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
~Determination of Tin in Tin Ore.~--Treat 5 grams of the dried and
finely-powdered ore with 30 c.c. of hydrochloric acid in a four-inch
evaporating dish. After the soluble oxides have been dissolved add 1 or
2 c.c. of nitric acid, boil off nitrous fumes, dilute, and filter. Dry
the filter, transfer the cleaned ore to a piece of combustion tube ten
or twelve inches long and narrowed at one end. Pass a current of
hydrogen through the tube and heat to redness for 30 minutes; cool
whilst the gas is still passing. Dissolve in 20 c.c. of dilute
hydrochloric acid and keep the solution tinted with permanganate of
potassium. When the colour of the permanganate becomes permanent dilute
to a bulk of 50 c.c. with water, filter, and wash. Heat; add a rod of
zinc weighing about 3 grams; allow to stand for a few minutes; decant
through a filter; and wash, removing the remaining zinc and returning
the tin to the beaker. Treat with 5 c.c. of dilute nitric acid, boil for
some time, take up with water, filter, wash, dry, ignite, and weigh as
stannic oxide.
VOLUMETRIC METHOD.
~Titration with Solution of Permanganate of Potassium.~--This titration
may be made either directly on the solution of stannous chloride
(prepared by dissolving the precipitated metal in hydrochloric acid), or
indirectly, on a solution of ferrous chloride (produced by the reducing
action of the precipitated metal on ferric chloride). The standard
solution of permanganate of potassium is made by dissolving 5.356 grams
of the salt in water and diluting to one litre. 100 c.c. are equivalent
to 1.00 gram of tin.
The precipitated tin is transferred to a flask; and dissolved in 10 c.c.
hydrochloric acid, with the aid of heat and in an atmosphere of carbonic
acid. The acid and metal are placed in the flask; which is then filled
with the gas, and stopped with a cork provided with a rubber valve. When
solution is complete the flask is again filled with carbonic acid. Fifty
c.c. of water freed from air and saturated with carbonic acid are then
added. This water is made by adding a gram of bicarbonate of soda and 2
c.c. of hydrochloric acid to 100 c.c. of water: the effervescence sweeps
out the dissolved oxygen. The permanganate of potassium solution is then
run in from a stop-cock burette in the usual way until a faint pink
tinge is obtained.
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