[Note 6: On ignition the calcium oxalate loses carbon dioxide and carbon monoxide, leaving calcium oxide:
CaC_{2}O_{4}.H_{2}O —> CaO + CO_{2} + CO + H_{2}O.
For small weights of the oxalate (0.6 gram or less) this reaction may be brought about in a platinum crucible at the highest temperature of a Tirrill burner, but it is well to ignite larger quantities than this over the blast lamp until the weight is constant.]
[Note 7: The heat required to burn the filter, and that subsequently applied as described, will convert most of the calcium oxalate to calcium carbonate, which is changed to sulphate by the sulphuric acid. The reactions involved are
CaC_{2}O_{4} —> CaCO_{3} + CO,
CaCO_{3} + H_{2}SO_{4} —> CaSO_{4} + H_{2}O + CO_{2}.
If a porcelain crucible is employed for ignition, this conversion to sulphate is to be preferred, as a complete conversion to oxide is difficult to accomplish.]
[Note 8: The determination of the calcium may be completed volumetrically by washing the calcium oxalate precipitate from the filter into dilute sulphuric acid, warming, and titrating the liberated oxalic acid with a standard solution of potassium permanganate as described on page 72. When a considerable number of analyses are to be made, this procedure will save much of the time otherwise required for ignition and weighing.]
DETERMINATION OF MAGNESIUM
PROCEDURE.—Evaporate the acidified filtrates from the calcium precipitates until the salts begin to crystallize, but do !not! evaporate to dryness (Note 1). Dilute the solution cautiously until the salts are brought into solution, adding a little acid if the solution has evaporated to very small volume. The solution should be carefully examined at this point and must be filtered if a precipitate has appeared. Heat the clear solution to boiling; remove the burner and add 25 cc. of a solution of disodium phosphate. Then add slowly dilute ammonia (1 volume strong ammonia (sp. gr. 0.90) and 9 volumes water) as long as a precipitate continues to form. Finally, add a volume of concentrated ammonia (sp. gr. 0.90) equal to one third of the volume of the solution, and allow the whole to stand for about twelve hours.
Decant the solution through a filter, wash it with dilute ammonia water, proceeding as prescribed for the determination of phosphoric anhydride on page 122, including; the reprecipitation (Note 2), except that 3 cc. of disodium phosphate solution are added before the reprecipitation of the magnesium ammonium phosphate instead of the magnesia mixture there prescribed. From the weight of the pyrophosphate, calculate the percentage of magnesium oxide (MgO) in the sample of limestone. Remember that the pyrophosphate finally obtained is from one fifth of the original sample.