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Fluorosilicic acid is generally obtained unintentionally in phosphate fertilizer manufacturers, particularly during wet phosphoric acid and triple superphosphate (TSP) production from fluorapatite. Since sustainability is a major environmental concern, phosphoric acid production factories have a fluorine recovery process as fluorinated products, mainly consisting of fluorosilicic acid (H2SiF6). To optimize the control of the fluorine recovery during the phosphate chemical process and to investigate the valorization alternatives of the concomitantly produced fluorosilicic acid, the main fluorine-based by-products have to be analyzed.