The distillation flask is closed with a rubber stopper carrying a
bulb-tube which ends above in a glass tube about three-quarters of a
meter long, bent at an acute angle, and passing obliquely downward on
a convenient support. This tube is connected by a rubber, with the end
tube bent nearly at a right angle and dipping into the standardized
acid in the erlenmeyer receiver. The general arrangement of the
distilling apparatus is shown in figure 12. Since the contents of
the vessel are warmed by mixing with the soda-lye, the flame can be
turned on at full head at once at the commencement of the operation.
In about a quarter of an hour the liquid in the receiver will be
at the boiling-point, and the boiling should be continued for five
minutes more, making twenty minutes in all for the completion of the
distillation. By this boiling the contents of the receiver are not
charged with carbon dioxid, as might happen if a condenser were used.
The receiver contains twenty cubic centimeters of a standardized
sulfuric acid solution and about fifty cubic centimeters of water.
[Illustration: FIGURE 12. DISTILLATION APPARATUS OF HALLE
AGRICULTURAL LABORATORY.]
The acid used should contain 38.1 grams of sulfuric acid of 1.845
specific gravity in a liter; and it should be set by titration with
chemically pure sodium carbonate. For this purpose seven-tenths gram of
sodium carbonate is heated in a platinum crucible for two hours over a
small flame, weighed, and placed in an erlenmeyer together with twenty
cubic centimeters of the sulfuric acid, care being taken to avoid loss
from the vigorous evolution of carbon dioxid. After boiling for ten
minutes all the carbon dioxid is removed from solution. After cooling,
the excess of acid is determined by titration with a standardized
barium hydroxid solution, using rosolic acid as indicator.
The solution of barium hydroxid is made as follows: Digest, with warm
water, 260 grams of caustic baryta, Ba(OH)₂, until it is nearly all
dissolved, filter, and make up to a volume of ten liters and keep in
a flask free of carbon dioxid. A solution of barium hydroxid is to be
preferred to the corresponding sodium compound for titration. If traces
of carbonate be formed in the two liquids, the sodium salt will remain
in solution while the barium compound will settle at the bottom of the
flask.
_The Indicator._—The indicator used to determine the end of the
reaction is made by dissolving one gram of rosolic acid in fifty cubic
centimeters of alcohol. From one to two drops are enough for each
titration. The color reaction is less definite as the quantity of
ammonia in the liquid increases. When the titration solutions have been
prepared as above described it is found to require about ninety of the
barium hydroxid to neutralize twenty cubic centimeters of the sulfuric
acid.
By direct titration with sodium carbonate it is ascertained how many
grams of nitrogen the twenty cubic centimeters of sulfuric acid
represent.
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