Ek. Paleologos et al., SPECIATION ANALYSIS OF CR-III-CR-VI USING FLOW-INJECTION ANALYSIS WITH FLUOROMETRIC DETECTION, Analyst, 123(5), 1998, pp. 1005-1009
A relatively simple, sensitive, selective, automatic fluorimetric meth
od for the simultaneous determination of chromium(III) and chromium(vr
) by flow injection analysis (FIA) was developed, The method is based
on the selective oxidation of the non-fluorescing reagent 2-(alpha-pyr
idyl)thioquinaldinamide (PTQA), which with Cr-VI yields an intensely f
luorescent product (lambda(ex) = 360 nm; lambda(em) = 300 nm), Chromiu
m(III) is oxidized on-line to Cr-VI with sodium metaperiodate and the
Cr-VI is subsequently treated with PTQA, Fluorescence due to the sum o
f Cr-III and Cr-VI is measured and Cr-III is determined from the diffe
rence in fluorescence values. The effects of various analytical parame
ters, such as acidity, flow rate, sample volume, temperature, reagent
concentration and interfering species, were studied. Kinetic studies u
sing both the stopped-flow technique and the FIA procedure were utiliz
ed in order to study and optimise the oxidation conditions for Cr-III
On th, basis of its oxidation efficiency. The calibration graphs were
rectilinear in the ranges 0.1-10 mu g ml(-1) for Cr-VI and 0.1-1.0 mu
g ml(-1) for Cr-III, The method was successfully verified by performin
g recovery experiments of Cr in several standard reference materials (
peach leaves, sediments and tea), and it was applied to the speciation
analysis of Cr-III-Cr-VI in environmental waters (mineral, tap and di
stilled water), a food sample (tomato juice) and synthetic mixtures. U
p to 30 samples per hour can be analyzed with a relative standard devi
ation of about 0.1-2%.