the reasons stated on page 141 care must be taken that the
solution does not become alkaline if the electrolysis is long
continued.]
[Note 5: Urea reacts with nitrous acid, which may be formed in the
solution as a result of the reducing action of the liberated hydrogen.
Its removal promotes the complete precipitation of the copper. The
reaction is
CO(NH_{2})_{2} + 2HNO_{2} --> CO_{2} + 2N_{2} + 3H_{2}O.]
[Note 6: The electrodes must be washed nearly or quite free from
the nitric acid solution before the circuit is broken to prevent
re-solution of the copper.
If several solutions are connected in the same circuit it is obvious
that some device must be used to close the circuit as soon as the
beaker is removed.]
[Note 7: The electrodes upon which the copper has been deposited
may be cleaned by immersion in warm nitric acid. To remove the lead
dioxide, add a few crystals of oxalic acid to the nitric acid.]
DETERMINATION OF IRON
Most brasses contain small percentages of iron (usually not over 0.1
per cent) which, unless removed, is precipitated as phosphate and
weighed with the zinc.
PROCEDURE.--To the solution from the precipitation of copper and
lead by electrolysis, add dilute ammonia (sp. gr. 0.96) until the
precipitate of zinc hydroxide which first forms re-dissolves, leaving
only a slight red precipitate of ferric hydroxide. Filter off the
iron precipitate, using a washed filter, and wash five times with hot
water. Test a portion of the last washing with a dilute solution of
ammonium sulphide to assure complete removal of the zinc.
The precipitate may then be ignited and weighed as ferric oxide, as
described on page 110.
Calculate the percentage of iron (Fe) in the brass.
DETERMINATION OF ZINC
PROCEDURE.--Acidify the filtrate from the iron determination with
dilute nitric acid. Concentrate it to 150 cc. Add to the cold solution
dilute ammonia (sp. gr. 0.96) cautiously until it barely smells of
ammonia; then add !one drop! of a dilute solution of litmus (Note 1),
and drop in, with the aid of a dropper, dilute nitric acid until the
blue of the litmus just changes to red. It is important that this
point should not be overstepped. Heat the solution nearly to boiling
and pour into it slowly a filtered solution of di-ammonium hydrogen
phosphate[1] containing a weight of the phosphate about equal
to twelve times that of the zinc to be precipitated. (For this
calculation the appro
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