Flow injection determination of selenium by successive retention of Se(IV) and tetrahydroborate(III) on an anion-exchange resin and hydride generation electrothermal atomization atomic absorption spectrometry with in-atomizer trapping: Part 1. Method development and investigation of interferences
A sample solution was passed at 20 ml min −1 through a column (150×4 mm 2) of Amberlite IRA-410Stron anion-exchange resin for 60 s. After washing, a solution of 0.1% sodium borohydride was passed through the column for 60 s at 5.1 ml min −1. Following a second wash, a solution of 8 mol l −1 hydrochl...
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Veröffentlicht in: | Spectrochimica acta. Part B: Atomic spectroscopy 1998-12, Vol.53 (14), p.1931-1943 |
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Zusammenfassung: | A sample solution was passed at 20
ml min
−1 through a column (150×4
mm
2) of Amberlite IRA-410Stron anion-exchange resin for 60
s. After washing, a solution of 0.1% sodium borohydride was passed through the column for 60
s at 5.1
ml
min
−1. Following a second wash, a solution of 8
mol
l
−1 hydrochloric acid was passed at 5.1
ml
min
−1 for 45
s. The hydrogen selenide was stripped from the eluent solution by the addition of an argon flow at 150
ml
min
−1 and the bulk phases were separated by a glass gas–liquid separator containing glass beads. The gas stream was dried by passing through a Nafion® dryer and fed, via a quartz capillary tube, into the dosing hole of a transversely heated graphite cuvette containing an integrated L’vov platform which had been pretreated with 120
μg of iridium as trapping agent. The furnace was held at a temperature of 250°C during this trapping stage and then stepped to 2000°C for atomization. The calibration was performed with aqueous standards solution of selenium (selenite, SeO
3
2−) with quantification by peak area. A number of experimental parameters, including reagent flow rates and composition., nature of the gas–liquid separator, nature of the anion-exchange resin, column dimensions, argon flow rate and sample pH, were optimized. The effects of a number of possible interferents, both anionic and cationic were studies for a solution of 500
ng
1
−1 of selenium. The most severe depressions were caused by iron (III) and mercury (II) for which concentrations of 20 and 10
mg
1
−1 caused a 5% depression on the selenium signal. For the other cations (cadmium, cobalt, copper, lead,. magnesium, and nickel) concentrations of 50–70
mg
1
−1 could be tolerated. Arsenate interfered at a concentration of 3
mg
−1, whereas concentrations of chloride, bromide, iodide, perchlorate, and sulfate of 500–900
mg
l
−1 could be tolerated. A linear response was obtained between the detection limit of 4
ng
1
−1, with a characteristic mass of 130
pg. The RSDs for solutions containing 100 and 200
ng
1
−1 selenium were 2.3% and 1.5%, respectively. |
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ISSN: | 0584-8547 1873-3565 |
DOI: | 10.1016/S0584-8547(98)00243-2 |