use.]
[Note 2: Soda-lime absorption tubes are to be preferred if a
satisfactory quality of soda lime is available and the number of
determinations to be made successively is small. The potash bulbs will
usually permit of a larger number of successive determinations without
refilling, but they require greater care in handling and in the
analytical procedure.]
[Note 3: Soda lime is a mixture of sodium and calcium hydroxides. Both
combine with carbon dioxide to form carbonates, with the evolution
of water. Considerable heat is generated by the reaction, and the
temperature of the tube during absorption serves as a rough index of
the progress of the reaction through the mass of soda lime.
It is essential that soda lime of good quality for analytical purposes
should be used. The tube should not contain dust, as this is likely to
be swept away.]
[Note 4: The solution of the hydroxide for use in the Geissler bulb
must be highly concentrated to insure complete absorption of the
carbon dioxide and also to reduce the vapor pressure of the solution,
thus lessening the danger of loss of water with the air which passes
through the bulbs. The small quantity of moisture which is then
carried out of the bulbs is held by the calcium chloride in the
prolong tube. The best form of absorption bulb is that to which the
prolong tube is attached by a ground glass joint.
After the potassium hydroxide is approximately half consumed in the
first bulb of the absorption apparatus, potassium bicarbonate is
formed, and as it is much less soluble than the carbonate, it often
precipitates. Its formation is a warning that the absorbing power of
the hydroxide is much diminished.]
!The Analysis!
PROCEDURE.-- Weigh out into the flask (B) about 1 gram of limestone.
Cover it with 15 cc. of water. Weigh the absorption apparatus (F)
or (F') accurately after allowing it to stand for 30 minutes in the
balance case, and wiping it carefully with a lintless cloth, taking
care to handle it as little as possible after wiping (Note 1). Connect
the absorption apparatus with (e) and (f). If a soda-lime tube is
used, be sure that the arm containing the soda lime is next the tube
(E) and that the glass stopcocks are open.
To be sure that the whole apparatus is airtight, disconnect the rubber
tube from the flask (A), making sure that the tubes (a) and (b) do not
contain any hydrochloric acid, close the pinchcocks (a) and (k) and
open (h). No bubbles
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