Preparation of perchloric acid
50 grams of ammonium perchlorate are added to 60 ml of distilled water in a 500 ml beaker. 40 ml by volume of 68% nitric acid are added to the ammonium perchlorate solution and the solution is heated to a rolling boil (88-92°C). While heating, prepare a solution 15 ml of 30% hydrochloric acid in 25 ml distilled water. Once the ammonium perchlorate nitric acid solution is above 80° C, begin adding dropwise, the hydrochloric acid solution over a period of 25-30 minutes. The rate of addition should be sufficient to replace the lost water from boiling to ensure the volume remains constant. Once all the hydrochloric acid is added, allow the solution to boil for 30 minutes before increasing the heat to 135-140° C to drive off the remaining water, nitric and hydrochloric acids. The resultant solution should be pure perchloric acid. If there is any ammonium perchlorate remaining, it will crystalize out upon cooling.
The production of percholoric acid, Thesis by Horace C. Adams, 1925
PERCHLORIC ACID, 7601-90-3, UNII-V561V90BG2, CHEBI:29221, HSDB 1140, EINECS 231-512-4, UN1802, UN1873, Perchloric acid, >72% acid by mass [Forbidden], Perchloric acid standard solution, Perchlorsaeure, Ueberchlorsaeure, Hyperchloric acid, PERCHLORICACID, HClO4, hydroxidotrioxidochlorine, Perchloric acid solution, ACMC-1BEIA, AC1Q7DBV, Perchloric acid concentrate, AC1L2NB8, [ClO3(OH)], KSC379C1J, 30755_RIEDEL, 311421_ALDRICH, 319228_ALDRICH, 34288_RIEDEL, 35418_RIEDEL, 380083_ALDRICH, 38330_RIEDEL, CHEMBL1161634, 34288_FLUKA, 35418_FLUKA, 77227_FLUKA, 77228_FLUKA, 77232_FLUKA, 77233_FLUKA, 77234_FLUKA, CTK2H9114, 319228_FLUKA, MolPort-003-928-449, VLTRZXGMWDSKGL-UHFFFAOYSA-N, 30755_SIAL, 77228_SIAL, 77232_SIAL, 77233_SIAL, 77234_SIAL, V561V90BG2, 244252_SIAL, 311413_SIAL, Perchloric acid, >72% acid by mass, AKOS015843797, MCULE-1858636187, RL04894, RTR-024389, TRA0055236, UN 1802, Perchloric acid, >50% but not >72% acid, by mass [UN1873] [Oxidizer, Corrosive], AN-21793, IN001968, KB-59505, R240, SC-81648, Perchloric acid, not >50% acid, by mass, LS-102366, TR-024389, FT-0693827, 3B4-1616, I14-19670, Perchloric acid, >50% but not >72% acid, by mass, Perchloric acid, not >50% acid, by mass [UN1802] [Corrosive, Oxidizer], Perchloric acid, not >50% acid, by mass [UN1802] [Corrosive, Oxidizer], Perchloric acid, >50% but not >72% acid, by mass [UN1873] [Oxidizer, Corrosive], 101200-37-7, 102278-63-7, 106644-01-3, 111341-24-3, 119630-46-5, 139339-89-2, 143171-41-9, 153389-31-2, 200863-18-9, 47999-51-9, 766444-83-1, 845752-15-0, 90149-16-9, 92785-38-1, 957554-95-9, 95912-44-0, 95998-58-6
Perchlorate, PERCHLORATE ION, CID24247, Pca, LCP