An Introductory Course of Quantitative Chemical Analysis: With Explanatory NotesTalbot, Henry Paul
Science
An Introductory Course of Quantitative Chemical Analysis: With Explanatory Notes
Talbot, Henry Paul
Chemistry, Analytic -- Quantitative
PROCEDURE.--Place in a porcelain crucible about 6 grams (roughly
weighed) of the purest sodium bicarbonate obtainable. Rest the
crucible upon a triangle of iron or copper wire so placed within a
large crucible that there is an open air space of about three eighths
of an inch between them. The larger crucible may be of iron, nickel or
porcelain, as may be most convenient. Insert the bulb of a thermometer
reading to 350°C. in the bicarbonate, supporting it with a clamp so
that the bulb does not rest on the bottom of the crucible. Heat
the outside crucible, using a rather small flame, and raise the
temperature of the bicarbonate fairly rapidly to 270°C. Then regulate
the heat in such a way that the temperature rises !slowly! to 300°C.
in the course of a half-hour. The bicarbonate should be frequently
stirred with a clean, dry, glass rod, and after stirring, should be
heaped up around the bulb of the thermometer in such a way as to cover
it. This will require attention during most of the heating, as the
temperature should not be permitted to rise above 310°C. for any
length of time. At the end of the half-hour remove the thermometer and
transfer the porcelain crucible, which now contains sodium carbonate,
to a desiccator. When it is cold, transfer the carbonate to a
stoppered weighing tube or weighing-bottle.
STANDARDIZATION
PROCEDURE.--Clean carefully the outside of a weighing-tube, or
weighing-bottle, containing the pure sodium carbonate, taking care
to handle it as little as possible after wiping. Weigh the tube
accurately to 0.0001 gram, and record the weight in the notebook. Hold
the tube over the top of a beaker (200-300 cc.) and cautiously remove
the stopper, making sure that no particles fall from it or from the
tube elsewhere than in the beaker. Pour out from the tube a portion
of the carbonate, replace the stopper and determine approximately how
much has been removed. Continue this procedure until 1.00 to 1.10
grams has been taken from the tube. Then weigh the tube accurately
and record the weight under the first weight in the notebook.
The difference in the two weights is the weight of the carbonate
transferred to the beaker. Proceed in the same way to transfer a
second portion of the carbonate from the tube to another beaker of
about the same size as the first. The beakers should be labeled and
plainly marked to correspond with the entries in the notebook.
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