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This method is for determining the alkalinity and fluoride content of alkaline solutions used for neutralization of HF in alkylation plants. Two procedures are included. The first procedure determines the alkalinity of the sample by colorimetric titration. The second procedure determines fluoride concentration using a fluoride ion-selective electrode. Fluoride, as mass-% KOH required for neutralization, is determined over a range of 0.016 to approximately 50 mass-%.