2003 Volume 19 Issue 9 Pages 1269-1275
A new sensitive chromogenic reagent, 9,10-phenanthaquinone monoethylthiosemicarbazone (PET), has been synthesized and used in the spectrophotometric determination of Tl(III). In HNO3, H2SO4 or H3PO4 acids, PET can react immediately at room temperature with Tl(III) to form a red 2:1 complex with a maximum absorption at 516 nm. The different analytical parameters affecting the extraction and determination processes have been examined. The calibration curve was found to be linear over the range 0.2 - 10 μg cm-3 with a molar absorptivity of 2.2 × 104 dm3 mol-1 cm-1 . Sandell’s sensitivity was found to be 0.0093 μg cm-2. No interference from macroamounts of foreign ions was detected, except for Pd(II). However, Pd(II) does not affect the determination process, because its complex with PET has its λmax at 625 nm. The proposed method has been applied to the determination of Tl(I and III) in synthetic and natural samples after separation by flotation (in oleic acid/kerosene) and solid-phase extraction (on polyurethane foam) techniques. The two methods were found to be accurate and not subject to random error, but solid-phase extraction was preferred because it is cheap, simpler and there is no contamination risk coming from flotation reagents.
