Shake the mixture vigorously until mixed, allow to stand in the dark for 16 to 24 hours, and again weigh the flask and its contents. Weigh the flask and its contents, add to the phenol 1.13 times its weight of the iron–sulfuric acid solution prepared as directed, insert the stopper in the flask, and allow to stand, without cooling but with occasional mixing, until the phenol is liquefied. Solidify the phenol in an ice bath, breaking the top crust with a glass rod to ensure complete crystallization. Purify phenol by distillation, discarding the first 10% and the last 5%, collecting the distillate, with exclusion of moisture, in a dry, tared glass-stoppered flask of about twice the volume of the phenol. To 3 volumes of this solution contained in a volumetric flask add sulfuric acid, with cooling, to make 100 volumes. Mix, heat until effervescence ceases, and dilute with water to 50 mL. Dissolve 1.054 g of ferrous ammonium sulfate in 20 mL of water, and add 1 mL of sulfuric acid and 1 mL of 30 percent hydrogen peroxide.
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