heavy metal ions due to competition for active sites of thesorbent is overcome using a highly selective macrocycle immobilized on silica gel (Pb-02). Lead is adsorbed on a microcolumn (50 μl) packed with Pb-02, and after washing the column with dilute nitric acid, air is introduced to remove all solution from the column and connecting tubing. The sorbed analyte is then eluted quantitatively into the graphite tube atomizer, preheated to 100°C, with 36 μ1 of ETDA solution (0,035 mol l~(-1), pH 10.5), propelled by air in order to minimize dispersion. The collection efficiency was 77% and with a sample loading flow rate of 3 ml min~(-1) and a 60 s preconcentration time, the enhancement factor was 77 and the throughput was 17 samples per hour. The relative standard deviation (n = 10) at the 300 ng l~(-1) level was 2.7%, and the detection limit (3σ) was 0,4 ng l~(-1). No interference from heavy metals was observed, but ions of Ba~(2+), Sr~(2+) and K~+ were found to interfere when the concentration ratios of interferent to lead exceeded values of 2000, 20 000 and 200000, respectively. Quantitative recovery of lead was achieved from sodium, magnesium, aluminum, lanthanum and heavy metal salt solutions. The high selectivity and sensitivity, combined with extremely low blank values, make the proposed technique particularly attractive for the analysis of high-purity reagents, semiconductors and other high-purity materials Results are presented for the determination of lead in some high-purity reagents.