Flow injection hydride generation electrothermal atomic absorption spectrometry with in-atomizer trapping for the determination of lead in calcium supplements

Abstract

Lead hydride was generated from acid solution, containing potassium ferricyanide as an oxidizing agent, by the reaction with alkaline borohydride solution. The effects of reaction conditions (hydrochloric acid, ferricyanide and borohydride concentrations), and the lengths of reaction and stripping coils were studied. The effects of trapping temperature and argon flow rate were also investigated. Under the conditions giving the best peak area sensitivity, the detection limit (concentration giving a signal equal to three S.D. of the blank signal) was 0.12 mgl − 1 for a 1000 ml injection volume. The detection limit was improved to 0.03 mgl − 1 when the ferricyanide was purified b y passage through a cation-exchange resin. Two calcium supplement materials were analyzed by the flow i njection ( , respectively.

A Simple and Sensitive Flow-Injection On-line Preconcentration Coupled with Hydride Generation Atomic Fluorescence Spectrometry for the Determination of Ultra-trace Lead in Water, Wine, and Rice

“…23 observation obtained by HG-AAS. 21 The ethanol interference was attributed to variations in the pH and in the oxidationreduction potentials of substances present in the reaction medium. 31 However, in the present on-line preconcentration system, at least 40% ethanol could be tolerated without any significant effect on the Pb signal, thanks to separation of the matrix.…”

“…1,[19][20][21] However, for wine samples' analysis, ethanol matrix markedly suppresses the efficiency of lead hydride generation, 22 which calls for the development of simple on-line preconcentration and separation procedures. To date, such work dealing with the combination of flow injection/sequential injection on-line preconcentration and separation with hydride generation atomic fluorescence spectrometry (HG-AFS) is rare, 2 due to the narrow range of acidity required for the generation of lead hydride.…”

Determination of lead in wine and rum samples by flow injection-hydride generation-atomic absorption spectrometry

“…Better sensitivity was reported by using potassium ferricyanide, K 3 Fe(CN) 6 ), a relatively mild oxidant [15][16][17][18][19][20]. Lead hydride generation with a mixture of potassium ferricyanide and hydrochloric or nitric acid has been successfully applied to the determination of Pb in various samples, including soil and sediments [18,19], calcium matrices [20,21], urine [17], dialysis concentrates [15], geochemical deposits and paint [22].…”

Determination of trace lead in waters by flow injection hydride generation atomic absorption spectrometry

“…9,10 However, high blanks were found. The in-atomizer trapping procedure, which concentrate the lead in the atomizer prior to atomization, was reported by Tyson et al 11 In this procedure, has a greater sensitivity than that of direct introduction of the sample solution into the furnace, as a much larger volume of sample can be processed. The detection limit was 0.12 g L -1 for a 1000 L injection volume.…”

“…10,11 In this study, a flow injection hydride generation atomic absorption spectrometry (FI-HG-AAS) system was employed for lead determination. The merging zones approach to flow injection system utilizes the synchronized introduction of samples and reagents into unsegmented carrier streams.…”