=208. Schmitt’s Modified Method.=—The method is a modification of that
already described by the author in which a mixture of powdered zinc
and iron is used as a reducing agent.[176] The process is carried out
as follows: Ten grams of the nitrate are dissolved and the volume made
up to half a liter. Ten cubic centimeters of glacial acetic acid and
ten grams of the fine metallic powder, iron and zinc, are placed in a
flask of a capacity of about three-quarters of a liter and twenty-five
cubic centimeters of the solution of the nitrate added. The flask is
covered during the reduction to prevent loss by spraying, and after
the solution is complete, which is the case in about ten minutes,
the contents of the flask are diluted with from 200 to 300 cubic
centimeters of water, thirty cubic centimeters of caustic soda of 1.25
specific gravity added, and the whole distilled as in the kjeldahl
process. It must be noted that it is essential that the iron be finely
divided; it is mixed with the powdered zinc in equal parts. The total
nitrogen can be determined in guanos and nitrate mixtures by the
following simple alteration in procedure: One gram of the substance is
dissolved in water, five cubic centimeters of glacial acetic acid, and
from two to three grams of the mixed metallic powder added, and the
whole gently heated for ten or fifteen minutes. After the contents of
the flask have cooled, twenty-five cubic centimeters of sulfuric acid
are cautiously added in small portions, undue frothing being restrained
by the addition of a fragment of paraffin wax. The acetic acid is then
driven off by heating, and the remaining contents of the flask boiled
until the organic matter is completely decomposed, as in the kjeldahl
process. About two hours boiling is required. Neutralization and
distillation are then practiced as in the ordinary manner. The method
is also applicable to the determination of nitrates in drinking water,
provided nitrites and ammonia be absent.
=209. Krüger’s Method for Nitric Acid.=—About three-tenths gram of the
substance dissolved in water is mixed with twenty cubic centimeters of
a hydrochloric acid solution of stannous chlorid holding 150 grams of
tin per liter.[177] One and a half grams of spongy tin prepared by the
action of zinc on stannous chlorid are added. The flask containing the
mixture is heated until the tin is dissolved, by which time the nitric
acid is completely reduced. The subsequent distillation and titration
are accomplished as usual. In the case of nitro and nitroso compounds,
after the solution of the tin, twenty cubic centimeters of sulfuric
acid are added and heated until sulfuric vapors escape. After cooling,
the amido substances formed are oxidized by potassium bichromate before
the distillation takes place.
Public-domain text, read in full here on John Shaqi.
Reviews
Reviews
No reviews yet
Be the first to share your thoughts on this work.
Elsewhere in the archive
Join the Discussion
Join the discussion
Sign in to leave a comment or review.
Sign InorCreate an account