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
The tube A has an inside diameter of 18 mm. and is 300 mm. long; the
small tube has an inside diameter of 6 mm. and extends 100 mm. below
the stopcock. At the base of the tube A are placed some pieces of
broken glass or porcelain, covered by a plug of glass wool about 8 mm.
thick, and upon this is placed a thin layer of asbestos, such as is
used for Gooch filters, 1 mm. thick. The tube is then filled with the
amalgamated zinc (Note 1) to within 50 mm. of the top, and on the zinc
is placed a plug of glass wool. If the top of the tube is not already
shaped like the mouth of a thistle-tube (B), a 60 mm. funnel is fitted
into the tube with a rubber stopper and the reductor is connected
with a suction bottle, F. The bottle D is a safety bottle to
prevent contamination of the solution by water from the pump. After
preparation for use, or when left standing, the tube A should be
filled with water, to prevent clogging of the zinc.
[Note 1: The use of fine zinc in the reductor is not necessary and
tends to clog the tube. Particles which will pass a 10-mesh sieve, but
are retained by one of 20 meshes to the inch, are most satisfactory.
The zinc can be amalgamated by stirring or shaking it in a mixture of
25 cc. of normal mercuric chloride solution, 25 cc. of hydrochloric
acid (sp. gr. 1.12) and 250 cc. of water for two minutes. The solution
should then be poured off and the zinc thoroughly washed. It is then
ready for bottling and preservation under water. A small quantity of
glass wool is placed in the neck of the funnel to hold back foreign
material when the reductor is in use.]
STANDARDIZATION
PROCEDURE.--Weigh out into Erlenmeyer flasks two portions of iron wire
of about 0.25 gram each. Dissolve these in hot dilute sulphuric acid
(5 cc. of concentrated acid and 100 cc. of water), using a covered
flask to avoid loss by spattering. Boil the solution for two or
three minutes after the iron has dissolved to remove any volatile
hydrocarbons. Meanwhile prepare the reductor for use as follows:
Connect the vacuum bottle with the suction pump and pour into the
funnel at the top warm, dilute sulphuric acid, prepared by adding 5
cc. of concentrated sulphuric acid to 100 cc. of distilled water. See
that the stopcock (C) is open far enough to allow the acid to run
through slowly. Continue to pour in acid until 200 cc. have passed
through, then close the stopcock !while a small quantity of liquid
is still left in the funnel!. Discard the filtrate, and again
pass through 100 cc. of the warm, dilute acid. Test this with the
permanganate solution. A single drop should color it permanently; if
it does not, repeat the washing, until assured that the zinc is not
contaminated with appreciable quantities of reducing substances. Be
sure that no air enters the reductor (Note 1).
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