All about coffee by William H. Ukers

11. _Soluble Phosphoric Acid in the Ash--Official_

Acidify the solution of soluble ash, obtained in 9, with dilute nitric acid and determine phosphoric acid (P_2_O_5). For percentages up to 5 use an aliquot corresponding to 0.4 gram of substance, for percentages between 5 and 20 use an aliquot corresponding to 0.2 gram of substance, and for percentages above 20 use an aliquot corresponding to 0.1 gram of substance. Dilute to 75-100 cc., heat in a water-bath to 60°-65° C., and for percentages below 5 add 20-25 cc. of freshly filtered molybdate solution. For percentages between 5 and 20 add 30-35 cc. of molybdate solution. For percentages greater than 20 add sufficient molybdate solution to insure complete precipitation. Stir, let stand in the bath for about 15 minutes, filter _at once_, wash once or twice with water by decantation, using 25-30 cc. each time, agitate the precipitate thoroughly and allow to settle; transfer to the filter and wash with cold water until the filtrate from two fillings of the filter yields a pink color upon the addition of phenolphthalein and one drop of the standard alkali. Transfer the precipitate and filter to the beaker, or precipitating vessel, dissolve the precipitate in a small excess of the standard alkali, add a few drops of phenolphthalein solution, and titrate with the standard acid.