The theory of the process rests on the fact that by a careful
admixture of a nitrogenous substance diluted with land plaster, with
phenolsulfuric acid, it is possible to change the nitric acid into
nitro-phenol, and by the reducing action of zinc dust to change the
nitro-product formed into amido-phenol. This afterwards is transformed
into ammonium sulfate by heating with sulfuric acid, by which process,
at the same time, all other nitrogenous compounds present in the
substance, as with Kjeldahl’s method, likewise form ammonium sulfate,
only with the difference that addition of mercury is here absolutely
necessary for the complete transformation of the slowly decomposed
amido-phenol which again brings about the necessity of decomposing
the nitrogenous mercury compounds formed in the solution by potassium
sulfid, which is added after or with the soda-lye.
=191. The Dutch Jodlbaur Method.=—The Royal Experiment Station of
Holland directs that the jodlbaur process be carried out as indicated
below.[162]
The reagents necessary are:
1. _Phenolsulfuric acid_, prepared by dissolving 100 grams of pure
crystallized phenol in pure sulfuric acid (1.84) and making up the
solution to a liter with the same sulfuric acid:
2. _Zinc_, carefully washed and thoroughly dried:
3. _Sodium hydroxid solution_, the same as is used in the kjeldahl
method:
4. _Potassium sulfid solution_, made by dissolving 355 grams of
potassium sulfid (K₂S), or sodium sulfid solution, made by dissolving
250 grams of sodium sulfid (Na₂S) in a liter of water.
As apparatus, are necessary oxidation flasks holding about 200
cubic centimeters, and distillation flasks holding about 750 cubic
centimeters, both of bohemian glass.
_Manipulation._—Weigh one gram of substance, moisten it with water,
dry, and introduce into an oxidation flask. Cover with fifteen cubic
centimeters of phenolsulfuric acid and, after cooling, thoroughly mix
by gently shaking. After five minutes add from two to three grams of
zinc in small proportions, keeping the flask cool, then twenty cubic
centimeters of sulfuric acid, and finally two drops of mercury. Boil
the mixture till the fluid is colorless. Cool and dilute. Wash into
a distillation flask and add an excess of sodium hydroxid solution
and twenty-five cubic centimeters of the sodium (or potassium) sulfid
solution. Distil and titrate as in the kjeldahl method.
=192. The Halle-Jodlbaur Method.=—At the Halle station it is
the uniform practice to mix the nitrate with gypsum before the
combustion.[163] In the case of Chile phosphates ten grams are rubbed
with an equal amount of gypsum, and two grams of the mixture, equal
to one gram of the nitrate, taken for the determination. In the case
of saltpeter mixtures which contain over eight per cent of nitrogen,
one gram of the mixture with gypsum is taken, of guanos one and a half
grams, and of lower forms of nitrates or mixtures thereof, from three
to five grams.
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