ximate percentage of zinc is that found by
subtracting the sum of the percentages of the copper, lead and iron
from 100 per cent.) Keep the solution just below boiling for fifteen
minutes, stirring frequently (Note 2). If at the end of this time the
amorphous precipitate has become crystalline, allow the solution to
cool for about four hours, although a longer time does no harm (Note
3), and filter upon an asbestos filter in a porcelain Gooch crucible.
The filter is prepared as described on page 103, and should be dried
to constant weight at 105 deg.C.
[Footnote 1: The ammonium phosphate which is commonly obtainable
contains some mono-ammonium salt, and this is not satisfactory as a
precipitant. It is advisable, therefore, to weigh out the amount of
the salt required, dissolve it in a small volume of water, add a drop
of phenolphthalein solution, and finally add dilute ammonium hydroxide
solution cautiously until the solution just becomes pink, but do not
add an excess.]
Wash the precipitate until free from sulphates with a warm 1 per cent
solution of the di-ammonium phosphate, and then five times with 50 per
cent alcohol (Note 4). Dry the crucible and precipitate for an hour at
105 deg.C., and finally to constant weight (Note 5). The filtrate should
be made alkaline with ammonia and tested for zinc with a few drops of
ammonium sulphide, allowing it to stand (Notes 6, 7 and 8).
From the weight of the zinc ammonium phosphate (ZnNH_{4}PO_{4})
calculate the percentage of the zinc (Zn) in the brass.
[Note 1: The zinc ammonium phosphate is soluble both in acids and in
ammonia. It is, therefore, necessary to precipitate the zinc in a
nearly neutral solution, which is more accurately obtained by adding
a drop of a litmus solution to the liquid than by the use of litmus
paper.]
[Note 2: The precipitate which first forms is amorphous, and may have
a variable composition. On standing it becomes crystalline and then
has the composition ZnNH_{4}PO_{4}. The precipitate then settles
rapidly and is apt to occasion "bumping" if the solution is heated to
boiling. Stirring promotes the crystallization.]
[Note 3: In a carefully neutralized solution containing a considerable
excess of the precipitant, and also ammonium salts, the separation
of the zinc is complete after standing four hours. The ionic changes
connected with the precipitation of the zinc as zinc ammonium
phosphate are similar to those described for magnesium amm
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