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
Unfortunately the difference in the two titrations does not depend
merely on the quantity of zinc present; as it is also influenced by the
extent of dilution, the degree of alkalinity of the solution, and the
quantity of cyanide present. In an experiment with .055 gram of zinc
sulphate and .1 gram of potassium cyanide the difference in the two
finishing points was only .1 c.c.; whereas with .4 gram of potassium
cyanide, the other conditions being the same, the difference was 1.5
c.c. of standard silver nitrate. On the assumption that all the zinc was
present as potassium zinc cyanide (K_{2}ZnCy_{4}) the difference should
have been 5 c.c. in each case. Again, repeating the experiment with .4
gram of potassium cyanide, but with .11 gram of crystallised zinc
sulphate, the difference was 6.5 c.c.: that is, merely doubling the
quantity of zinc increased the difference by more than four times. Hence
it would appear better to use the method with the iodide and make a
separate assay for the zinc. But since the student may be called on to
use the other method, he is advised to practice it also.
~The assay without iodide.~--The standard solution of silver nitrate is
placed in a small burette divided into tenths of a c.c. Ten c.c. of the
cyanide solution to be assayed is transferred to a small flask and
diluted with water to about 70 c.c. The silver solution is then run in
from the burette (with constant shaking of the flask), a little at a
time but somewhat rapidly, until a permanent turbidity appears. Since 1
c.c. of the silver nitrate solution corresponds to .01 gram of potassium
cyanide, it also corresponds to .1 per cent. of this salt counted on the
10 c.c. of cyanide solution taken. The titration should be performed in
a fairly good uniform light. The learner should practice on a fairly
pure solution of potassium cyanide at first, and this may conveniently
have a strength of about 1 per cent. For practice with solutions
containing zinc make a solution containing 1.1 gram of crystallised zinc
sulphate in 100 c.c. and slowly add measured quantities of from 1 to 5
c.c. of this to the 10 c.c. of cyanide liquor before diluting for the
titration.
If a cyanide solution blackens on the addition of the silver nitrate it
contains sulphide. In this case, shake up a considerable bulk of the
liquor with a few grams of lead carbonate, allow to settle and make the
assay on 10 c.c. of the clear liquor.
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