The distilling apparatus of Aubin is preferred by the French chemists,
an apparatus so arranged with a reflux partial condenser, that nearly
all the aqueous vapor is returned in a condensed state to the flask
while the ammonia, on account of its great volatility, is carried
over into the receiver. To avoid the regurgitation which might be
caused by the concentrated ammonia gas coming in contact with the acid
the separable part of the condensing tube is expanded into a bulb
large enough to hold all the acid which lies above its mouth. By the
means of this apparatus the ammonia is all collected in the standard
acid without greatly increasing its volume and the titration is thus
rendered sharper. The employment of caustic magnesia has the advantage
of not decomposing any organic matters or cyanids that may be present.
If the sample under examination hold part of its ammonia as ammonium
magnesium phosphate it will be necessary first to treat it with
sulfuric acid in order to set the ammonia free and then to use enough
of the magnesium oxid to neutralize the excess of the sulfuric acid and
still supply the two grams necessary for the distillation. When the
sample contains a considerable quantity of organic matter it sometimes
tends to become frothy towards the end of the distillation. This
trouble can be avoided by introducing into the flask one or two grams
of paraffin.
Where carbon dioxid is given off during the distillation the contents
of the receiver must be boiled before titration, or else lacmoid must
be used as an indicator instead of litmus.
=202. Determination of Thiocyanates in Ammoniacal Fertilizers.=—The
extended use of ammonium sulfate as a fertilizer renders it important
to determine the actual constituents which may be present in samples
of this material. The following bodies have been found in commercial
ammonium sulfates: Sulfuric acid, chlorin, ammonia, thiocyanic acid,
potash, soda, lime and iron oxid. These are found in the soluble
portions. In the insoluble portions have been found silica, sulfuric
acid, lime, magnesia and iron oxid. A sample of commercial ammonium
sulfate analyzed by Jumeau contained the following substances:[170]
Per cent.
Moisture 10.5109
Ammonium sulfate 67.8453
Ammonium thiocyanate 9.3935
Sodium sulfate 9.2429
Potassium sulfate 0.9774
Calcium sulfate 0.6800
Iron thiocyanate 0.5000
Magnesium chlorid traces
Silica 0.0830
Undetermined 0.7670
The determination of the thiocyanic acid in the thiocyanate is
generally made by the oxidation of the sulfur to sulfuric acid and its
subsequent weighing in the form of barium sulfate. Jumeau has modified
the method by determining the amount of the thiocyanate by means of a
titrated liquid. The method is practiced as follows:
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