A Sensitive Cloud Point Extraction–Spectrophotometric Determination of Vanadium Using Pyrogallol and Aliquat 336

A novel centrifuge-less cloud-point extraction (CL-CPE) method based on pyrogallol (PG) was developed for the spectrophotometric determination of total vanadium. The method employs a mixed micelle-mediated extraction system comprising the nonionic surfactant Triton X-114 and the ionic liquid Aliquat 336 (A336), which serves as a source of monovalent cations capable of forming an ion pair with the anionic vanadium–PG chelate. The extracted species, (A336+)[VIV(OH)(PG)2], exhibits several absorption maxima (309, 362, and 436 nm), providing enhanced selectivity through appropriate wavelength selection according to the sample matrix. The principal absorption maximum occurs at 309 nm. At a sevenfold preconcentration factor, the method provides high sensitivity at this wavelength, with a molar absorptivity of 3.2 × 107 L mol−1 cm−1, a limit of detection of 0.11 ng mL−1, and a Sandell sensitivity of 1.6 × 10−3 ng cm−2. The applicability of the method was demonstrated through the analysis of drinking water samples, spent vanadium catalyst materials, and vanadium-containing dietary supplements. The method was further evaluated using the RGBfast model, a white analytical chemistry assessment tool that integrates analytical performance, environmental sustainability, and practical and economic efficiency. The evaluation indicated a high overall whiteness score.