Disclosed is a process for recovering and recycling waste methanesulfonic acid (MSA) and phosphorous acid (H.sub.3 PO.sub.3) in a bisphosphonation process for reuse in the process. The recovery process involves treating a waste crude mother liquor stream with HCl to remove sodium ion, as sodium chloride, recovering HCl--H.sub.2 O by atmospheric distillation, separating and dehydrating a mixture of methanesulfonic acid and phosphorous acid by vacuum distillation for recycle. The substantially dry methanesulfonic acid and phosphorous acid, and previous HCl, can all be recycled back to the process for reuse.