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
If the cyanide liquor be suspected to contain free prussic acid, take 10
c.c. for the assay as usual; but, before titrating, add .1 or .2 gram of
sodium carbonate. On no condition must caustic soda or ammonia be added.
The difference between the results, with and without the addition of
carbonate of soda, is supposed to measure the quantity of free prussic
acid. If this has to be reported it is best done as "prussic acid
equivalent to ... per cent. of potassium cyanide." Suppose, for example,
the difference in the two titrations equals 1 c.c. of standard silver
nitrate; the prussic acid found would be equivalent to .1 per cent. of
potassium cyanide.
~The assay with iodide.~--The standard solution of silver nitrate is
placed in a burette divided into tenths of a c.c. Take 10 c.c. of the
cyanide liquor, which should previously have been treated with white
lead for the removal of sulphides if these happened to be present.
Transfer to a small flask, add 3 or 4 drops of a solution of potassium
iodide and 2 or 3 c.c. of a solution of sodium hydrate; dilute to 60 or
70 c.c. with water. If much zinc is present the soda may be increased to
20 or 30 c.c. with advantage. The standard solution should be run in
somewhat rapidly, but a little at a time, so that the precipitate at
first formed shall be small and have only a momentary existence. The
titration is continued until there is a permanent yellowish turbidity.
The most satisfactory and exact finish is got by ignoring any faint
suspicion of a turbidity and accepting the unmistakable turbidity which
the next drop of silver nitrate is sure to produce. This finishing point
gives results which are exactly proportional to the quantity of cyanide
present; and it can be recognised with more than ordinary precision even
in solutions which are not otherwise perfectly clear.
Each c.c. of the standard silver nitrate solution corresponds to .01
gram of potassium cyanide; and if 10 c.c. of the liquor are taken for
assay this corresponds to .1 per cent. or 2 lbs. to the short ton or
2.24 lbs. to the long ton. As already explained the result should be
reported as "cyanide equivalent to so much per cent. of potassium
cyanide."
The following experimental results were obtained with a solution of
potassium cyanide made up to contain about 1.2 per cent. of the salt.
~Effect of varying cyanide.~--The bulk before titration was in each case
60 c.c.; 2 c.c. of soda and 3 drops of potassium iodide were used in
each case.
Cyanide added 40 c.c. 30 c.c. 20 c.c. 10 c.c. 5 c.c. 1 c.c.
Silver required 47.0 c.c. 35.25 c.c. 23.5 c.c. 11.7 c.c. 5.8 c.c. 1.15 c.c.
Accepting the result for 40 c.c. as correct, the others are in very
satisfactory agreement.
~Effect of varying dilution.~--The conditions were those of the 40 c.c.
experiment in the last series; but varying amounts of water were used in
diluting.
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