# Water to Fuel to Water: The Fuel Cycle of the Future

## Experimental Procedure

Note Before Beginning: This science fair project requires you to hook up one or more devices in an electrical circuit. Basic help can be found in the Electronics Primer. However, if you do not have experience in putting together electrical circuits you may find it helpful to have someone who can answer questions and help you troubleshoot if your project is not working. A science teacher or parent may be a good resource. If you need to find another mentor, try asking a local electrician, electrical engineer, or person whose hobbies involve building things like model airplanes, trains, or cars. You may also need to work your way up to this project by starting with an electronics project that has a lower level of difficulty.

### Creating the Galvanostatic Electrochemical Cell

1. To start this science fair project, you should assemble the necessary chemicals, electrodes, components, and instruments you need, as specified in the Materials and Equipment list above. Make sure you are familiar with all of the items in the Terms, Concepts, and Questions section above. If you get stuck, or need more detailed explanations, watch the second video in the Introduction by MIT researchers Yogesh Surendranath, Thomas Teets, and Dr. Elizabeth R. Young. It takes you through the project step-by-step.
2. Build a circuit on the breadboard consisting of the batteries, resistor, and voltmeter/multimeter, as shown in Figure 1 below. If you do not have experience building a circuit on a breadboard, use the Science Buddies Breadboard Guide as a reference. Figure 1 shows you what the completed circuit should look like using two different types of breadboards.

Figure 1. The photos on the top show how the various components in the circuit can be wired onto two different types of breadboard. Below each breadboard photo is a photo of the completed circuit using that type of breadboard, including multimeter leads. Note: The Science Buddies kit uses the type of breadboard shown on the left.

1. Using Figure 1 as a visual reference, connect the four 9V batteries in series using some wire and 6 alligator clips.
1. Cut each piece of wire to the desired length with the wire cutters.
2. 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.
3. Note: For some alligator clips, such as the ones in the Science Buddies kit, the stripped wire will need to be coiled around the alligator clips and then screwed in place. This is shown in Figure 2 below.
4. 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. If you are using alligator clips similar to these ones, you will need to coil the stripped wire around the alligator clip and then screw the wire in place. Note: This type of alligator clip is included in the Science Buddies kit.

2. 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 Breadboard Guide if you are confused).
1. 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.
3. Connect the 10K Ohm resistor as shown in Figure 1. (Note: orientation does not matter.)
1. 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.
2. 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.
4. Connect the positive (red) lead from the voltmeter/multimeter to the breadboard as shown in Figure 1.
1. 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).
5. Connect the negative (black) lead from the voltmeter/multimeter to the breadboard as shown in Figure 1.
1. 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.)
6. 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).
1. If you are using the type of breadboard shown on the right, skip this step.
7. 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.
1. 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 Guide to Using 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.
1. 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.
1. 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.
2. Note: If you are using the Science Buddies kit for this project idea, use the 500 mL jar for this step.
2. 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.
1. 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.
2. 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.
3. Note: If you are using the Science Buddies kit for this project idea, use the blue Styrofoam block and 250 mL beaker in the kit for this step.

Figure 3. The photos above show one possible method for suspending the nickel electrodes in the beaker to make the electrochemical cell.

1. 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.
1. 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.
2. Place the stir bar in the bottom of the jar.
1. 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.
3. Connect the nickel electrodes to the rest of the circuit using copper wire and alligator clips as shown below in Figure 4.
1. 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).
1. 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.

Figure 4. The completed galvanostatic electrochemical cell, using two different types of breadboards, is pictured in the top two pictures. One type of breadboard is shown in the left pictures, and a second type is shown in the right pictures. In the top left picture, the leads going up are connected to the nickel electrodes (not pictured). The bottom left picture shows a close-up of the breadboard shown in the top left picture. The bottom right image is a schematic of the completed galvanostatic electrochemical cell pictured in the top right. Note: If you are using the Science Buddies kit for this project idea, you will be using the type of breadboard shown in the left pictures.

Technical Note #1

By following steps 1-7 above you have constructed a simplified galvanostat. This means that the electrochemical cell passes the same current through the cell at all times, and the voltage read-out varies based on the efficiency or property of the electrodes.

The four 9-volt batteries generate a maximum of 36 (9v per battery x 4 batteries in series =36v). You typically will get less than 36 volts depending on how fresh the batteries are. The circuit is completed by two other resistors attached in series. One resistor is the electrochemical cell itself (the nickel electrodes in the phosphate buffer), and the other resistor is a 10,000 Ohm resistor you specifically place in series. This 10,000 Ohm resistor is critical to stabilize the electrochemical cell and ensure that a constant current is passed at all times. The reason for this is that most of the voltage (~30v) drops across the 10,000 Ohm resistor, and approximately 1.5-3v are dropped across the electrochemical cell. It is important to drop most of the voltage through the resistor because this will set the current that passes through the rest of circuit. Small variations in the electrochemical cell will have little effect because the 10,000 Ohm resistor is the dominant factor. Using Equation 3 below, and assuming that approximately 30 volts are dropped over the 10,000 Ohm resistor, the current can be calculated to be 3mA (30v / 10,000 Ohms = 0.003 A = 3mA). This calculation indicates there are 3mA of current flowing through the electrochemical cell.

Equation 3:

• I is current in amperes (A)
• V is voltage in volts (v)
• R is resistance in ohms

### Adding the Cobalt Catalyst and Measuring Its Effects

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.
1. 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.

Technical Note #2

The voltage readout you measure in step 2, above, is the voltage required by the electrochemical cell to maintain a constant current of 3mA (see Technical Note #1 to learn how the current was calculated). This voltage is the sum of the energy required to drive the water-splitting reaction 1.23v + overpotential) and any resistive losses in the cell. If there were no resistive losses, and the water splitting reaction was completely efficient, the necessary voltage to maintain the 3mA current would be 1.23v. From the Introduction, you already know that the water-splitting reaction is not completely efficient and instead has a significant overpotential. In the steps below, you are watching the overpotential drop as the cobalt catalyst is electroplated onto the nickel electrode (specifically, the anode). This drop in overpotential is reflected in a drop in the voltage you measure across the circuit. As the overpotential required by the cell decreases (through addition of the catalyst), the voltage necessary to maintain the 3mA current also decreases. This indicates that you are running the water splitting reaction closer to the absolute, ideal limit. The efficiency of the reaction can be calculated using Equation 4 below.

Equation 4:

If the reaction was 100% efficient, it would require only 1.23v to maintain the 3mA of current passing through the cell. The voltmeter/multimeter would thus read 1.23v. As an example, let us imagine that the initial voltmeter/multimeter reading (in step 2 above) for your electrochemical cell was 2.46v. According to Equation 4, this would mean that without the catalyst, the reaction was 50% efficient (1.23v / 2.46v = 0.50 = 50%). If voltage readings after the addition of the catalyst dropped to 2.12v, then the efficiency would rise to 58% (1.23v / 2.12v = 0.58 = 58%).

1. 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.
1. 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. As shown in the picture above, only a small amount of cobalt nitrate should be added to the buffer at a time.

1. 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.
1. As the reaction takes place, you will see tiny bubbles forming on the nickel electrodes, similar to those in Figure 6 below.

Figure 6. In the beginning, as shown in the photo on the top, there are no bubbles on the nickel electrodes. As the reaction proceeds, the gases formed can be seen as tiny bubbles covering the electrodes, as shown in the photo on the bottom.

1. 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.
1. Record in your lab notebook how long it takes the voltage to stabilize again and what that final voltage reading is.
2. 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.
1. 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.
2. As you add more cobalt nitrate, how does the brown film on the anode change? Record any observations in your lab notebook.
3. 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.
1. The solution that the electrodes were in still contained some un-reacted cobalt nitrate, so the electrodes should be transferred to fresh phosphate buffer.
2. 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.
3. 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.
1. Using Equation 4 and the information in Technical Note #2, calculate the final efficiency of the electrochemical cell with the cobalt-catalyst.
2. 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?
3. How quickly did the cobalt-catalyst form?
4. Plot the rate of increase in efficiency for the number of times you repeated step 6. Was the rate of efficiency increase constant?
5. Clean up and disposal.
1. The phosphate buffer solution can safely be disposed of down the drain.
2. 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.

Technical Note #3

Above, we saw that the efficiency of the reaction is determined by the voltage drop across the electrochemical cell. Higher voltages lead to lower efficiency. But what about the speed at which we produce hydrogen and oxygen? Above, we were running our cell at 3mA, and this current is directly proportional to the rate of hydrogen and oxygen production. What if we slow this rate to 1mA, 0.1mA, or 0.01mA? How would that affect the voltage? Knowing the relationship between the current (rate) and the voltage (energy input) is essential to designing water splitting systems that are practical. As described in Variation 1, change the resistor so that the current is varied between 3mA and 30mA. Plot the cell voltage as a function of the log of the current passed in the cell. Do you get a straight line? What is the slope? Repeat this experiment with catalysts formed for different metal salts (see Variation 2). Plot all of your results on the same graph to determine which catalyst performs the best. Remember that lower voltages and higher currents equal better catalysts.

### Troubleshooting

For troubleshooting tips, please read our FAQ: Water to Fuel to Water: The Fuel Cycle of the Future.

## Variations

• Consider adding a different resistor to your galvanostatic cell. Based on Technical Note #1, calculate the current that would pass through your cell. Add that resistor. What is the voltage now read by the voltmeter? You should stay within a range of 3mA to 30 μA (i.e. you should only use larger resisters than the 10K Ohms). Using a range of different resistors, you can determine the voltage required to run the electrochemical cell at each current delivered by the galvanostatic circuit. More information about this is provided in Technical Note #3.
• Can the water oxidation catalyst be made from metals other than cobalt? How well do these other metals work? You can purchase different metal salt compounds such as ones containing nickel, iron or manganese and try to add those for the electroplating procedure. You can compare the efficiencies of the electrochemical cells with various metal-based catalysts. How do they compare to the cobalt-based catalyst?
• In the Experimental Procedure above, electricity from batteries is used to split water. How would you change the setup to get the energy from sunlight instead of batteries?

## Share your story with Science Buddies!

Q: Can I use a buffer that is different from the one listed in the Materials and Equipment section?
A: For this science project to work as expected, you should use the 0.1 M phosphate buffer solution, pH 7.0 that is described in the Materials and Equipment section. The phosphate in the buffer is needed, in the amounts specified, for the correct chemical reaction with the cobalt nitrate to take place. If you use a different kind of buffer, such as phosphate buffered saline (PBS), this may not react correctly with the cobalt nitrate and the anode will not be coated with the correct chemical. If the reaction is working, the anode should develop a brown film after adding the first pinch of cobalt nitrate, and the film should grow larger and darker as more cobalt nitrate is added. You can try experimenting with different buffers, but if you do this be sure to include the 0.1 M phosphate buffer solution, pH 7.0, as a positive control.
Q: Why does the anode need to be submerged in the phosphate buffer solution half way?
A: If the anode is submerged much less than half way in the phosphate buffer solution, then only a small film will develop on the anode and this can make your results less accurate. Also, if a smaller volume of phosphate buffer solution is used, then it will be difficult to have even small pinches of the cobalt nitrate dissolve completely, and you may end of with cobalt nitrate pieces floating in the solution.
Q: Why do I need to use a stir plate and stir bar?
A: A stir plate and stir bar are needed to help dissolve the cobalt nitrate as it is added. It is true that stirring with a stirrer or spoon could dissolve the cobalt nitrate in the phosphate buffer solution, but this should not be done for three important reasons:
1. Cobalt nitrate can cause skin and eye irritation, and consequently stirring the cobalt nitrate into solution in an open beaker without eye protection can be dangerous.
2. For this science project to work correctly, it is very important that the nickel metal electrodes do not get jostled and moved out of position. It can take several minutes of stirring for the cobalt nitrate to completely dissolve and when the electrodes are taken off of the beaker, set aside, and then set back on the beaker, this increases the chance that they will be knocked out of the position they were originally in and affect the results.
3. The chemical reactions that happen as the cobalt nitrate dissolves in the buffer could be disrupted by side-reactions that may happen with a stirrer or spoon. (Stir bars are treated so that they should not be reactive.)
Q: My results are not what I expected them to be. Why might this be?
A: Here are the kind of voltage readings you should be seeing throughout this science project:
• In the circuit with only the batteries, resistor, and voltmeter/multimeter, the voltage should read > 30 Volts (V). If it is less than this, you probably need to use fresher batteries.
• When the circuit is completed (it includes the nickel strip electrodes in the original 0.1 M phosphate buffer solution, pH 7.0), the voltage should then read between 1.9-2.4 V. It may take 20 minutes or more for the reading to stabilize. If your stabilized voltage is not within this range, check the following:
• Make sure everything is hooked up correctly (using Figures 2 to 4 for reference).
• Check that none of the alligator clips or exposed wires are touching each other.
• Make sure that the electrodes are 1-2 centimeters (cm) apart.
• Check that all of the alligator clips and wires are securely attached where they are supposed to be.
• If your voltage is lower than this range, the electrodes may not be sufficiently clean; if they do not look completely clean, put them in a cup or jar again with fresh cola for at least five minutes, making sure they are entirely immersed the whole time.
• After four or five pinches of cobalt nitrate, the voltage should be significantly less, such as around 1.7 V if your original completed circuit reading was 1.9 V. Each time a pinch of cobalt nitrate is added, the voltage should decrease and it may take between 5 to 25 minutes for the voltage reading to stabilize, so some patience is required! If you do not see the voltage decrease after waiting for 15 to 20 minutes, check and do the following:
• Make sure that the stir bar is dissolving the cobalt nitrate. If the stir bar seems to be missing pieces of settled cobalt nitrate, gently move the jar on the stir plate a little so the stir bar is stirring the cobalt nitrate. Be careful not to change the position of the electrodes.
• Try adding a slightly larger pinch of cobalt nitrate.
• When the electrodes are placed in fresh phosphate buffer at the end of the experiment, the voltage should be lower than it was in the original completed circuit, but a little higher than your last reading in the phosphate buffer with cobalt nitrate in it. For example, if your original completed circuit reading was 1.9 V, and it stabilized at 1.7 V after adding several pinches of cobalt nitrate, the reading in fresh phosphate buffer may be around 1.7-1.8 V. It may take at least 10 minutes for this final reading to stabilize. If the voltage in the fresh phosphate buffer at the end of the experiment is not lower than it was in the original completed circuit, check the following:
• Make sure everything is still hooked up correctly and the electrodes have not been knocked out of position.
• Check that the fresh buffer level is not higher than the original buffer level was (or, in other words, make sure the fresh buffer does not go above where the brown film is coating the anode).
• Tip: When you lift up the nickel metal electrodes to add a pinch of cobalt nitrate, do not set the electrodes down as this may knock them out of position. If the electrodes become knocked out of their original position, this can affect your results.
Q: I am not sure if I am wiring the breadboard correctly. What should I do?
A: Refer to Figures 1 and 4 in the project idea for how to wire the breadboard. The breadboard does not need to be wired exactly as shown in these figures; as long as the correct circuit is being made, the project should work. This is how the complete circuit should be set up in this science project:
• Connect the positive end of the series of batteries to the power bus (far left) column on the breadboard.
• Connect the resistor so that it will transmit electricity from the power bus to the voltmeter/multimeter's positive lead. How to do this depends on which type of breadboard you have; see Figures 1 and 4 for details.
• Connect the voltmeter/multimeter's positive lead so that it receives the electricity from the resistor. This means that the positive lead will be in the same row as the resistor.
• Connect one of the nickel strip electrodes so that it is also in this row. This will be the anode.
• Connect the other nickel strip electrode so that it will transmit electricity to the other half of the breadboard. This will be the cathode.
• Connect the voltmeter/multimeter's negative lead so that it receives electricity from the cathode. This means that the negative lead will be in the same row as the cathode.
• Depending on the type of breadboard you have (see Figures 1 and 4), you may then need to connect a wire from this row to the ground bus (far right) column on the breadboard. Then connect the negative end of the series of batteries to the ground bus column.
• If you do not need to connect a wire to the ground bus, just connect the negative end of the series of batteries to the far right column, in the same row as the voltmeter/multimeter's negative lead and cathode.

Q: How do I know when the voltage has "stabilized"?
A: It may take as much as 25 minutes, and possibly even more time, for the voltage to stabilize when you are taking measurements in this science project. If the voltage is staying within a certain voltage range that is about ± 0.02 V (such as ranging from 1.71-1.75 V) for at least five minutes, then it has probably stabilized.
Q: How do I use a voltmeter/multimeter to measure the voltage?
A: In this science project you will be performing voltage tests with the voltmeter/multimeter. Please refer to the Science Buddies Guide to Using a Multimeter and the manual for your voltmeter/multimeter for help on doing this. Make sure that the leads of the voltmeter/multimeter are connected to the circuit as shown in Figures 1 and 4 in the project idea.

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