The nitric acid is estimated by the ferrous iron or other appropriate
method in another portion of the substance.
This method can be used even when the fertilizer contains ammonium
magnesium phosphate. In this case digest one gram for fifteen hours in
dilute soda-lye solution, which easily dissolves the ammonium magnesium
phosphate. Filter and wash the insoluble part with the tannin solution.
The residue is treated as above. The filtered solution distilled with
soda-lye furnishes the ammonia. The nitrates are estimated by one of
the methods above mentioned.
=205. Nitric Nitrogen.=—The methods of estimating nitric nitrogen,
both when present in weighable quantities and as mere traces have
been sufficiently described in the first volume. For convenience,
however, the standard methods of procedure will be given here. The
moist combustion methods adapted to nitrates and the volumetric copper
oxid process have already been described. Of the reduction methods
the process of Ulsch is one of the easiest of application and also
reliable. As practiced by the official chemists the manipulation is
conducted as described in the first volume, page 539.
=206. Ulsch Method, Applicable to Mixed Fertilizers.=—The method of
Ulsch which is found to give good results with pure nitrates or with
nitrates in the absence of other forms of nitrogen may also be adapted
to mixed fertilizers containing nitrogen in more than one form. Street
has developed such a method and shown, by analytical data, that it is
applicable in a great number of cases.[174] The process is based on the
substitution of magnesia for soda in the distillation and is carried on
as follows:
Place one gram of the sample in a half liter flat-bottomed flask. Add
about thirty cubic centimeters of water, one gram of reduced iron, and
ten cubic centimeters of sulfuric acid diluted with an equal volume
of water, shake well, and allow to stand for a short time. This will
remove the danger of an explosion caused by the otherwise violent
action which takes place. Close the neck of the flask with a rubber
stopper through which passes a glass dropping-bulb filled with water.
The flask having been stoppered, place it on a slab to which a moderate
heat is applied. Allow the solution to come slowly to a boil and then
boil for five minutes and cool. Add about 100 cubic centimeters of
water, a little paraffin, and about five grams of magnesium oxid. Boil
for forty minutes, after which time all the ammonia will be distilled,
and collect the ammonia in set acid.
The magnesia causes a slight frothing, which can easily be controlled
by adding a little paraffin and by bringing to a boil very gradually.
Fully forty minutes are necessary to distil all the ammonia. Tests were
made after thirty minutes boiling and traces of ammonia were still
found; after forty minutes these traces entirely disappeared.
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