Procedure.—Weigh out two portions of about 0.5 gram each (Note 1) into tall, slender lipless beakers of about 100 cc. capacity. Dissolve the metal in a solution of 5 cc. of dilute nitric acid (sp. gr. 1.20) and 5 cc. of water, heating gently, and keeping the beaker covered. When the sample has all dissolved (Note 2), wash down the sides of the beaker and the bottom of the watch-glass with water and dilute the solution to about 50 cc. Carefully heat to boiling and boil for a minute or two to expel nitrous fumes.
Meanwhile, four platinum electrodes, two anodes and two cathodes, should be cleaned by dipping in dilute nitric acid, washing with water and finally with 95 per cent alcohol (Note 3). The alcohol may be ignited and burned off. The electrodes are then cooled in a desiccator and weighed. Connect the electrodes with the binding posts (or other device for connection with the electric circuit) in such a way that the copper will be deposited upon the electrode with the larger surface, which is made the cathode. The beaker containing the solution should then be raised into place from below the electrodes until the latter reach nearly to the bottom of the beaker. The support for the beaker must be so arranged that it can be easily raised or lowered.
If the electrolytic apparatus is provided with a mechanism for the rotation of the electrode or stirring of the electrolyte, proceed as follows: Arrange the resistance in the circuit to provide a direct current of about one ampere. Pass this current through the solution to be electrolyzed, and start the rotating mechanism. Keep the beaker covered as completely as possible, using a split watch-glass (or other device) to avoid loss by spattering. When the solution is colorless, which is usually the case after about 35 minutes, rinse off the cover glass, wash down the sides of the beaker, add about 0.30 gram of urea and continue the electrolysis for another five minutes (Notes 4 and 5).
If stationary electrodes are employed, the current strength should be about 0.1 ampere, which may, after 12 to 15 hours, be increased to 0.2 ampere. The time required for complete deposition is usually from 20 to 24 hours. It is advisable to add 5 cc. of nitric acid (sp. gr. 1.2) if the electrolysis extends over this length of time. No urea is added in this case.
When the deposition of the copper appears to be complete, stop the rotating mechanism and slowly lower the beaker with the left hand, directing at the same time a stream of water from a wash bottle on both electrodes. Remove the beaker, shut off the current, and, if necessary, complete the washing of the electrodes (Note 6). Rinse the electrodes cautiously with alcohol and heat them in a hot closet until the alcohol has just evaporated, but no longer, since the copper is likely to oxidize at the higher temperature. (The alcohol may be removed by ignition if care is taken to keep the electrodes in motion in the air so that the copper deposit is not too strongly heated at any one point.)