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
[Note 6: If the end-point is not permanent, that is, if the blue of
the iodo-starch is discharged after standing a few moments, the cause
may be an insufficient quantity of sodium bicarbonate, leaving the
solution slightly acid, or a very slight precipitation of an antimony
compound which is slowly acted upon by the iodine when the latter is
momentarily present in excess. In either case it is better to discard
the analysis and to repeat the process, using greater care in the
amounts of reagents employed.]
CHLORIMETRY
The processes included under the term !chlorimetry! comprise
those employed to determine chlorine, hypochlorites, bromine, and
hypobromites. The reagent employed is sodium arsenite in the presence
of sodium bicarbonate. The reaction in the case of the hypochlorites
is
NaClO + Na_{3}AsO_{3} --> Na_{3}AsO_{4} + NaCl.
The sodium arsenite may be prepared from pure arsenious oxide,
as described below, and is stable for considerable periods; but
commercial oxide requires resublimation to remove arsenic sulphide,
which may be present in small quantity. To prepare the solution,
dissolve about 5 grams of the powdered oxide, accurately weighed,
in 10 cc. of a concentrated sodium hydroxide solution, dilute the
solution to 300 cc., and make it faintly acid with dilute hydrochloric
acid. Add 30 grams of sodium bicarbonate dissolved in a little water,
and dilute the solution to exactly 1000 cc. in a measuring flask.
Transfer the solution to a dry liter bottle and mix thoroughly.
It is possible to dissolve the arsenious oxide directly in a solution
of sodium bicarbonate, with gentle warming, but solution in sodium
hydroxide takes place much more rapidly, and the excess of the
hydroxide is readily neutralized by hydrochloric acid, with subsequent
addition of the bicarbonate to maintain neutrality during the
titration.
The indicator required for this process is made by dipping strips of
filter paper in a starch solution prepared as described on page 76,
to which 1 gram of potassium iodide has been added. These strips are
allowed to drain and spread upon a watch-glass until dry. When touched
by a drop of the solution the paper turns blue until the hypochlorite
has all been reduced and an excess of the arsenite has been added.
DETERMINATION OF THE AVAILABLE CHLORINE IN BLEACHING POWDER
Bleaching powder consists mainly of a calcium compound which is a
derivative of both hydrochloric and hypochlorous acids. Its formula is
CaClOCl. Its use as a bleaching or disinfecting agent, or as a source
of chlorine, depends upon the amount of hypochlorous acid which it
yields when treated with a stronger acid. It is customary to express
the value of bleaching powder in terms of "available chlorine," by
which is meant the chlorine present as hypochlorite, but not the
chlorine present as chloride.
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