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
1. _With Stannous Chloride._--Fill a burette with a solution of stannous
chloride,[67] and cautiously run the liquid into the hot assay solution
(in which the iron is present as _chloride_) until the colour is
discharged. A large excess of the stannous chloride must be avoided.
Then add 5 c.c. of a 2-1/2 per cent. solution of mercuric chloride, this
will cause a white precipitate (or a grey one if too large an excess of
the stannous chloride has been added). Boil till the solution clears,
cool, dilute, and titrate.
2. _With Sulphuretted Hydrogen._--Cool the solution and pass through it
a current of washed sulphuretted hydrogen till the liquid smells
strongly of the gas after withdrawal and shaking. A white precipitate of
sulphur will be formed, this will not interfere with the subsequent
titration provided it is precipitated in the cold. If, however, the
precipitate is coloured (showing the presence of the second group
metals), or if the precipitation has been carried out in a hot solution,
it should be filtered off. Boil the solution until the sulphuretted
hydrogen is driven off; this may be tested by holding a strip of filter
paper dipped in lead acetate solution in the steam issuing from the
flask. The presence of sulphuretted hydrogen should be looked for rather
than its absence. It is well to continue the boiling for a few minutes
after the gas has been driven off. Cool and titrate.
3. _With Sodium Sulphite._--Add ammonia (a few drops at a time) until
the precipitate first formed redissolves with difficulty. If a permanent
precipitate is formed, redissolve with a few drops of acid. To the warm
solution add from 2 to 3 grams of sodium sulphite crystals. The solution
will become strongly coloured, but the colour will fade away on standing
for a few minutes in a warm place. When the colour is quite removed, add
20 c.c. of dilute sulphuric acid, and boil until the steam is quite free
from the odour of sulphurous acid. Cool and titrate.
4. _With Zinc._--Add about 10 grams of granulated zinc; if the hydrogen
comes off violently add water; if, on the other hand, the action is very
slow, add sufficient dilute sulphuric acid to keep up a brisk
effervescence. The reduction is hastened by warming, and is complete
when the solution is quite colourless and a drop of the liquid tested
with sulphocyanate of potassium gives no reaction for ferric iron.
Filter through "glass wool" or quick filtering paper. The zinc should be
still giving off gas rapidly, indicating a freely acid solution; if not,
acid must be added. Wash with water rendered acid. Cool and titrate.
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