Indirect spectrofluorimetric determination of arsenic at nanotrace levels in alloys, underground water, industrial waters and sewage sludge

Abstract

An inexpensive and virtually specific nonextractive Spectrofluorimetric method for the determination of As(III) (1 ng/ml-1 μg/ml) in 0.18–1.08N H₂SO₄ has been developed. A known excess of Cr(VI) is allowed to quantitatively oxidize As(III) in the essential presence of a mixture of iodide and chloride as catalyst, followed by the addition of excess 2-(α-pyridyl) thioquinaldinamide and measurement of the fluorescence intensity (λ_em(max) = 488 nm λ_ex(max) = 360 nm) caused by Cr(VI) remaining after As(III) oxidation. The measurement is repeated without As(III) addition and the decrease in fluorescence intensity gives the As(III) concentration with the help of a calibration graph. The method is very precise and accurate (S. D. = ± 0.474, R. S. D. = 0.95%, for the analysis of 50ng/ml As(III), 11 replicates). The detection limit is 0.3ng/ml As(III). Large excesses of over fifty cations, anions and some complexing agents do not interfere. The method has been successfully applied for arsenic determination in various complex matrices: environmental waters, sewage sludges and several certified reference materials (alloys). This method has also been extended to determine As(V), after its reduction to As(III), in water samples, waste discharge water and sewage sludges.