Scientific American Supplement, No. 324, March 18, 1882Various
Science
Scientific American Supplement, No. 324, March 18, 1882
Various
Science -- Periodicals
When no more carbonic acid is evolved, another tube from this last flask
is connected with the aspirator, the pinch-cock of the pipette open, and
air drawn through the apparatus for about half a minute, and thus all
the carbonic acid evolved absorbed, or the flasks may be slightly
heated. If danger of more carbonic acid being absorbed from the air is
feared, and always in very accurate analysis, a potassa tube may be
connected to the pipette before drawing the air through. The precipitate
formed is allowed to settle, 50 c.c. of the supernatant solution
is removed with a pipette and transferred to a beaker; 50 c.c. of
decinormal nitric acid and some water is added with sufficient cochineal
tincture. It is then titrated back with decinormal soda; from this is
now readily deducted the amount of carbonic acid, and from that the
MnO_{2}, holding in view that 44 parts of carbonic acid is equivalent to
43.5 of MnO_{2} or 98.87 per cent, and that 1 c.c. of the N/10 baryta
solution is equivalent to 0.0022 grm. of CO_{2}.
If a carbonate, chloride, or nitrate, be present in the native binoxide,
it must be removed with some sulphuric acid. This is afterward
neutralized with a little caustic soda. This method yields the
following results for its value in amount of manganese to 100:
99.91-99.902-99.895, and can be executed in about twenty minutes.
Fifteen determinations can be carried on at once without loss of time,
this, however, depending on the operator's skill. I have made many
assays, and assays by this method with similarly excellent results.
Of the other methods, Bunsen's is acknowledged to be the most accurate,
but is, of course, too troublesome to be used in technical work,
although it is used in scientific analysis. Ordinary samples are not
sufficiently accurate to allow the use of this method.
The methods of reducing with iron and titrating this with chromate of
potassa, etc., have given a constant average of from 98.60-99.01. These
results are fair, but hard to obtain expeditiously.
Of the methods of precipitating the compounds of the protoxide and
estimating the acid, that of the phosphate is by far the most accurate,
titrating with uranium solution; 99.82 is a nearly constant average
with me, much depending on the operator's familiarity with the uranium
process.
The methods of Lenssen, or ferricyanide of potassium method, yields very
widely differing results. I have found the figures of Fresenius about
the same as my own in this case; that is from 98.00-100.10.
Public-domain text, read in full here on John Shaqi.
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