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This method is for determining total fluoride in aluminosilicate catalysts and molecular sieves, and inorganic fluoride in aqueous samples. The method is particularly useful for catalysts containing zirconia or other metals that interfere with other procedures. The range of fluoride typically determined is from 0.005 to approximately 20 mass-% for catalysts or molecular sieves, and 0.005 to approximately 50 mass-% for aqueous samples.