Scientific American Supplement, No. 324, March 18, 1882Various
Science
Scientific American Supplement, No. 324, March 18, 1882
Various
Science -- Periodicals
The element manganese having many peculiarities in its reactions
with the other elements, is now extensively used in the arts, its
combinations entering into and are used in many of the important
processes; it is consequently often brought before the chemist in his
analysis, and has to be determined in most cases with considerable
accuracy. Many methods have been proposed for this, all of them of more
or less value; those yielding the best results, however, requiring a
considerable length of time for their execution, and involving so large
an amount of manipulatory skill as to render them fairly impracticable
to a chemist at all pressed for time, and receiving but a mere trifle
for the results.
As I have had to make numerous estimations of manganese in various
compounds, as a public analyst, I have been induced to investigate the
volumetric methods at present in use to find their comparative values,
and if possible to work out a new one, setting aside one or more of the
difficulties met with in the use of the older ones. This paper is a part
summary of the results. First, I will detail my process of estimation,
then on the separation.
From all compounds of manganese, excepting those containing cobalt and
nickel, the manganese is precipitated as binoxide; those containing
these two elements are treated with phosphoric acid, or as noted under
Separation.
A.--The Estimation. The binoxide of commerce, as taken from the mine, is
well sampled, powdered, and dried at 100°C. 0.5 gramme of this is taken
and placed in a 250 c.c. flask; in analysis the binoxide on the filter,
from the treatments noted under separation is thoroughly washed with
warm water; it is then washed down in a flask, as above, after breaking
the filter paper; sufficient water is added to one-third fill the flask,
and about twice the approximate weight of the binoxide in the flask of
oxalate of potassa; these are agitated together. A twice perforated
stopper is fitted to this flask, carrying through one opening a 25 c c.
pipette nearly filled with sulphuric acid, sp. gr. 1.4, the lower point
of which just dips below the mixture in the flask, and the upper end,
carrying a rubber tube and pinch cock to control the flow of acid.
Through the other opening passes a glass tube bent at an acute angle
and connected by a short rubber tube to an adjoining flask, two-thirds
filled with decinormal baryta solutions. These connections are all made
air tight. Sulphuric acid is allowed in small portions at a time to
flow into the mixture. Carbonic acid is evolved, and, passing into
the adjoining flask, is absorbed by the baryta, precipitating it as
carbonate. To prevent the precipitate forming around or choking up the
entrance tube, the flask must be agitated at short intervals to break it
off. The reaction so familiar to us in other determinations is expressed
thus:
MnO_{2}+KO,C_{2}O_{3}+2SO_{3} = MnO,SO_{3}+KO.SO_{3}+2CO_{2},
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