I.

EXPERIMENT TITLE : REDOX AND ELECTROCHEMISTRY CELL

II. EXPERIMENT DATE : March 17th, 2014 at 07.00
III. END OF THE EXPERIMENT : March 17th, 2014 at 09.30
IV. EXPERIMENT PURPOSE :
1. To identification redox reaction based on color changing which observed
2. To determine electricity movement capacity of galvanic cell
3. To examine KI solution electrolysis
V. BASIC THEORY :

1. REDOX REACTION

Electrochemistry is the branch of chemistry that deals with the interconvertion

of electrical energy and chemical energy. Electrochemical processes are Redox
(reduction-oxidation) reactions include all chemical reactions in which atoms have
their oxidation state changed. This can be either a simple redox process, such as the
oxidation of carbon to yield carbon dioxide (CO2) or the reduction of carbon by
hydrogen to yield methane (CH4), or a complex process such as the oxidation of
glucose (C6H12O6) in the human body through a series of complex electron transfer
processes.

OXIDATION AND REDUCTION IN TERMS OF OXYGEN TRANSFER

Definitions : Oxidation is gain of oxygen; Reduction is loss of oxygen.

For example, in the extraction of iron from its ore:

Because both reduction and oxidation are going on side-by-side, this is known as a
redox reaction.

Experiment Report | Redox and Electrochemical Cell 1

 Oxidising And Reducing Agents

An oxidising agent is substance which oxidises something else. In the above

example, the iron(III) oxide is the oxidising agent. A reducing agent reduces
something else. In the equation, the carbon monoxide is the reducing agent.

 Oxidising agents give oxygen to another substance.

 Reducing agents remove oxygen from another substance.

OXIDATION AND REDUCTION IN TERMS OF HYDROGEN TRANSFER

These are old definitions which aren't used very much nowadays. The most likely place
you will come across them is in organic chemistry.

Definitions: Oxidation is loss of hydrogen; Reduction is gain of hydrogen.

Notice that these are exactly the opposite of the oxygen definitions.
For example, ethanol can be oxidised to ethanal:

You would need to use an oxidising agent to remove the hydrogen from the ethanol. A
commonly used oxidising agent is potassium dichromate(VI) solution acidified with
dilute sulphuric acid.

Ethanal can also be reduced back to ethanol again by adding hydrogen to it. A possible
reducing agent is sodium tetrahydridoborate, NaBH4. Again the equation is too
complicated to be worth bothering about at this point.

An update on oxidising and reducing agents

 Oxidising agents give oxygen to another substance or remove hydrogen from it.
 Reducing agents remove oxygen from another substance or give hydrogen to it.

Experiment Report | Redox and Electrochemical Cell 2

OXIDATION AND REDUCTION IN TERMS OF ELECTRON TRANSFER

This is easily the most important use of the terms oxidation and reduction at A' level.
Definitions: Oxidation is loss of electrons ;Reduction is gain of electrons.

It is essential that you remember these definitions. There is a very easy way to
do this. As long as you remember that you are talking about electron transfer:

L E O the lion says G E R !

Oxidation

Reduction
Gain
Electron

Electrons
Lost

Example:
Copper (II) oxide and magnesium oxide are both ionic. Being in the form of non-
metal ions. If this reaction is rewritten as an ionic equation, it turns oxide ions are
spectator ions (ions audience).

Magnesium is a reducing agent (reductant). In contrast, the copper (II) electron

transfer from magnesium to produce magnesium ions. Thus, the copper (II) acts as
an oxidizing agent (oxidant).

2. ELECTROLYTIC CELLS

Electrolysis is the process in which electrical energy is used to cause a

nonspontaneous chemical reaction to occur. An electrolytic cell is an apparatus for
carrying out electrolysis. The same principles underlie electrolysis and the process
that take place in galvanic cells.

Experiment Report | Redox and Electrochemical Cell 3

 Electrolysis is the passage of a direct electric current through an ionic substance
that is either molten or dissolved in a suitable solvent, resulting in chemical
reactions at the electrodes and separation of materials.The main components
required to achieve electrolysis are :

 An electrolyte : a substance containing free ions which are the carriers of

electric current in the electrolyte. If the ions are not mobile, as in a solid salt
then electrolysis cannot occur.
 A direct current (DC) supply : provides the energy necessary to create or
discharge the ions in the electrolyte. Electric current is carried by electrons in
the external circuit.
 Two electrodes : an electrical conductor which provides the physical interface
between the electrical circuit providing the energy and the electrolyte

Electrodes of metal, graphite and semiconductor material are widely used. Choice
of suitable electrode depends on chemical reactivity between the electrode and
electrolyte and the cost of manufacture.

PROCESS OF ELECTROLYSIS

The key process of electrolysis is the interchange of atoms and ions by the removal
or addition of electrons from the external circuit. The desired products of
electrolysis are often in a different physical state from the electrolyte and can be
removed by some physical processes. For example, in the electrolysis of brine to
produce hydrogen and chlorine, the products are gaseous. These gaseous products
bubble from the electrolyte and are collected.
2 NaCl + 2 H2O → 2 NaOH + H2 + Cl2

Experiment Report | Redox and Electrochemical Cell 4

 A liquid containing mobile ions (electrolyte) is produced by:

 Solvation or reaction of an ionic compound with a solvent (such as water) to

produce mobile ions
 An ionic compound is melted (fused) by heating
An electrical potential is applied across a pair of electrodes immersed in the
electrolyte.
Each electrode attracts ions that are of the opposite charge. Positively charged ions
(cations) move towards the electron-providing (negative) cathode, whereas
negatively charged ions (anions) move towards the positive anode.
At the electrodes, electrons are absorbed or released by the atoms and ions. Those
atoms that gain or lose electrons to become charged ions pass into the electrolyte.
Those ions that gain or lose electrons to become uncharged atoms separate from
the electrolyte. The formation of uncharged atoms from ions is called discharging.
The energy required to cause the ions to migrate to the electrodes, and the energy
to cause the change in ionic state, is provided by the external source of electrical
potential.

OXIDATION AND REDUCTION AT THE ELECTRODES

Oxidation of ions or neutral molecules occurs at the anode, and the reduction of
ions or neutral molecules occurs at the cathode. For example,

The anode: Fe2+aq → Fe3+aq + e–

The cathode: Fe(CN)3-6 + e– → Fe(CN)4-6

The substances oxidised or reduced can also be the solvent (usually water) or the
electrodes. It is possible to have electrolysis involving gases. (Such as when using
a Gas diffusion electrode)

ENERGY CHANGES DURING ELECTROLYSIS

The amount of electrical energy that must be added equals the change in Gibbs free
energy of the reaction plus the losses in the system. The losses can (in theory) be
arbitrarily close to zero, so the maximum thermodynamic efficiency equals the
enthalpy change divided by the free energy change of the reaction. In most cases, the

Experiment Report | Redox and Electrochemical Cell 5

electric input is larger than the enthalpy change of the reaction, so some energy is
released in the form of heat. In some cases, for instance, in the electrolysis of steam
into hydrogen and oxygen at high temperature, the opposite is true. Heat is absorbed
from the surroundings, and the heating value of the produced hydrogen is higher than
the electric input.

3. GALVANIC OR VOLTAIC CELLS

A galvanic cell, or voltaic cell, named after Luigi Galvani, or Alessandro Volta
respectively, is an electrochemical cell that derives electrical energy from spontaneous
redox reactions taking place within the cell. It generally consists of two different
metals connected by a salt bridge, or individual half-cells separated by a porous
membrane.

Volta was the inventor of the voltaic pile, the first electrical battery. In common
usage, the word "battery" has come to include a single galvanic cell, but a battery
properly consists of multiple cells.

In its simplest form, a half-cell consists of a solid metal (called an electrode) that is
submerged in a solution; the solution contains cations of the electrode metal and
anions to balance the charge of the cations. In essence, a half-cell contains a metal in
two oxidation states; inside an isolated half-cell, there is an oxidation-reduction
(redox) reaction that is in chemical equilibrium, a condition written symbolically as
follows (here, "M" represents a metal cation, an atom that has a charge imbalance due
to the loss of "n" electrons):

Mn+ (oxidized species) + ne- M (reduced species)

Experiment Report | Redox and Electrochemical Cell 6

A galvanic cell consists of two half-cells, such that the electrode of one half-cell is
composed of metal A, and the electrode of the other half-cell is composed of metal B;
the redox reactions for the two separate half-cells are thus:
An+ + ne- A
Bm+ + me- B
In general, then, these two metals can react with each other:
m A + n Bm+ n B + m An+

In other words, the metal atoms of one half-cell are able to induce reduction of the
metal cations of the other half-cell; conversely stated, the metal cations of one half-
cell are able to oxidize the metal atoms of the other half-cell. When metal B has a
greater electronegativity than metal A, then metal B tends to steal electrons from
metal A (that is, metal B tends to oxidize metal A), thus favoring one direction of the
reaction:

m A + n Bm+ n B + m An+
This reaction between the metals can be controlled in a way that allows for doing
useful work:
 The electrodes are connected with a metal wire in order to conduct the electrons
that participate in the reaction. In one half-cell, dissolved metal-B cations
combine with the free electrons that are available at the interface between the
solution and the metal-B electrode; these cations are thereby neutralized, causing
them to precipitate from solution as deposits on the metal-B electrode, a process
known as plating. This reduction reaction causes the free electrons throughout the
metal-B electrode, the wire, and the metal-A electrode to be pulled into the metal-
B electrode. Consequently, electrons are wrestled away from some of the atoms
of the metal-A electrode, as though the metal-B cations were reacting directly
with them; those metal-A atoms become cations that dissolve into the
surrounding solution. As this reaction continues, the half-cell with the metal-A
electrode develops a positively charged solution (because the metal-A cations
dissolve into it), while the other half-cell develops a negatively charged solution
(because the metal-B cations precipitate out of it, leaving behind the anions);
unabated, this imbalance in charge would stop the reaction.

Experiment Report | Redox and Electrochemical Cell 7

  The solutions are connected by a salt bridge or a porous plate in order to conduct
the ions (both the metal-A cations from one solution, and the anions from the
other solution), which balances the charges of the solutions and thereby allows
the reaction between metal A and metal B to continue without opposition.
By definition:
 The anode is the electrode where oxidation (loss of electrons) takes place; the
anode attracts anions (negatively charged ions flow to the anode, while electrons
are expelled through the wire). The metal-A electrode is the anode.
 The cathode is the electrode where reduction (gain of electrons) takes place; the
cathode attracts cations (positively charged, oxidized metal ions flow toward
cathode as electrons are travel through the wire). The metal-B electrode is the
cathode.

VI. TOOLS AND MATERIALS

TOOLS MATERIALS
A. B.
1. Beaker glass 1. H2O2 3% 11. K2Cr2O7 0,1M
2. Test tube 2. FeCl3 0,1M 12. CuSO4 1M
3. Rack 3. HNO3 concentrated 13. ZnSO4 1M
4. U-pipe 4. Amyllum 14. KNO3 1M
5. Carbon 5. I2 solution 15. Phenolphthalein
6. Voltmeter 6. (NH4)2Fe(SO4)2 16. CHCl3
7. Battery 6 volt 7. KSCN 0,1M 17. Cooper plat
8. Cable 8. H2SO4 2M 18. Zinc plat
9. KI 0,1M

Experiment Report | Redox and Electrochemical Cell 8

VII. LANES WORK

1. REDOX REACTION

A.
Tube 1 Tube 2 Tube 3

5 drops I2 1 ml KI 0.1 M 5 1 ml KI 0.1 M 5 drops 1 ml KI 0.1 M 5 drops

solution drops starch solution starch solution starch solution

- diluted - added 1 ml H2SO4 2M - added 1 ml H2SO4 2M - added HNO3

concentrate
- added 2 drops starch - added 0.5 ml H2O2 3% - added FeCl3 0.1 M
solution

Color changing Color changing Color changing

Similar Color

B.

U-Tube
H2SO4 2M solution until ±
2cm from the top of the tube

+ 2 ml of K2Cr2O7 0,1 M + 2 ml of concentrate (NH4)2Fe(SO4)2

on the top of the left tube
+5 drops of KSCN 0,1 M on the top
of right tube
2 ml of FeCL3
Color of solution Color of solution
Compare solution + KSCN

Immersed carbon
Immersed carbon
electrode 2 cm
electrode 2 cm

Color of solution

Experiment Report | Redox and Electrochemical Cell 9

 2. GALVANIC CELL

Beaker glass 1 Beaker glass 2

15 ml of CuSO4 0.1M 25 ml of ZnSO4 0.1M

- entered into beaker glass 100 ml - entered into beaker glass 100 ml

- immerse the copper plat - immersed the zinc plate

- connected with salt bridge that made from

rolled tissue paper and immersed in KCl
solution
Voltage

3. ELECTROLYTIC CELL

KI 0.25 M

- entered into U-tube until 2 cm from the top tube

- Immersed carbon electrode 2 cm in the right and left tube.

Connected left carbon electrode Connected right carbon electrode

with positive of 6V electrode with negative of 6V electrode

Color of solution Color of solution

2 ml result of electrolysis Color changing 2 ml result of electrolysis

from Anode from cathode

- took result test tube - took into test tube

- added by 1 ml of CHCl3 - added phenolphthalein

Color Changing - added FeCl3

Color changing

Experiment Report | Redox and Electrochemical Cell 10

 VIII. RESULT OF THE EXPERIMENT
Result of The Experiment
Experiment Procedure Assumption/Reaction Conclusion
Before After
1. REDOX REACTION I2: yellow I2+amylum: black Test tube 1: 2KI(aq) Redox reaction between
solution bluish +H2SO4(aq) +H2O2(aq) → I2 and starch solution
A. Tube 1 Tube 2 Tube 3
KI: colorless Tube 1: 2H2O(aq) + K2SO4(aq) + produce black bluish
5 drops I2 1 ml KI 0.1 1 ml KI 0.1 1 ml KI 0.1 solution KI+amylum+H2S I2(s) colour.
solution M 5 drops M 5 drops M 5 drops
starch starch starch Amylum: O4+H2O2: purple Redox reaction which
solution solution solution colorless Tube 2: Test tube 2: occur on comparison, 2

- added 1 ml - added 1 ml - added solution KI + amylum+ 2KI(aq) +H2SO4(aq) and 3 tube produce
- diluted
HNO3
H2SO4 2M H2SO4 2M H2SO4: colorless H2SO4+ FeCl3: +FeCl3(aq) → 2FeCl3(aq) similar colour.
concentrate
- added 2
drops starch - added 0.5 ml - added FeCl3 solution black yellowish + K2SO4(aq) + I2(aq) +
solution H2O2 3% 0.1 M
H2O2: colorless Tube 3: HCl(aq)
Purple Black Black solution KI+Amylum+HN
Yellowish Bluish HNO3: colorless O3:black bluish Test tube 3
solution 2KI(aq) + 2HNO3(aq) →
2KNO3(aq) + I2(aq) +
H2(g)

Similar
Color

Experiment Report | Redox and Electrochemical Cell 11

 U-Tube H2SO4: colorless Left tube: FeCl3(aq) + KSCN(aq) Redox reaction on the
H2SO4 2M solution until ± solution H2SO4+ K2Cr2O7: → Fe(SCN)3(aq) + left tube produce yellow
2cm from the top of the tube yellow 3KCl(aq) colour.
K2Cr2O7: orange Right tube: Redox reaction on the
+ 2 ml of
+ 2 ml of
concentrate solution H2SO4 + Left side: right tube produce red
K2Cr2O7 0,1 M (NH4)2Fe(SO4)2
2 ml of FeCL3 (NH4)2Fe(SO4)2 + H2SO4(aq)+ K2Cr2O7(aq) blood colour which have
on the top of the
left tube solution + KSCN
+5 drops of KSCN: colorless KSCN : red blood → HCrO4(aq) + same colour as
Compare KSCN 0,1 M on solution Comparison K2SO4(aq) + H2O(l) comparison solution.
the top of right
solution: FeCl+
Yellow solution Red Blood
(NH4)2Fe(SO4)2 : KSCN : red blood Right side:
Immersed carbon Immersed
light orange H2SO4(aq) + Fe(SO4)2(aq)
electrode 2 cm carbon
electrode 2 cm solution → Fe(SCN)3(aq) +
Color of solution 2K2SO4(aq) + H2(g)
2. GALVANIC CELL CuSO4 : blue CuSO4: light blue Anode : Galvanic cell by using
solution solution Zn(s) → Zn2+(aq) + 2e-
Beaker glass 1 Beaker glass 2 ZnSO4 and CuSO4
ZnSO4: colorless
15 ml of CuSO4 0.1M 25 ml of ZnSO4 0.1M solution ZnSO4: colorless Cathode : produce voltage 0,9 volt
- entered into beaker glass 100 ml - entered into beaker solution Cu2+(aq) + 2e- → Cu(s)
glass 100 ml KCl: colorless
- immerse the copper plat - immersed the zinc solution V1=90/250 x 2.5 Rex tot:
plate Zink: shine = 0.9 v Zn(s) + Cu2+(aq) →
- connected with salt bridge that white plate V2=225/250x1 Zn2+(aq) + Cu(s)
=0.9 v
made from rolled tissue paper and
Copper: shine V3=45/250x5 Ecell= 1.10 volt
immersed in KCl solution brown plate =0.9v
Voltage
Experiment Report | Redox and Electrochemical Cell 12
 3. KI: colorless Right(cathode): (A)2I-(aq) → I2(aq) + 2e- Electrolytic KI solution
ELECTROLYTIC CELL
solution colorless solution (C)2H2O(aq) + 2e- → produce yellow color on
-
CHCl3: colorless H2(g) + 2OH (aq) the anode and colorless
KI 0.25 M
solution Left(anode): Reaction on the cathode.
- entered into U-tube until 2 cm from
the top tube FeCl3: yellow yellow solution 2H2O(aq) + 2I-(aq) → Solution on the anode

- Immersed carbon electrode 2 cm in solution H2(g) + OH-(aq) produce bilayer reddish

Connected left carbon Connected right carbon
electrode with positive electrode with negative
of 6V electrode of 6V electrode
Yellow solution Colorless solution +
Bubbles
PP: colorless Anode+CHCl3: purple and yellow when
solution reddish purple I2(aq)+ 2CHCl3(aq) → 2 it added by CHCl3
layer on bottom CHI(aq)+3 Cl2 (g) Solution on the cathode
and yellow layer FeCl3(aq)+KI(aq)→I- changes to red blood
on top (aq)FeCl2(aq)+KCl(aq) after it added by pp and
FeCl3(aq)+3H2OCl(aq)→ FeCl3

2 ml result of Color 2 ml result of Cathode Fe(OH)2(s)+3 HCl(aq)

electrolysis from changing electrolysis from +phenolphthalein 3OH-(aq)+ FeCl3(aq)→
Anode cathode
+ FeCl3: red Fe(OH)3(aq)+3Cl-(aq)
- took result test tube - took into test
tube blood turbid no
- added by 1 ml of
precipitate
CHCl3 - added
phenolphthalein
Bilayer
reddish purple - added FeCl3
and yellow Red Blood

Experiment Report | Redox and Electrochemical Cell 13

IX. ANALYSIS

1. REDOX REACTION

In the first experiment is identificating redox reaction based on colour changing which
observed. There is two parts on first experiment, that is A and B experiment. On the
experiment A we use KI solution to identificate redox reaction. The first thing we have to
make standard of comparison solution by diluting 5 drops of I2 solution and then adding 2
drops of starch solution. Next, prepare 3 reaction tubes. On each of the test tube we are
adding 1 ml of KI 0,1 M solution and starch solution. In the tube I, we are adding 1 ml of
H2SO4 2M and 0,5 ml H2O2 3% solution. In the tube II, we are adding 1 ml H2SO4 2M
and 0,5 ml of FeCl3 0,1 M. In the tube III, are adding 2 drops of concentrate HNO3. The
reaction is:

Test tube 1: 2KI(aq) +H2SO4(aq) +H2O2(aq) → 2H2O(aq) + K2SO4(aq) + I2(s)

Test tube 2: 2KI(aq) +H2SO4(aq) +FeCl3(aq) → 2FeCl3(aq) + K2SO4(aq) + I2(aq) + HCl(aq)

Test tube 3: 2KI(aq) + 2HNO3(aq) → 2KNO3(aq) + I2(aq) + H2(g)

The standard of comparison solution changes colour from yellow to black bluish. Colour
of the solution on the tube I changes from colourless to purple. In the tube II colour of
solution changes from colourless to black yellowish. Meanwhile, in the tube III the colour
changes to black bluish which is similar to comparison solution.

On the experiment B. Firstly, we have to make standard of comparison solution by

adding 2 ml FeCl3solution on the test tube and then adding a few drops of KCNS 0,1 M.
Next, we are adding H2SO4 solution into U-tube which placed on the beaker glass until
±2 cm from the tip tube. After that, we are adding 2 ml of K2Cr2O7 on the left side of the
tube and adding 2 ml of saturated (NH4)2Fe(SO4)2 and 5 drops of KCNS 0,1 M on the
right side of the tube. Then, we immersing carbon electrode on both side of the tube until
it submerged ± 2 cm and then connecting both electrodes by wire. The reaction is:

Standard of comparison: FeCl3(aq) + KSCN(aq) → Fe(SCN)3(aq) + 3KCl(aq)

Experiment Report | Redox and Electrochemical Cell 14

 Left side: H2SO4(aq)+ K2Cr2O7(aq) → HCrO4(aq) + K2SO4(aq) + H2O(l)

Right side: H2SO4(aq) + Fe(SO4)2(aq) → Fe(SCN)3(aq) + 2K2SO4(aq) + H2(g)

The standard of comparison solution on the tube changes colour from yellow to red
blood. On the left side of the tube changes colour from colourless to orange after it
added by K2Cr2O7 and did not change after carbon electrode is immersed on it.
Meanwhile, solution on the right side of the tube changes colour from colourless to
orange (+) after it added by Fe(SO4)2 and changes to red blood after carbon electrode
is immersed in it, this colour changing is similar with the standard of comparison
solution.

2. GALVANIC CELL

The second experiment has purpose to determine electricity movement capacity of

galvanic cell. Firstly, we preparing 2 clean and dry beaker glass 100 ml. Next, we are
adding 15 ml CuSO4 0,1 M solution on the beaker glass I and 25 ml of ZnSO4 0,1 M
solution into beaker glass II. Then, immersed copper plat into beaker glass I and zinc
plate into beaker glass II. Connecting both plat with voltmeter. After that, we make
salt bridge from tissue which rolled and immersed in the KCl solution. The reaction is:

Anode: Zn(s) → Zn2+(aq) + 2e-

Cathode: Cu2+(aq) + 2e- → Cu(s)

Rex tot: Zn(s) + Cu2+(aq) → Zn2+(aq) + Cu(s)

The arrow of voltmeter moves to right. When use 2.5 volt as the smallest scale the
arrow point out number 90, when we use 1 volt as the smallest scale, the arrow point
out number 225 and when use 5 as the smallest scale, the arrow point out number 45.
Color of ZnSO4 solution did not change. Meanwhile, color of CuSO4 solution is fading
and become light blue.

Experiment Report | Redox and Electrochemical Cell 15

 3. ELECTROLYTIC CELL

The third experiment has purpose to examine the electrolysis of KI solution. Firstly,
we are adding KI 0,25 M solution on the U-tube which placed on the beaker glass until
± 2 cm from the tip tube. Then, immersing 2 carbon electrodes in both sides of the U-
tube until it immersed ± 2 cm. Next, connecting carbon electrode on the right side to
negative polar of the current source (adaptor 6 volt) and carbon electrode on the left
side to positive polar. After 5 minutes, the solution on the left side changes colour to
yellow and on the right side bubbles formed. The reaction is:

Anode: 2I-(aq) → I2(aq) + 2e-

Cathode: 2H2O(aq) + 2e- → H2(g) + 2OH-(aq)

Net reaction: 2H2O(aq) + 2I-(aq) → H2(g) + OH-(aq)

Next, break the current flow. Then, taking 2 ml of solution result of electrolysis on
cathode by pipette and entering to test tube, and then adding a few drops of
phenolphthalein and 2 ml of FeCl3 0,1 M solution. When it added by phenolphthalein
the color changes from colorless to soft pink and when it added by FeCl3 0,1 M the
color changes to red blood. The reaction is:

FeCl3(aq)+KI(aq)→I-(aq)FeCl2(aq)+KCl(aq)

FeCl3(aq)+3H2OCl(aq)→Fe(OH)2(s)+3 HCl(aq)

3OH-(aq)+ FeCl3(aq)→ Fe(OH)3(aq)+3Cl-(aq)

After that, taking 2 ml solution result of electrolysis on anode into another test tube,
then adding 1 ml of CHCl3 and shaking it. Bilayer reddish purple and yellow formed
and crystal are formed. The reaction is:

I2(aq)+ 2CHCl3(aq) → 2 CHI(aq)+3 Cl2 (g)

Experiment Report | Redox and Electrochemical Cell 16

X. EXPLANATION

1. REDOX REACTION

In the first experiment is identificating redox reaction based on colour changing which
observed. There is two parts on first experiment, that is A and B experiment. On the
experiment A we use KI solution to identificate redox reaction. The first thing we have to
make standard of comparison solution by diluting 5 drops of I2 solution and then adding 2
drops of starch solution. The purpose of making standard of comparison solution is to
proofing that I- have been oxidized become I2. Next, prepare 3 reaction tubes. On each of
the test tube we are adding 1 ml of KI 0,1 M solution and starch solution. In the tube I,
we are adding 1 ml of H2SO4 2M and 0,5 ml H2O2 3% solution. In the tube II, we are
adding 1 ml H2SO4 2M and 0,5 ml of FeCl3 0,1 M. In the tube III, are adding 2 drops of
concentrate HNO3. The reaction is:

Test tube 1: 2KI(aq) +H2SO4(aq) +H2O2(aq) → 2H2O(aq) + K2SO4(aq) + I2(s)

Test tube 2: 4 FeCl3 + 6 H2SO4 + 2 KI→4 FeSO4 + I2 + 12 HCl + 2 KSO4

Test tube 3: 2KI(aq) + 2HNO3(aq) → 2KNO3(aq) + I2(aq) + H2(g)

The I- on the comparison solution can be identificate by its yellow colour. After it added
by starch solution the colour changes to black bluish. The I- have been oxidized become
I2, it can be indicate because the free iodide forming black bluish on starch solution
(Svehla, 1997: 351). On the tube I, When potassium iodide and starch solution is added to
Hydrogen peroxide which was preserved by dilute sulphuric acid, forming Iodide slowly
and the solution little by little become dark blue, which eventually become darker:

H2O2+ 2H+ + 2I-→I2 + 2H2O (Svehla, 1997: 406)

In the tube II, with existence of sulphuric acid freeing chlor from chloride and regenerate
the iodide and colour of FeCl3 is yellow. So, the colour changes from colourless to black
yellowish. Meanwhile, in the tube III the colour changes to black bluish. The I- have been
oxidized become I2, it can be indicate because the free iodide forming black bluish on
starch solution which is similar to comparison solution.

Experiment Report | Redox and Electrochemical Cell 17

On the experiment B. Firstly, we have to make standard of comparison solution by
adding 2 ml FeCl3solution on the test tube and then adding a few drops of KCNS 0,1 M.
Next, we are adding H2SO4 solution into U-tube which placed on the beaker glass until
±2 cm from the tip tube. After that, we are adding 2 ml of K2Cr2O7 on the left side of the
tube and adding 2 ml of saturated (NH4)2Fe(SO4)2 and 5 drops of KCNS 0,1 M on the
right side of the tube. Then, we immersing carbon electrode on both side of the tube until
it submerged ± 2 cm and then connecting both electrodes by wire. The reaction is:

Standard of comparison: FeCl3(aq) + KSCN(aq) → Fe(SCN)3(aq) + 3KCl(aq)

Left side: H2SO4(aq)+ K2Cr2O7(aq) → HCrO4(aq) + K2SO4(aq) + H2O(l)

Right side: H2SO4(aq) + Fe(SO4)2(aq) → Fe(SCN)3(aq) + 2K2SO4(aq) + H2(g)

The standard of comparison solution on the tube changes colour from yellow to red
blood. Red blood colour is emerged because forming a complex:

3SCN- + Fe3+ Fe(SCN)3 (Svehla, 1997: 338)

On the left side of the tube changes colour from colourless to orange after it added by
K2Cr2O7 and did not change after carbon electrode is immersed on it. Potassium
dichromate produce orange colour on water. In the strong acid solution, dichromate ion is
reduced become chromium (III):

Cr2O72-+ 14H+ +6e-→ 2Cr3++7H2O (Svehla, 1997: 116)

Oxidation number of Cr changes from +6 to +3. The solution changes to light green from
Cr3+ ion.

Meanwhile, solution on the right side of the tube changes colour from colourless to
orange (+) after it added by Fe(SO4)2 and changes to red blood which is emerged because
forming a complex after carbon electrode is immersed in it, this colour changing is
similar with the standard of comparison solution.

Experiment Report | Redox and Electrochemical Cell 18

 2. GALVANIC CELL

The second experiment has purpose to determine electricity movement capacity of

galvanic cell. Firstly, we preparing 2 clean and dry beaker glass 100 ml. Next, we are
adding 15 ml CuSO4 0,1 M solution on the beaker glass I and 25 ml of ZnSO4 0,1 M
solution into beaker glass II. Then, immersed copper plat into beaker glass I and zinc
plate into beaker glass II. Connecting both plat with voltmeter. After that, we make salt
bridge from tissue which rolled and immersed in the KCl solution. The salt bridge
function is to neutralize electrons excessive on the solution. The reaction is:

Anode: Zn(s) → Zn2+(aq) + 2e-

Cathode: Cu2+(aq) + 2e- → Cu(s)

Rex tot: Zn(s) + Cu2+(aq) → Zn2+(aq) + Cu(s)

As a zinc atom provides the electrons, it becomes a positive ion and goes into aqueous
solution, decreasing the mass of the zinc electrode. On the copper side, the two
electrons received allow it to convert a copper ion from solution into an uncharged
copper atom which deposits on the copper electrode, increasing its mass. The two
reactions are typically written. The letters in parentheses are just reminders that the zinc
goes from a solid (s) into a water solution (aq) and vice versa for the copper. It is typical
in the language of electrochemistry to refer to these two processes as "half-reactions"
which occur at the two electrodes.

The zinc "half-reaction" is classified as oxidation since

it loses electrons. The terminal at which oxidation
occurs is called the "anode". The copper "half-
reaction" is classified as reduction since it gains
electrons. The terminal at which reduction occurs is
called the "cathode".

The zinc metal gives up 2 electrons and goes into aqueous solution. Electrons from Zinc
flowed through the wire and catch by Ca2+ ion which is stick on the copper plate and
makes the plate thicker and cause SO42- excessive. The K+ ion on the salt bridge absorb

Experiment Report | Redox and Electrochemical Cell 19

 the over SO42-. Meanwhile, on the anode the SO42- gather with Zinc plate, it makes Cl-
ion on the salt bridge move toward the anode.

An electric current flows from anode to the cathode because there is difference in
electrical potential energy between the electrodes. Zinc/copper cell under the standard
conditions, the calculated cell potential:

E˚cell = E˚Zn/Zn2+ +E˚Cu2+/Cu

= 0,76 V +0,34 V

= 1,10 V

Meanwhile, on our experiment the galvanic cell produce electrical potential 0,9 volt,
based on Nernst equation, it may affected by Zn2+ and Cu2+ concentration. Colour of
ZnSO4 solution did not change. Meanwhile, color of CuSO4 solution is fading and
become light blue.

3. ELECTROLYTIC CELL

The third experiment has purpose to examine the electrolysis of KI solution. Firstly, we
are adding KI 0,25 M solution on the U-tube which placed on the beaker glass until ± 2
cm from the tip tube. Then, immersing 2 carbon electrodes in both sides of the U-tube
until it immersed ± 2 cm. Next, connecting carbon electrode on the right side to negative
polar of the current source (adaptor 6 volt) and carbon electrode on the left side to
positive polar. The battery serves as an “electron pump” driving electrons to the anode,
where reduction occurs, and withdrawing electrons from the anode, where oxidation
occurs.

In this electrolytic cell, two separate half reactions occur at each electrode. The iodide
anion I- is oxidized to I2 at the anode. This is confirmed by the appearance of a yellow-
brown color in solution which is due to the formation of triiodide ions (I3-). This reaction
occurs as follows: I2 (aq) + I- (aq)→ I3- (aq)
At the cathode the reduction of hydrogen in water to H2 gas is confirmed by the evolution
of gas coupled with the observation of a pink color in solution, indicative of OH- in the

Experiment Report | Redox and Electrochemical Cell 20

presence of phenolphthalein indicator. At the anode is oxidized I-because its reduction
potential value is smaller when compared to H2O. So that the cathode is reduced H2O.
These two half-reactions and the overall redox reaction are shown below:
Anode: 2I-(aq) → I2(aq) + 2e-

Cathode: 2H2O(aq) + 2e- → H2(g) + 2OH-(aq)

Net reaction: 2H2O(aq) + 2I-(aq) → H2(g) + OH-(aq)+ I2(aq)

This process is a major iodide, hydroxide and hydrogen gas.

After 5 minutes, the solution on the left side changes colour to yellow and on the right
side bubbles formed. Next, break the current flow. Then, taking 2 ml of solution result of
electrolysis on cathode by pipette and entering to test tube, and then adding a few drops
of phenolphthalein and 2 ml of FeCl3 0,1 M solution. When it added by phenolphthalein
the colour changes from colourless to soft pink and when it added by FeCl3 0,1 M the
solution continued to be identified with the addition of FeCl3 and will form a precipitate
of iron (III) hydroxide brownish red indicating the presence of hydroxide ions at the
cathode so that it can be concluded the reducer is H2O produce H2 gas and OH-. The
reaction is:

FeCl3(aq)+KI(aq)→I-(aq)+FeCl2(aq)+KCl(aq)

FeCl3(aq)+3H2OCl(aq)→Fe(OH)3(s)+3 HCl(aq)

3OH-(aq)+ FeCl3(aq)→ Fe(OH)3(aq)+3Cl-(aq)

After that, taking 2 ml solution result of electrolysis on anode into another test tube, then
adding 1 ml of CHCl3 and shaking it. To identify the presence of I2, the addition of a
solution of CHCl3. CHCl3 is because the compound is non-polar and polar compounds I2
so in identification we will see two layers are formed between I2 and CHCl3 solution
because polar compounds dissolve in polar compounds, while also non-polar compounds
dissolve in non-polar compounds. Above the layer (first layer) is the solution of I2 and the
bottom layer is a solution of CHCl3, and this is because the density of I2 is smaller in

Experiment Report | Redox and Electrochemical Cell 21

 comparison with the density of CHCl3. Bilayer reddish purple and yellow formed and
crystal are formed. The reaction is:

I2(aq)+ 2CHCl3(aq) → 2 CHI(aq)+3 Cl2 (g)

XI. DISCUSSION
On the third experiment, when we add FeCl3 to cathode solution it should be forming
brown reddish precipitate of Iron (III) hydroxide which insoluble in overly reagents.
Fe3+ + 3OH-→Fe(OH)3 (Svehla, 1997: 261)
But, in our experiment precipitate is not formed. It because the connection to the battery
is unintentionally broken when we touched the wire.

XII. CONCLUSION
1. Redox reaction can be identified by color changing of the solution.

2. Electricity movement on the galvanic cell Each electrode attracts ions that are of the
opposite charge. Positively charged ions (cations) move towards the electron-providing
(negative) cathode, whereas negatively charged ions (anions) move towards the positive
anode. At the electrodes, electrons are absorbed or released by the atoms and ions. Those
atoms that gain or lose electrons to become charged ions pass into the electrolyte. Those
ions that gain or lose electrons to become uncharged atoms separate from the electrolyte.
The formation of uncharged atoms from ions is called discharging. The energy required
to cause the ions to migrate to the electrodes, and the energy to cause the change in ionic
state, is provided by the external source of electrical potential.

3. The electrolysis of KI solution is In this electrolytic cell, two separate half reactions
occur at each electrode. The iodide anion I- is oxidized to I2 at the anode. This is
confirmed by the appearance of a yellow-brown color in solution which is due to the
formation of triiodide ions (I3-). This reaction occurs as follows: I2 (aq) + I- (aq)→ I3- (aq)
At the cathode the reduction of hydrogen in water to H2 gas is confirmed by the evolution
of gas coupled. At the anode is oxidized I-because its reduction potential value is smaller
when compared to H2O. So that the cathode is reduced H2O.

Experiment Report | Redox and Electrochemical Cell 22

XIII. ANSWER OF THE QUESTION
1. At redox reaction there is not necessary source of current, meanwhile at electrolysis
there is necessary current, why? And explain the real function of current?
Answer :

Because electrolysis, occur in non-spontaneous redox reaction, so the energy required

to perform the reaction. Current function is as a source of energy that is required in the
electrolysis cell. The electrical energy required is direct current electrical energy. For
the process of electrolysis is necessary to the electrode, electrolyte solution, and a
source of direct current. In the electrolysis cell cathode is connected to the pole (-), and
the anode is connected to the pole (+) current source. When electric current is applied
to the electrolyte, the cation will undergo reduction by capturing electrons and anions
will undergo oxidation by removing electrons. While the redox reaction does not
require electric current because, he has reacted spontaneously, so it does not need
electric currents reacting.
2. What is the meaning with salt bridge? What the function and explain how to make the
salt bridge with tissue paper?
Answer :

Salt bridge is a bridge in which there are positive ions and negative ions.
The function of the salt bridge is to balance the ions in solution, which can maintain
neutrality, because the salt bridge containing positive ions and negative.
Method of making a salt bridge of tissue paper are the paper towel roll and drop of
with saline solution (KCl, NaCl, Na2SO4, etc). After that, place the tip of the tissue in
a beaker I and the other end take place in another beaker.

XIV. REFERENCESS
Anne Marie Helmenstine, Ph.D. 2009. Redox Reaction.(online).(
http://chemistry.about.com/od/stoichiometry/a/redoxreaction.htm), (March, 19th 2014,
8.00 p.m)

Experiment Report | Redox and Electrochemical Cell 23

Brady, James E. 1982. General Chemistry 3rd edition: Principles and Structures. New
York: John Wiley & Sons

Chang, Raymond. 1998.Chemistry:Sixth Edition.Mc.Graw-Hill.United of America

Noname.2013.Electrolytic Cell.(online).( http://en.wikipedia.org/wiki/Electrolytic_cell),

(March, 19th 2014, 8.20 p.m)

Noname.2013.Galvanic Cell.(online).( http://en.wikipedia.org/wiki/Galvanic_cell),

(March, 19th 2014, 8.20 p.m)

Svehla,G.1985.Vogel Buku Teks Analisis Oraganik Kualitatif Makro dan Semimikro.

Jakarta: Kaliman Media Pusaka

Experiment Report | Redox and Electrochemical Cell 24

ATTACHMENT

1. REDOX REACTION
A.

Left: KI solution (colorless) I2 solution I2 solution+ amyllum

Right: Amyllum (colorless) Yellow Black bluish (comparison)

KI+Amyllum KI+Amyllum KI+Amyllum

Colorless solution Colorless solution Colorless solution

Experiment Report | Redox and Electrochemical Cell 25

 KI+Amyllum KI+Amyllum KI+Amyllum
+H2SO4+H2O2 +H2SO4+FeCl3 +concentrated HNO3

Black bluish Black yellowish Black bluish

B.

H2SO4 2M solution Left: +K2Cr2O7 (yellow) Left: +K2Cr2O7 (yellow)

Colorless solution Right: +(NH4)2Fe(SO4)2 Right: +(NH4)2Fe(SO4)2

+KSCN (Orange) +KSCN (red blood)

Experiment Report | Redox and Electrochemical Cell 26

 Left: +K2Cr2O7 (yellow)

Right: +(NH4)2Fe(SO4)2 +KSCN (red blood)

Tube (comparison) : FeCl3+KSCN (red blood)

2. GALVANIC CELL

CuSO4 : blue solution, CuSO4: colorless solution

Connected to volt meter

Experiment Report | Redox and Electrochemical Cell 27

2. ELECTROLYTIC CELL

3.

KI 0,25 M Left: connect to (+) polar 2 ml solution from anode

(yellow)

Right: connect to(–) polar

Colorless Solution (bubbles) Yellow solution

2 ml solution from 2 ml solution from 2 ml solution 2 ml solution

anode +CHCl3 cathode cathode + cathode +
phenolphthalein phenolphthalein
Bilayer: yellow and Colorless +FeCl3 (red blood)
reddish purple Soft pink

Experiment Report | Redox and Electrochemical Cell 28