When the decomposition is ended the crucible is strongly heated so as
to hold the platinum sponge, which is produced, together sufficiently
to prevent its being removed in the subsequent washing of the crucible
by decantation. By the ignition at a high temperature necessary to
secure this, the greater part of the calcium chlorid is volatilized.
After cooling, a few drops of concentrated hydrochloric acid are placed
in the crucible and if the slightest yellow color be shown the acid is
evaporated and the ignition repeated, with the addition of a little
oxalic acid. In most cases the slight yellow color produced comes
from a trace of iron and will therefore appear again after the second
ignition. The crucible is subsequently washed by repeated decantations,
finally with boiling water, and after drying is ignited and weighed.
The advantage of this process is that without further trouble the
reduced metal is completely freed of any salts of the alkaline earths,
etc., which have been carried down with it and also from any of the
uncombined sodium chlorid which may not have been washed out by the
alcohol. In fact, the results obtained in this way are nearly always
lower than those obtained through the direct weighing of the double
salt, and the wash water which is first poured off contains, as a rule,
traces of the alkaline earths and almost without exception some sodium
chlorid. Correction for the filter ash is unnecessary because the ash
is completely dissolved by the treatment received. The platinum sponge
which is collected in the crucible in this way is removed in case it
does not adhere to the sides and the crucible is then ready for the
next operation.
=265. Sources of Error in the Platinum Method.=—In the comparative work
done in the determination of potash by the members of the Association
of Official Agricultural Chemists there has been noted, from year to
year, marked differences in the data obtained by different analysts.
Such differences often are due to personal errors, or a failure to
accurately follow the directions for manipulation. Sometimes, however,
they are due to sources of error in the processes employed. In the
platinum method these sources of error have been long known to exist.
Chief among these is the remarkable facility with which potash becomes
incorporated with the precipitates of other bodies. The character
and magnitude of some of these errors have lately been studied by
Robinson.[214]
Public-domain text, read in full here on John Shaqi.
Reviews
Reviews
No reviews yet
Be the first to share your thoughts on this work.
Elsewhere in the archive
Join the Discussion
Join the discussion
Sign in to leave a comment or review.
Sign InorCreate an account