A text-book of assaying : $b for the use of those connected with mines.Beringer, C. (Cornelius)
Science
A text-book of assaying : $b for the use of those connected with mines.
Beringer, C. (Cornelius)
Assaying
The filtrate containing the tin is rendered acid with hydrochloric acid,
and filtered. The precipitate is rinsed into a half-pint beaker, covered
with 20 c.c. of hydrochloric acid, and boiled down to about 20 c.c. The
solution is filtered off from the sulphur and sulphide of arsenic,
which, after washing with hot water, is transferred to a flask labelled
"arsenic." A strip of sheet zinc (2 in. by 1 in.) is placed in the
solution. The evolution of hydrogen should be brisk. In five or ten
minutes decant off a few c.c. of the liquid, and test with sulphuretted
hydrogen for tin. If no yellowish precipitate is formed, decant off the
rest of the liquid, and wash the precipitated metal with hot water two
or three times by decantation. The metal should be in a lump; if there
are any floating particles they must be made to sink by compression with
a glass rod. Transfer the washed metal to an evaporating dish 3 or 4 in.
across, and cover with a few c.c. of hot water. Add nitric acid drop by
drop till the tin is completely attacked. Evaporate nearly to dryness,
and add a drop or two more of nitric acid and 20 c.c. of water. Boil and
filter. Wash with hot water, dry, ignite, and weigh as stannic oxide,
SnO_{2}. Calculate to metallic tin by multiplying by 0.7867.[76]
The filtrate from the first treatment with sulphuretted hydrogen will
probably no longer smell of the gas. Warm and pass the gas for a few
minutes longer. Filter off any precipitate of sulphide of arsenic, and
transfer it to the flask for "arsenic." Boil the filtrate (ignoring any
signs of a further precipitation of arsenic) with a few c.c. of nitric
acid, and separate the iron as basic acetate. Wash; reserve the filtrate
for cobalt.
~Iron.~--Rinse back the "basic acetate," precipitate into the flask, add
ammonia, dilute with water to about 100 c.c., and pass sulphuretted
hydrogen for a few minutes. Filter, and wash with hot water. Collect the
filtrate in the flask labelled "arsenic." Boil the precipitate with
dilute sulphuric acid, filter, and titrate the filtrate with the
permanganate of potassium solution after boiling off the sulphuretted
hydrogen. Report the result as iron. The sulphuric acid will not effect
complete solution, a light black residue will remain, chiefly sulphur;
this must be rinsed into the filtrate from the acetate separation. It
contains cobalt.
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