actory, since it is impossible to
carry shades of color in the memory and to duplicate them from day to
day.]
[Note 2: While variation of two parts in one thousand in the values
obtained by an inexperienced analyst is not excessive, the idea must
be carefully avoided that this is a standard for accurate work to be
!generally applied!. In many cases, after experience is gained, the
allowable error is less than this proportion. In a few cases a
larger variation is permissible, but these are rare and can only
be recognized by an experienced analyst. It is essential that the
beginner should acquire at least the degree of accuracy indicated if
he is to become a successful analyst.]
STANDARDIZATION OF HYDROCHLORIC ACID
SELECTION AND PREPARATION OF STANDARD
The selection of the best substance to be used as a standard for acid
solutions has been the subject of much controversy. The work of Lunge
(!Ztschr. angew. Chem.! (1904), 8, 231), Ferguson (!J. Soc. Chem.
Ind.! (1905), 24, 784), and others, seems to indicate that the best
standard is sodium carbonate prepared from sodium bicarbonate by
heating the latter at temperature between 270 deg. and 300 deg.C. The
bicarbonate is easily prepared in a pure state, and at the
temperatures named the decomposition takes place according to the
equation
2HNaCO_{3} --> Na_{2}CO_{3} + H_{2}O + CO_{2}
and without loss of any carbon dioxide from the sodium carbonate, such
as may occur at higher temperatures. The process is carried out as
described below.
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 deg.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 deg.C. Then regulate
the heat in such a way that the temperature rises !slowly! to 300 deg.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
|