Creating the Galvanostatic Electrochemical Cell

Figure 1.
a.Using Figure 1 as a visual reference, connect the four 9V batteries in series using some wire
and 6 alligator clips.

i.Cut each piece of wire to the desired length with the wire cutters.

ii.When using wire to attach components in a circuit, the ends of each piece of wire need to be
stripped, with the wire stripper, before creating the connection.

iii.Note: For some alligator clips, the stripped wire will need to be coiled around the alligator
clips and then screwed in place. This is shown in Figure 2 below.

iv.Connect the batteries so that the negative end of one battery is connected to the positive end
of the next battery in the series.

Figure 2.
b.Using a piece of wire, connect the positive end of the series of batteries to the breadboard
power bus (far left column, see the Science Buddies reference How to Use a Breadboard if you
are confused).

i.In Figure 1, for the type of breadboard shown on the left this is the far left "+" column, and
for the type of breadboard shown on the right this is the unmarked far left column.

c.Connect the 10K Ohm resistor as shown in Figure 1. (Note: orientation does not matter.)

i.For the breadboard shown on the left, one end of the resistor is connected to the same
column as the positive end of the batteries, and the other end of the resistor is connected to
position 1a.

ii.For the breadboard shown on the right, one end of the resistor is connected to the same row
as the positive end of the batteries, and the other end of the resistor is connected to another
position in the same column.

d.Connect the positive (red) lead from the voltmeter/multimeter to the breadboard as shown in
Figure 1.

i.For both types of breadboards, the voltmeter/multimeter's positive lead is connected to a

position in the same row as the end of the resistor (in the breadboard shown on the left, this is
position 1c).
e.Connect the negative (black) lead from the voltmeter/multimeter to the breadboard as shown
in Figure 1

i.For both types of breadboards, the voltmeter/multimeter's negative lead is connected to a

position on the right half of the breadboard. (In the breadboard on the left in Figure 1, position
7h is used.)

f.If you are using the type of breadboard shown on the left in Figure 1, connect a small piece of
wire between a position in the same row as the voltmeter/multimeter's negative lead (7j is used
in Figure 1) and the ground bus (the far right "-" column).

i.If you are using the type of breadboard shown on the right, skip this step.

g.Using a piece of wire, attach the negative (-) end of the series of batteries to the ground bus
(far right column) of the breadboard as shown in Figure 1.

i.If you are using the type of breadboard shown on the right, make sure this is in the same row
as the voltmeter/multimeter's negative lead.

3.The circuit is now complete and should look like the circuit in Figure 1. Using the
voltmeter/multimeter, make sure the circuit reads >30V. If you need help using a multimeter,
consult the Science Buddies reference How to Use a Multimeter, as well as the instruction
manual that came with your voltmeter/multimeter.

4.Use the nickel metal strips as electrodes. The nickel electrodes will serve as the scaffold for
formation or electroplating of the cobalt catalyst.

a.To clean the electrodes (nickel metal strips), pour some cola into a cup or jar. Put both
electrodes in the cola. Make sure the nickel is entirely immersed. Cola contains phosphoric acid.
This acid will do a great job of cleaning the surface of the electrodes. After a few minutes,
remove the nickel electrodes, wash them off with plain water, and dry them.

i.If the jar is too small to immerse the electrodes, do the procedure once then flip the
electrodes over (putting the end that was not previous immersed in the Cola) and repeat.

ii.Note: Use the 500 mL jar for this step.

b.Construct a method to secure electrodes within a small beaker or jar that leaves the top of the
electrodes readily available to make an electrical connection to the rest of the circuit you started
preparing above. An example of a method to secure the electrodes is shown in Figure 3 below
using a piece of Styrofoam to hold the electrodes securely in place.
 i.It is important to ensure that the separation between the electrodes remains the same
throughout the experiment. When securing the electrodes make sure to:

·Position the electrodes 1-2 centimeters (cm) apart.

·Make sure the electrodes are securely in place and not dangling freely or touching the sides
of the beaker.

ii.Position the electrodes so that they will, later, once the buffer has been added to the
beaker, only be immersed half way in the buffer. Note: It is critical that the top of the electrodes
do not touch the buffer.

iii.Note: Use the Styrofoam disc and the 250 mL beaker for this step.

Figure 3.
5.Add 0.1 M phosphate buffer solution, pH 7.0, to the beaker with electrodes so that the nickel
electrodes are submerged half way in the buffer solution.

a.Note: If you only have 500 mL of phosphate buffer, the most you should fill the beaker with
is 250 mL because in a later step you will need to use this same amount of phosphate buffer
again.

6.Place the stir bar in the bottom of the jar.

a.Make sure that the electrodes are not so low that they will be bumped by the stir bar. If they
are, raise them up until they are not.

7.Connect the nickel electrodes to the rest of the circuit using copper wire and alligator clips as
shown below in Figure 4.

a.For both types of breadboards shown, one wire is connected to a position in the same row as
the voltmeter/multimeter's positive lead, and the other wire is connected to a position in the
same row as the voltmeter/multimeter's negative lead (on the other half of the breadboard).

i.For example, for the breadboard shown on the left, one wire is connected to position 1e,
and the other wire is connected to position 7f.

Adding the Cobalt Catalyst and Measuring Its Effects

Figure 4.
1.With the electrodes securely in place inside the small beaker, place the beaker on the
magnetic stir plate. Turn on the stir plate and get the stir bar moving at a constant rate.

a.Make sure that the stir bar does not bump the electrodes. Adjust the electrodes if needed,
but then keep them in the same position throughout the rest of the experiment.

2.Monitor the voltage readout on the voltmeter/multimeter. It should range between 1.9-2.4v
and will take at least five minutes to stabilize. After the voltage reading has stabilized, record
this voltage in your lab notebook. This is the baseline voltage value for your electrochemical cell.

3.Using Equation 4, below, and the information in Technical Note #2, calculate the baseline
efficiency of the water splitting reaction in your electrochemical cell.

4.Now it is time to add the reactant necessary to form the cobalt-based catalyst. Put on a pair of
disposable gloves and, using the metal scoop, add a pinch of the cobalt nitrate to the jar with
the phosphate buffer and either start the stopwatch, or write down the time in your lab
notebook. With the cobalt source and the energy provided by the batteries, the catalyst will
start to form.

a.Adding small amounts of cobalt nitrate each time is critical. The cobalt nitrate
concentration must remain very low so the solution does not become cloudy. See Figure 5,
below, for a visual reference of how much cobalt nitrate to add at a time.

Figure 5.
5.The cobalt-based catalyst will begin to electroplate onto the anodic (connected to + side of
the battery) nickel electrode. As the catalyst film grows, you will see a brown film growing on
the anode, and the voltage readout on the voltmeter/multimeter will slowly drop. Eventually,
after several minutes, the voltage will settle to a stable reading. Record this voltage readout.
Also record how long it took, using either the stopwatch or clock, to reach a stable voltage
reading.

a.As the reaction takes place, you will see tiny bubbles forming on the nickel electrodes,
similar to those in Figure 6 below.

Figure 6.
6.Once the voltage readout stabilizes, you can add more cobalt nitrate to the solution to
initiate formation of more cobalt-based catalyst. Again, add only a small amount of cobalt
nitrate at a time.
 a.Record in your lab notebook how long it takes the voltage to stabilize again and what that
final voltage reading is.

7.Repeat step 6 until the voltage does not appear to change with the addition of more cobalt
nitrate. In this instance, the cobalt-based catalyst will continue to work, but no additional
catalyst material will form.

a.This may take a total of four or five additions of small amounts of cobalt nitrate, and with
each addition it may take around 5 to 20 (or more) minutes for the voltage to stabilize.

b.As you add more cobalt nitrate, how does the brown film on the anode change? Record
any observations in your lab notebook.

8.Use a permanent marker to make a mark on the side of the beaker where the phosphate
buffer solution level is. Then, have a helper carefully remove the nickel electrodes from the
beaker and hold them. While the helper is holding the electrodes, empty the beaker (the
phosphate buffer solution can safely be disposed of down the drain), rinse and dry the beaker,
and then re-fill it with the same amount of fresh phosphate buffer that was originally in the
beaker. This means you will be re-filling the beaker to the mark you just made on it using the
permanent marker.

a.The solution that the electrodes were in still contained some un-reacted cobalt nitrate, so
the electrodes should be transferred to fresh phosphate buffer.

b.Note: Be careful that you or your helper does not jostle the electrodes when transferring
them to the new solution. It is important that they remain in the same position relative to each
other and stay the same distance apart or it could give you inaccurate results.

c.At this point you have finished forming the cobalt-based catalyst on the nickel electrodes.
Measure and record the stabilized voltage one last time. The voltage readout in pure phosphate
buffer reflects the operating potential of the electrochemical cell.

9.Analyze your data.

a.Using Equation 4 and the information in Technical Note #2, calculate the final efficiency of
the electrochemical cell with the cobalt-catalyst.

b.Compare the original efficiency of the cell calculated in step 3 to the final efficiency. How
much does the cobalt-based catalyst increase the efficiency of the electrochemical cell?

c.How quickly did the cobalt-catalyst form?

 d.Plot the rate of increase in efficiency for the number of times you repeated step 6. Was the
rate of efficiency increase constant?

10.Clean up and disposal.

a.The phosphate buffer solution can safely be disposed of down the drain.

b.The nickel electrodes can be saved with the cobalt-based catalyst still on them. Or, the
nickel electrodes can be recovered and used again by rinsing them in cola as in step 4a, above,
of the Creating the Galvanostatic Electrochemical Cell section.