[Determination of lead with GFAAS using online flow injection].
A cheap, rapid and sensitive method for the determination of trace amount of lead in water samples by graphite furnace absorption spectrometry coupled with online flow injection preconcentration with ammonium pyrrolidine dithiocarboxylate chelating cellulose (CC-APDC) was developed. There were six steps in the preconcentration of flow injection: first, 0.15 mL nitric acid was used for a complete elution, which exceeded the volume of the graphite tube, so the 40 mL solution was removed before eluting. Secondly, 40 mL maximum concentration elution solution was added to GFAAS by fixed volume sampling to improve the accuracy. In addition, traditional stopping gas measurement was substituted with small flow gas atomization (30 mL x min(-1), preconcention for 1 min) during the removal of high memory effect for ashing stage in graphite furnace, which develops tail-out phenomenon and makes blank value low and steady. Various parameters affecting the adsorption and elution, such as pH of the solution, eluent concentration, sample flow rate etc, were optimized. If miniflow in atomization step was used, the memory effect in the determination of lead by GFAAS could be removed. The CC-APDC was used for preparation and preconcentration. A good precision (RSD = 1.4%, n = 10), high enrichment factor (15) and sample throughput (50 h) with detection limit 0.12 microg x L(-1) were obtained. This method has been successfully applied to the water sample for lead determination with a recovery of 95%-105%.
Chen
Zhong-Lan
ZL
Department of Chemistry, Sichuan Teacher's University, Nanchong 637002, China. czl831@yahoo.com.cn
D017022:Flow Injection Analysis; D006108:Graphite / Q000737:chemistry; D006863:Hydrogen-Ion Concentration; D007854:Lead / Q000032:analysis*; D011759:Pyrrolidines / Q000737:chemistry; D015203:Reproducibility of Results; D013054:Spectrophotometry, Atomic / Q000379:methods*; D013859:Thiocarbamates / Q000737:chemistry; D014874:Water Pollutants, Chemical / Q000032:analysis
D011759:Pyrrolidines; D013859:Thiocarbamates; D014874:Water Pollutants, Chemical; C020972:pyrrolidine dithiocarbamic acid; D007854:Lead; D006108:Graphite