EXPERIMENT 6
QUANTITATIVE
DETERMINATION OF COPPER BY COULOMETRY
Objective: To quantitatively determine the
concentration of copper in an unknown solution.
An acidic, copper containing solution can be electrolyzed, causing the copper to deposit onto the cathode of the cell. The overall reaction is
Cu2+
+ H2O ® Cu(s) + ½ O2(g)
+ 2H+
The half reactions are as follows:
Cu2+
+ 2e- Û Cu(s)
½ O2(g)
+ 2H++ 2e- Û H2O
Using this idea, the amount of copper in a solution
can be determined by placing two platinum electrodes into an acidified copper
solution and applying an electrical current across it. The cathode can be weighed before the
experiment and after the experiment to determine how much copper has plated
onto it. This weight difference should
be equal to the amount of copper that was in the solution.
1)
Cleaning
the electrode – Handle the gauze electrode with a Kim-wipe or tissue and dip
the
electrode into a hot 8 M HNO3 solution to
remove any previous deposits. Wash the
electrode with distilled water and then with ethanol. Place the electrode into a 100°C oven for about 5 minutes
and then allow it to cool to room temperature.
Weigh the electrode accurately to obtain the initial weight.
2)
Preparation
of the solution – Place EXACTLY 50.00 mL of the copper sulfate solution into a
250 mL beaker and add to it 3 mL of 98% sulfuric
acid and 2 mL of 8M HNO3. To
measure the copper sulfate solution be sure to use a volumetric pipet.
3)
Electrolytical
cell setup – Position the gauze electrode (cathode) so that the gauze portion
is
not completely submerged into the copper
solution. Position the anode so that it
is not in contact with the cathode.
Switch on the electrical current and adjust to 2 amperes and also record
the voltage reading from the meter. In
addition, record the initial starting time after switching on the power.
4)
When
the blue color of the copper solution has disappeared COMPLETELY, add some
distilled water to submerge the unexposed portion of
the cathode. Wait several minutes and
check to see if additional deposition of copper has occurred on the fresh
portion of the cathode. If more copper
has deposited, wait an additional 10 minutes and check again. If no more copper has deposited then raise
the electrode assembly and shut off the current.
5)
Gently
wash the electrode with water and ethanol and place the electrode into the oven
for
five minutes.
6)
After
cooling to about room temperature, reweigh the electrode to find the final
mass. The
difference in final and initial weights is
approximately the amount of copper that was in the 50.00 mL of solution.
Please be sure to include
proper unit labels!
1 2
Electrical current used:
Voltage Used
Volume of solution used:
Approximate time for
hydrolysis:
Mass of Pt gauze electrode
prior to
electrolysis:
Concentration of CuSO4
Standard Deviation of the
two runs:
Questions:
1)
How do you know whether the
electrolysis is complete?
2)
Why is the
electrogravimetric technique considered to be very accurate?
3)
What is the major drawback
of the electrogravimetric device you used?
4) Be sure to include a sample calculation for the concentration of
CuSO4.
Notebook: Final Grade: