It is easy to see that in the Pavy process the quantity of ammonia in
the solution is rapidly diminished during the boiling and this has led
to the suggestion of other methods to exclude the air. Among these
have been recommended the introduction of a current of hydrogen or
carbon dioxid. One of the best methods of procedure is that proposed
by Allen, who recommends covering the copper solution by a layer of
paraffin oil (kerosene).[96]
=130. Process Of Peska.=—Peska has also independently made use of
Allen’s method of covering the solutions with a layer of paraffin oil
and finds it reliable.[97] The copper reagent employed by him has the
following composition:
Crystallized copper sulfate 6.927 grams
Ammonia, twenty-five per cent strength 160.00 cc.
The copper sulfate is dissolved in water, the ammonia added, and
the volume completed to half a liter with distilled water. A second
solution containing half a liter is made by dissolving 34.5 grams
of potassium-sodium tartrate and ten grams of sodium hydroxid and
completing the cool solution to half a liter with distilled water.
In all cases the water used in making up the above solutions must be
freshly boiled to exclude the air.
For the titration, fifty cubic centimeters of each of the above
solutions are taken, mixed and covered with a layer of paraffin oil
half a centimeter in depth. The reduction is not accomplished at a
boiling temperature, but at from 80° to 85°. The manipulation is
conducted as follows:
The mixed solutions are placed in a beaker, covered with oil, and
heated to 80°. The temperature is measured by a thermometer which also
serves as a stirring rod. The sugar solution is run down the sides
of the beaker from a burette of such a shape as to be protected from
the heat. After each addition of the sugar solution the mixture is
carefully stirred, keeping the temperature at from 80° to 85°. The
first titration is made to determine approximately the quantity of
sugar solution necessary to decolorize the copper. This done, the
actual titration is accomplished by adding at once the total amount
of sugar solution necessary to decolorize, less about one cubic
centimeter. Any sugar solution adhering to the side of the beaker
is washed down by distilled water, the contents of the beaker well
stirred, and the temperature kept at 85° for two minutes. The rest of
the sugar solution is then added in quantities of one-tenth of a cubic
centimeter until the decoloration is completed. The total time of the
final titration should not exceed five minutes. The sugar solution
should be as nearly as possible of one per cent strength. If a lower
degree of strength be employed a larger quantity of the sugar is
necessary to reduce a given quantity of copper.
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