CHM674 – Advanced Electrochemistry

Experiment 2: Electrolytic Cell – Electrolysis of Aqueous Solutions

Objectives:

a) to identify the reactions occurring at the anode and cathode during the electrolysis
of various aqueous salt solutions
b) to observe the electrolysis of water and the gases liberated at the electrodes.
c) to study the suitable electrode and aqueous solution for water splitting process.

Procedure Overview:

The products that result from the electrolysis of various salt solutions are observed and
identified.

Carbon/Graphite Rods, Copper wires/plates, U-tube or Beaker,

Power Supply or Battery 6 V, Two wire leads with crocodile clips,
Materials/Apparatus:
Retort stand with clamp or Cardboard with two holes, litmus paper
(blue)

NaCl solution, NaBr solution, Na2SO4 solution, Phenolphtalein

Chemicals:
indicator

1. Set Up the Electrolysis Apparatus

Connect two wire leads (different colours) attached to crocodile clips to a direct current
(DC) power supply. Mount a glass U-tube on a ring stand or clamp at a retort stand (as in
Figure 2.1a) or use a beaker to set up the electrolytic cell as in Figure 2.1b. Connect the
alligator clips to the corresponding electrodes, listed in Table 2.1.

2. Electrolyze the Solutions

Fill the U-tube or beaker three-forths full with a solution from Table 2.1 and add 10 drops
of phenolphtalein. Electrolyze the solution at 6V for 5 minutes. Use the suggested

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electrodes. During the electrolysis, look closely at each electrode watch for any evidence
of a reaction in the anode and cathode chambers. (Note: test for Cl 2 gas: A greenish-
yellow gas with a pungent and choking smell is released or the gas turns the blue litmus
paper red and then white)

Table 2.1: Electrolytic Cells for Study

Solution Electrodes (Anode and Cathode)

Distilled Water Carbon (Graphite)
0.001M NaCl Carbon (Graphite)
0.5 M NaCl Carbon (Graphite)
0.5 M NaBr Carbon (Graphite)
0.5 M Na2SO4 Polished Copper Metal Strips
0.5 M Na2SO4 Carbon (Graphite)

Safety:

Disposal: Discard all the salt solutions into the ‘Waste salts’ container.

Handling securely the power supply to avoid electrical shock.

Set up the elctrolytic cell either using beaker or U-tube as shown in Figure 2.1.

(a) (b)

Figure 2.1

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Report Sheet

Fill in the following tables (Table 1 and 2) with your observations and interpretations
from the electrolytic cells. Describe what you observe occuring at the two electrodes.

Table 1

Electrolyte Electrodes Observations (ie: Gas Evolved? Pink colour at

Solution electrode?)

Distilled Water Carbon/Carbon

(C/C)

0.001M NaCl Carbon/Carbon

(C/C)

0.5 M NaCl Carbon/Carbon

(C/C)

0.5 M NaBr Carbon/Carbon

(C/C)

0.5 M Na2SO4 Carbon/Carbon

(C/C)

0.5M Na2SO4 Copper/Copper

(Cu/Cu)

Table 2

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CHM674 – Advanced Electrochemistry

Electrolyte Dissociation of Electrolytes Expectation of selected ion and product

Solution

Ions migrating to cathode:

NaCl Ion discharged at cathode:
(Dilute) Product at cathode:

Ions migrating to anode:

Ion discharged at anode:
Product at anode:

NaCl Ions migrating to cathode:

(Concentrated) Ion discharged at cathode:
Product at cathode:

Ions migrating to anode:

Ion discharged at anode:
Product at anode:

Ions migrating to cathode:

NaBr Ion discharged at cathode:
Product at cathode:

Ions migrating to anode:

Ion discharged at anode:
Product at anode:

Ions migrating to cathode:

Na2SO4 Ion discharged at cathode:
Product at cathode:

Ions migrating to anode:

Ion discharged at anode:
Product at anode:

Questions:
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CHM674 – Advanced Electrochemistry

1. Would solid NaCl conduct electricity? Why did the salt make the water more
conductive to electricity?

2. What gases were formed at anode and cathode in beaker containing 0.5M NaCl?
Write the half-reaction that occurred in this beaker.

3. What was the purpose of adding phenolphtalein to the solution?

4. If copper electrodes had been used instead of the carbon (graphite) electrodes for the
electrolytic cells, the observed reactions may have been different. Why?

5. Why does more gas form at one electrode than at the other electrode for electrolysis
of 0.5M Na2SO4 solution?

6. In the electrolysis of an aqueous salt solution, the nitrate ion, NO 3- , migrates to the
anode. Considering that the nitrogen in the NO 3- (aq) is at its maximum oxidation
state (of +5), what electrolysis products(s) might you expect to observe at the anode?

7. Calculate the volume of gases that will be collected at anode and cathode when an
aqueous solution of Na2SO4 is electrolyzed for 2 hours with a 10 A current.

8. Describe in your own words the whole process of electrolysis of water from your
findings (including the electrochemical reactions occur at both electrodes, the
suitable electrode and electrolyte used).