Laboratory Methods of Inorganic Chemistry, 2nd English Ed. 1928

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160 SUBSTITUTED AMMONIUM COMPOUNDS.

about 40% of the weight of the potassium diazomethanedisul-
phonate. Dependent preparation: Sodium Hydrazoate, No. 72.

Monochloramine, NH 2 Cl; Hydrazine Sulphate according to
Raschig.^1
Ammonia is chlorinated by the action of sodium hypochlorite in dilute
aqueous solution:
NH 3 + NaOCl = NH 2 C1 + NaOH.
The monochloramine thus formed reacts with more ammonia to form hydra-
zine chloride:
NH 2 C1 + NH 3 = H 2 N .NH 2. HC1.
Place 600 g. of ice and a cold solution of 85 g. of sodium hy-
droxide in 160 c.c. of water in a one-liter flask, weigh the flask and
contents, wrap the flask in a towel, and pass in a rapid current of
chlorine until the gain in weight is exactly 71 grams; avoid an
excess of chlorine. Then on diluting to one liter, an approximately
molal solution of sodium hypochlorite is obtained.
Monochloramine. Add 50 c.c. of this sodium hypochlorite
solution to a mixture of 25 c.c. 2-normal ammonia and 75 c.c. of
water. The liquid ceases to smell of ammonia, and in its place a
peculiar, penetrating odor of monochloramine is noticeable which
is similar to that of nitrogen chloride. Nitrogen is evolved from
the solution at the same time, owing to the fact that monochlora-
mine decomposes slowly in an aqueous solution according to the
following equation:
3 NH 2 C1 = N 2 + NH.C1 + 2 HC1.


Hydrazine Sulphate. Mix 200 c.c. of 20% ammonia, 5 c.c. of
a 1% gelatin solution, and 100 c.c. of the above prepared molal
sodium hypochlorite in a one-liter Erlenmeyer flask, heat the
mixture immediately to boiling, and boil it for half an hour. The
solution is thereby concentrated to about one-fourth its original
volume. Cool it, then add 25 c.c. of 2-normal sulphuric acid, and
surround the flask with ice. Hydrazine sulphate crystallizes out
in the form of glistening, transparent crystals which are obtained
pure by recrystallizing from water. Yield, 5 to 6 grams.

This process, which is very interesting from a theoretical standpoint, is
now used technically for the production of hydrazine sulphate, whereby the
cost of the latter has been considerably reduced.
1
Raschig, Ber. 40, 4586 (1907).
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