PRACTICAL 1

ELECTROLYSIS
Aim
To examine the quantitative relationships involved in electrolysis.

Learning Objectives
By the end the practical, you should be able to:
1. Set up a circuit for electrolysis
2. Write equations for the reactions at the electrodes
3. Calculate the number of moles of electrons transferred during electrolysis
4. Calculate the number of moles gained or lost at a given electrode

Introduction
When electricity is passed through an electrolyte, a chemical reaction occurs and products
are formed at the electrodes. According to Faraday’s First law of electrolysis, the mass of
products formed at an electrode is proportional to the quantity of electricity passed.

Quantity of electricity, Q (Coulombs) = Current, I (amperes) x Time, t (seconds)

In this practical, you will measure current flowing and time the electricity is allowed to
flow through the electrolyte. Once current and time are known, quantity of electricity can
be calculated.

Since 1 mole of electrons = 96500 Coulombs

 n moles = 96500n Coulombs

But Q = I x t
I t
 n =
96500
You will also measure the number of moles of copper gained by the cathode and the
number of moles of copper lost by the anode.

Materials
1. Power Supply
2. Rheostat
3. Milliammeter (100mA)
4. Balance
5. Stop watch
6. Emery paper
7. 2 Cu sheets (about 9cm x 2cm)
8. 4 electrical leads with crocodile
9. 250 m beaker
10. 0.5 M CuSO4
11. 0.1 M CH3COOH (Acetic acid)
12. Acetone

Procedure
Rheosta
t

12V
mA

CuSO4

Copper plates

Figure 1: Electrolysis Arrangement

1. Clean the copper plate using the emery paper. Wash with acetone.
2. Mark the two strips as anode and cathode respectively.
3. Weigh both copper strips separately and record the values with power supply
off.
 4. Connect the circuit as in figure 1 with the strip labelled anode to positive(red)
and the other to negative(black) terminal of power supply.
5. Pour Copper sulphate in the beaker to the level of washed copper plates.
6. Set the power supply to 12V and the rheostat to minimum resistance.
7. Switch on power supply and start the stop watch.
8. Record the current flowing.
9. Leave the power supply on for about 30 minutes observing what is happening
in the beaker. Ensure that current remains constant by adjusting the rheostat.
Record the exact time of electrolysis.

10. Carefully remove the copper anode, rinse it with acetic acid and bloat gently
with filter paper.

11. Rinse the anode with acetone, allowing to dry and weigh the anode. Record
new mass.

12. Repeat steps 11 and 12 with the cathode, but with great care because the copper
that has been plated onto the electrode will not be attached firmly onto the
strip.

Results
Time =____________________
Current =____________________
Mass of the copper anode after electrolysis =_______________
Mass of the copper anode before electrolysis =______________
Mass lost by anode during electrolysis = _________________

Mass of copper cathode after electrolysis = ___________________

Mass of copper cathode before electrolysis = __________________
Mass gained by cathode during electrolysis = _________________

Questions
1. Calculate the number of moles of copper gained by the cathode from the mass
change.
2. Calculate the number of moles of copper lost by the cathode from the mass
change.

3. Compare the answers in 1 and 2. Comment on your results.

4. From your observation write the half reaction that occurred at:
(i) Cathode
(ii) Anode

5. Calculate the number of moles of electrons transferred during electrolysis from

the quantity of electricity passed
 PRACTICAL 2

ELECTROCHEMICAL CELLS
Aim
To give practical illustrations of the theory of electrochemical cells

Learning Objectives
By the end of the practical, you should be able to:
(a) Construct an electrochemical cell
(b) Test the Nernst equation on variation of cell potential with concentration

Introduction
An electrochemical cell is device that produces electricity from a reaction of chemicals. It
is made up of two half cells that are joined by salt bridge.

Figure 1 shows an example of a simple electrochemical cell known as Daniel Cell. The
arrangement for the Daniel cell and the half reactions occurring in each half-cell are
shown in figure 1. Each half-cell is made up of a metal electrode in contact with a
solution of a salt of the same metal and connected by a salt bridge and external circuit.
The half reaction equations show that the metal is both an electrode and a reactant or
product.

Voltmeter
V

Salt bridge
Zn (s)
Cu (s)
Anode Reaction Cathode Reaction
Oxidation half reaction: Reduction half reaction:
Zn (s) 2+ -
Zn (aq) + 2 e Cu2+ (aq) + 2 e- Cu (s)

Zn2+ (aq) Cu2+ (aq)

Figure 1. A Daniel cell

By convention, the Daniel cell is represented by the cell diagram:

 Zn(s)  Zn(aq, 1 M)  Cu (aq), 1 M)  Cu(s).

The solid single and double lines represent phase boundaries and the salt bridge
respectively and the first named electrode is the anode (the cathode is on the right hand
side)

Table 1 below shows the parts of a general cell and explains the conventional shorthand
representation of an electrochemical cell using the Daniel cell as an example.

Table 1: Electrochemical cells & cell diagrams

LHS Salt RHS
ANODE HALF CELL Bridge CATHODE HALF CELL
GENERAL ANODE Reduced Oxidised Oxidise Reduce CATHODE

Electrically conducting

balance
medium for passage of
ions for charge
CELL form of form of d form d form electrode
Electrod species species species of at which
e at oxidised oxidised reduced species reduction
which during during during reduced occurs
oxidatio reaction reaction reaction during
n occurs (Rred) (Rox) (OXoc) reaction
(OXred)
DANIEL Zn (s) Zn2+ (aq) KCl Cu2+ Cu (s)
CELL (sat) (aq)

Cell Diagram of a general Cell: Anode  Rred  Rox Oxox  Oxred Cathode

Cell Diagram of a Daniel Cell: Zn (s)  Zn (aq, 1 M)  Cu (aq), 1 M)  Cu (s)

In this representation, Rred and Rox represent the reduced and oxidized form of the reducing
agent and Oxox and Oxred represent the oxidized and reduced form respectively of the
oxidizing agent.

An electrochemical reaction occurs only when a conductor of electrons, usually a metal

wire, which joins the two electrodes, connects the two cells. This creates an external circuit.
The electrons flow down the wire from the anode to the cathode, giving an electric
current. The electrons are driven through the circuit by the potential difference set up
between the two half-cells.

The value of the potential difference provides a measure of the tendency of zinc to give
electrons to the copper ions and the tendency of the copper ions to accept electrons from
the zinc metal. This potential difference is at a maximum when no current is flowing, and
is called the electromotive force (e.m.f) of the cell, Ecell. The value of Ecell depends on a
number of factors, but when the concentrations of zinc and copper ions are both 1.0 M
and the temperature is 298 K, Ecell is said to have its standard value, indicated by Eocell.
Zinc is both the anode, the electrode at which oxidation occurs, and a reactant. The zinc
metal is oxidized to Zn2+ (aq) ions during the electrochemical process. Thus zinc (Zn (s)) is
the reduced form of the reducing agent, the species being oxidized during the redox
reaction. Copper metal is the cathode and also a product, the oxidizing agent (the reduced
form of the species that is reduced in the reaction).
The salt bridge is essential to complete the electrical circuit as it provides an inert electrically
conducting medium to allow ions to flow between the two half cells to maintain electrical
neutrality. The bridge can be an inverted U tube containing an electrolyte e.g. KCl,
NH4NO3 or a filter paper saturated with KNO3.

In the final part of this practical, you will test the Nernst equation by investigating the
effect of concentration on cell concentration for the Daniel cell.

Pre-Laboratory Exercises

1. What do you understand by the term electrochemistry? Give at least three

applications of electrochemistry.

2. What is the link between electrochemistry, redox reactions and oxidation numbers?
3. What is the difference between galvanic and electrolytic cells?
4. State Faraday’s law.
5. Give a definition of the common electrical units. How are they related?
6. State the Nernst equation.

Materials
1. 1.0 M Zinc sulphate(aq),
2. two equal beakers,
3. 1.0 M Copper sulphate (aq),
4. 0.1M Copper sulphate(aq),
5. 0.01M Copper sulphate(aq),
6. 0.001 M Copper sulphate(aq)
7. salt bridge,
8. Zinc foil,
9. Copper foil,
10. Emery/fine sand paper,
11. Voltmeter,
12. 1.0 M iron (II) sulphate (aq),
13. iron foil,
Procedure

1. Construction Of Cells

(a) Construction of a zinc/copper cell (Daniel cell)

Set up a zinc/copper cell as shown in Figure 1. Put about 50 cm3 of 1.0 M Zinc
sulphate (aq) solution into the left-hand beaker and 50 cm3 1.0 M Copper sulphate
(aq) into the right-hand beaker as shown in the diagram. Connect the two beakers
containing the solution by the salt bridge provided. Clean the zinc and copper foils
carefully with emery paper. Predict the polarity of the electrodes. Dip the two
electrodes into their respective ionic solutions and connect them with pieces of wire
to the voltmeter. Measure the e.m.f. of the cell.

(b) Construction of a zinc/iron cell

Using a clean iron nail for the iron electrode and an acidified 1.0 M iron (II) sulphate
(aq) solution as an electrolyte, set up a zinc/iron using a similar arrangement to the
previous, with a Fe/Fe2+ half-cell instead of the copper one (Figure 1). Use a fresh
salt bridge to connect the half cells.

(c). Construction of iron/copper cell

Set up iron/copper cell using the Fe/Fe2+ and Cu/Cu2+ half-cells used in the previous
two experiments. Remember to use a fresh salt bridge. Measure the e.m.f. of the
cell.

2. Testing The Nernst Equation: Effect Of Concentration On Ecell

When current is drawn from a Daniel cell, the reactions occurring at each electrode
are:
Zn (s)  Zn2+ (aq) + 2e- Anode
Cu2+ (aq) + 2e-  Cu (s) Cathode
However, when the e.m.f. of the cell is being measured, no current is being drawn
and each electrode is in equilibrium.

Set up a Daniel cell as in the first experiment and measure the Ecell using the following
different concentrations of Cu2+ (aq) solutions: 1.0 M, 0.1 M, 0.01 M, 0.001 M.
Take a reading as soon as the circuit is completed.

Caution: Use a fresh salt bridge for each solution and clean the electrodes very well.

Questions
1. Why does a reaction only occur when an electron conductor connects the
electrodes?
 2. Suggest why the salt bridge should be made of an inert material and indicate the
flow of the ions during the reaction.
3. For each of the cells, write down the anode and cathode half reactions and the
overall equations for the reaction.
4. Compare your value for Ecell with the literature value of Eocell for each cell and
rationalize any differences.
5. Comment on the relative tendencies of zinc, iron and copper to lose electrons and
predict relative values of Eocell of the following cells zinc/copper, zinc/iron and
iron/copper.
6. For each of these cells, give with reasons the cathode and anode half-cells for the
spontaneous reactions.
7. State the Le Chatelier’s principle and use it to predict the changes, which occur if the
iron concentration in each equilibrium half reaction is reduced.
8. Predict the effect of decreasing the concentration of copper ions on the tendency
of the copper electrode to accept electrons from the zinc. Hence predict the effect
on Ecell of decreasing the concentration of copper ions. Show that your prediction
agrees with the Nernst equation.
9. Given a 10 m pipette, 100 m volumetric flask, 1.0 M Cu2+ solution and de-ionised
water, how would you prepare 0.1 M, 0.01 M and 0.001 M Cu2+ solutions?
10. Suggest why it is especially important to ensure that the electrodes are clean at the
lower concentrations.
11. Does you value of Ecell increase or decrease when the Cu2+ concentration decreases.
12. Use the Nernst equation to estimate predicted values of Ecell for each of the Cu2+
Concentrations (1.0 M, 0.1 M, 0.01 M, 0.001 M). State any assumptions you make.
Compare your predicted values with your measured values and comment on the
differences, if any.
13. Use the Nernst equation to predict if the relation between Ecell and Cu2+ concentration
is a linear one and show how you could obtain a linear plot of the form
y = mx + c. where y represents Ecell and x is some function of the concentration of
copper ions that gives a linear relation. Identify m and c in your equation. Plot y
against x for your values and comment.
14. Suggest how you could improve the accuracy and precision of your results.
 Practical 3

Complexometric Calcium Determination (Experiment)

Introduction
Many metal ions form slightly dissociated complex ions. The formation of these can serve
as the basis of accurate and convenient titrations for such metal ions. Such determinations
are referred to as complexometric titrations. The accuracy of these titrations is high and
they offer the possibility of determinations of metal ions at concentrations at the millimole
level. Many cations will form complexes in solution with a variety of substances that have
a pair of unshared electrons (e.g. on N, O, S atoms in the molecule) capable of satisfying
the coordination number of the metal. The metal ion acts as a Lewis acid (electron pair
acceptor) and the complexing agent is a Lewis base (electron pair donor). The number of
molecules of the complexing agent, called the ligand, will depend on the coordination
number of the metal and on the number of complexing groups on the ligand molecule.

Simple complexing agents such as ammonia are rarely used as titrating agents because a
sharp end point corresponding to a stoichiometric complex is generally difficult to achieve.
This is true since the stepwise formation constants are frequently close together and not
very large, and a single stoichiometric complex cannot be observed. Certain ligands that
have two or more complexing groups on the molecule, however, do form well-defined
complexes and can be used as titrating agents. One such reagent that is widely used is
ethylenediaminetetraacetic acid (EDTA).

An organic agent which has two or more groups capable of complexing with a metal ion
is called a chelating agent. The complex which is formed in this manner is called a chelate.
Titration with such a chelating agent is called a chelometric titration which is a particular
type of complexometric titration. A pair of unshared electrons capable of complexing with
a metal ion is located on each of the two nitrogen atoms and each of the four carboxyl
groups. Thus there are six complexing groups in EDTA. We represent EDTA by the symbol
H4Y, which recognizes the fact that it is a tetraprotic acid. The four hydrogens in the
formula refer to the four acidic hydrogens on the four carboxyl groups. It is the
unprotonated ligand Y4- that is responsible for the formation of complexes with metal ions.
The present analysis is concerned with the determination of Ca by the use of a
complexometric titration of the type that is described above. The titration is performed by
adding a standard solution of EDTA to the sample containing the Ca. The reaction that
takes place is the following:
Ca2+ + Y4- ⇌ CaY2-
Before the equivalence point, the Ca2+ concentration is nearly equal to the amount of
unchelated (unreacted) calcium since the dissociation of the chelate is slight. At the
equivalence point and beyond, pCa is determined from the dissociation of the chelate at
the given pH. The equivalence point is detected through the use of an indicator which is
itself a chelating agent. The specific indicator used is Eriochrome Black T. It contains three
ionizable protons and we will represent it by the formula H3In. In neutral or somewhat
basic solutions, it is a doubly dissociated ion, HIn2-, which is blue in color. Eriochrome Black
T cannot be used as an indicator for the titration of calcium with EDTA, since it forms too
weak a complex with calcium to give a sharp end point. Therefore, a solution containing
the magnesium complex of EDTA, MgY2-, is introduced into the titration mixture. Since
Ca2+ forms a more stable complex with EDTA than magnesium, the following reaction
occurs:
MgY2−+Ca2+⇌CaY2−+Mg2+
The magnesium that is released in this manner then reacts with the doubly ionized ion of
the Eriochrome Black T. The complex that is formed between magnesium and that ion is
red, hence at the start of the Ca titration the solution is red. This reaction can be written
as follows:

Mg 2  HIn2-  MgIn -  H
blue red

The solution is then titrated with a standard solution of EDTA. At the beginning of the
titration, the EDTA reacts with the remaining calcium ion that has not been complexed.
After all the calcium has reacted the next portion of EDTA reacts with the magnesium
complex which was formed earlier. The added EDTA competes favorably with the red
magnesium-indicator complex (MgIn-), to give MgY2- and HIn2- and thereby giving a blue
color at the end point.

MgIn -  H  Y 4 -  MgY 2  HIn 2-

red blue

EXPERIMENTAL

Preparation of a 0.0100 M EDTA Solution

Dry about 2 g of EDTA dihydrate, Na2H2Y2.2H2O, in a drying oven at 80C for one hour.
Then accurately weigh out about .95 g ± 0.lmg. Quantitatively transfer the EDTA into a
250 mL volumetric flask, add distilled water with mixing then dilute to the mark with
distilled water. Mix well by inverting and shaking the tightly stoppered flask. Label this
solution "Standard EDTA".

Preparation of the Mg-EDTA Complex Indicator

Mix 0.744 g of dried EDTA with 0.492 g of MgSO4 in 100 mL of distilled water. Divide
the solution into two 50 mL portions. To one portion add a few drops of phenolphthalein.
Dropwise, counting the drops, add sufficient 0.1 M NaOH solution to turn the solution
faintly pink. ONCE THE NUMBER OF DROPS OF NaOH HAS BEEN DETERMINED,
DISCARD THIS Solution. To the second 50mL portion add the same number of drops of
0.1 M NaOH solution as were added to the first portion, then dilute to about 95 mL with
distilled water. Add 2 mL of pH 10 buffer solution and add a few drops of Eriochrome
Black T indicator solution. At this stage there are two possibilities, the solution is either red
or blue. If the solution is red, Mg2+ is in excess. In that case add 0.0100 M EDTA
solution dropwise until the solution just turns blue. If the solution is originally blue then
EDTA is in excess and in that case add

0.01 M MgSO4 solution dropwise until the solution just turns red, then add 0.100 M EDTA
dropwise to just turn the solution blue again.

Preparation of the Powdered Milk Solution

Dry approximately 5 g of powdered milk at 80C for one hour in a drying-oven. Accurately
weigh about 3 g of dry milk into a 250 mL beaker and add approximately 100 mL of
distilled water. Stir to dissolve. Transfer quantitatively with repeated washings with
distilled water into a 250 mL volumetric flask. Let stand for a sufficient length of time, so
that all bubbles disperse. If foaming occurs, it can be suppressed by the addition of 1 or 2
drops of n-octanol. Then dilute to the calibration mark with distilled water. Then mix well
by stoppering the flask and then inverting and shaking it repeatedly.

Titration of Milk Solution

Pipet an exact 50 mL aliquot of the milk solution into a 250 mL Erlenmeyer flask. Add
about 2 mL of pH 10 buffer, 10 mL of Mg-EDTA Indicator solution and 3 drops of
Eriochrome Black T indicator. Titrate with the standard 0.0100 M EDTA solution to a color
change from red to blue. Titrate at least two more milk samples using the same procedure
as before.

Treatment of Data and Report

From your experimental data calculate the percentage of Ca in the powdered milk for each
aliquot that you titrated. Then calculate an average percentage.
On the report sheet provided report the following data:
1. Milk unknown number
2. Weight of milk sample used.
3. Volume of EDTA solution used for each samples.
4. Percentage of Ca for each sample.
5. The average percentage of Ca.
6. The average deviation from the mean for the percent Ca in the samples

Questions on Complexometric Calcium

1. What is the indicator used in this titration?
2. Why can Eriochrome Black T not be used directly as an indicator?
3. What is the color of the doubly ionized Eriochrome Black T indicator in slightly
basic solution?
4. What is the purpose of adding NaOH solution dropwise to the Mg-EDTA mixture?
5. Is it possible to use the sodium salt of EDTA as a primary standard?
6. At what pH is the Ca titration carried out?
7. What are the conditional constants for Mg2+ and Ca2+ at the pH at which the
titration is carried out?
 PRACTICAL 4

SPECTROPHOTOMETRIC DETERMINATION OF IRON IN A NATURAL

WATER SAMPLE
Aim
To determine the concentration of iron in water using a spectrophotometric method

Learning Objectives
By the end of this practical, you should be able to:
(a). Form a coloured complex which can absorb light
(b). Prepare standard solutions of different concentration ranges
(c). Read % transmittance of coloured solutions of different concentrations
(d). Convert % transmittance to absorbance
(e). construct a calibration curve for a given standard using the absorbance read
versus the corresponding concentrations
(f). Use calibration curves to work out the concentrations of the unknown solutions.

Introduction

Preparation of a calibration curve

Calibration curves play a major role in the determination of sample analytes. They are
prepared by measuring absorbance of a series of standard analyte solutions having known
concentrations, which are plotted against their concentrations.

Spectrophotometric determination of iron in water depends on measurement of

absorbance of its solution, which is directly related to colour intensity and is proportional
to the concentration of the iron responsible for the colour. Thus the intense red complex
that Fe (II) forms with 2, 2 bipyridine (bipy) or 1, 10 – phenanthroline is exploited in the
determination of iron concentrations in the range of parts per million. The reaction is given
as
3 bipy + Fe2+ Fe (bipy)32+ or

Fe2+ + 3 phen H+ Fe (phen)32+ + 3H+

The complex Fe (bipy)32+ or Fe (phen)32+ which forms rapidly is stable over the pH range
of 3 to 9 and a suitable reagent for this is sodium acetate, which acts as a buffering reagent.
There is need to prevent oxidation of Fe (II) to Fe (III) and hydroxylamine hydrochloride
(NH2OH.HCl) is used for this purpose.

The absorbance so used is obtained from the measured % transmittance which is then
converted to absorbance as;

A = -log (%T); where A = absorbance, T = transmittance.

Materials
Hydroxylamine hydrochloride (NH2OH.HCl)
2, 2 bipyridine,
1, 10 – phenanthroline
Sodium acetate
3 M Sulphuric acid
Spectronic –20 spectrophometer
Ammonium iron (II) sulphate – 6 – water (Fe(NH4)2(SO4)26H2O)
Cuvette
Balance measuring up to 0.001 g decimal point.
250 ml volumetric flasks
Deionised water
100 ml volumetric flasks
10 ml pipette
50 ml volumetric flask

Procedure

Preparation of Standard Iron solution

1. Weigh to the nearest 0.1 mg, enough FeSO4(NH4SO4.6H2O) to prepare
250 m of a solution 0.002 in Fe(II).
2. Transfer the weighed salt to a 250 ml volumetric flask, dissolve it in deionised
water, add 8 m of 3 M H2SO4, dilute to the mark with deionised water.
3. Pipette 10 m o of the solution above into a 100 m volumetric flask, add 2 m of
3 M H2SO4 and dilute to the mark. This is your standard solution.
4. Prepare a set of four 50 m volumetric flasks by pipetting 5, 10, 15, and 20 m
of the standard solution into each of the flasks.
5. To each flask add 1 ml hydroxylamine hydrochloride, 15 m bipyridine solution
or phenanthroline and 4 m of 10% sodium acetate solution. Dilute to the mark.
6. Prepare a blank by adding 0.4 ml (about 10 drops) of 3 M H2SO4 to another
 50 m volumetric flask.
7. Measure the absorption spectra using the cuvettes provided. Read the % T of
each of the four standard iron solutions starting with the blank each time. Start
with the least concentrated solution and finishing with the most concentrated.
8. Work out their absorbance and report them in the table below against their
concentration
%T
Absorbance
Concentration

9. Using the results above, plot absorbance versus concentration (this is your
calibration curve).

Using a calibration curve to determine the quantity of iron in drinking water

10. Transfer 10 m of the water sample collected from different sources to a 100 ml
volumetric flask. Treat the water exactly the same way as the standard solutions.

11. Measure the absorbance of the water with respect to the blank.

Questions
1. Calculate the concentration of your standard iron solution
2. Work out the concentration of Fe (II) in each of the four flasks
3. What do you understand by a blank?
4. If you had a water sample in which you were to determine the concentration of
Fe (II), what would be the concentration of Fe (II) if the absorbance of the
solution were 0.23?
5. Work out the concentration of the Fe (II) in the water sample using your
calibration curve.
 PRACTICAL 5
Title: ANALYSIS OF IRON TABLETS FOR THE PRESENCE AND LEVEL OF IRON

Aim
To study the variability of the oxidation numbers of the transition metal elements and will
make an attempt to find the actual % of iron (II) sulphate in the iron tablets.

Learning Objectives
By the end of the practical, you should be able to:
(a). Write the different oxidation numbers that iron and manganese can take
(b). Determine the iron (II) content in iron tablets by titration against potassium
permanganate (VII), KMnO4.

Materials
Volumetric flask (250 m )
Conical flask (250 m )
100 m volumetric flask
Burette and stand,
Pipette (25 m ),
Filter funnel,
Filter paper,
Wash bottle,
Distilled water,
Weighing balance
5 Iron tablets (ferrous sulphate),
1.0 M sulphuric acid
0.01 M potassium permanganate (VII)

Introduction
Iron is essential for the human body. Its Principle role is as a constitute of hemoglobin, the
oxygen carrier agent in the blood. Iron is also present in a number of enzymes and
coenzymes involved in redox processes in the body.
Healthy adult males need little iron in their diet, but some group in the population need
substantial amounts of iron in order to produce extra hemoglobin. Such people include
growing children, pregnant and menstruating women and individuals who have for
various reason lost considerable amount of blood. A satisfactory intake of iron can
normally be ensured by eating a suitable diet, because certain food-liver, kidney, egg yolk
and spinach are rich in iron. Nevertheless, it is sometimes necessary to supplement the iron
taken in the natural diet with iron tablet.
Iron tablets bought at the chemist usually contain iron (II) sulphate (ferrous sulphate), a
cheap soluble form of iron.

Procedure

Solution of the tablets

Weighing accurately five of the iron tablets provided then dissolved in about 100 m of
1.0 M sulphuric acid in a conical flask. This will probably require heating but don’t heat
more than necessary to dissolve the tablets.
The outer coating of the tablets will probably not dissolve. So the solution will need
filtering. Filter the mixture into a beaker but make sure you don’t lose any of the solution.
Wash out the conical flask with water and pour the washing through the filter. Finally pour
distilled water over the residues and collect these washings as well. Pour the filtrate into a
250 m volumetric flask. Wash out the beaker and add the washings to the volumetric
flask. Make up to the mark with distilled water.
Titration with potassium manganate (VII)

Pipette 25 m of the iron (II) solution in to a 250 m conical flask. Add 25 m of 1.0M
sulphuric acid and titrate with potassium manganate (VII) solution. Repeat until you get
concordant readings of the potassium manganate (VII) solution. Record your observations.

Observations
Volume of MnO4( 1st Run 2nd Run 3rd Run 4th Run
m )
Initial volume
Final Volume
Volume used

Precautions
1. Iron tablet must be properly hydrolyzed water for better result.

Questions
1. Write the oxidation number of Iron and manganese I iron (II) and MnO4
2. Why should the tablets not be heated more than necessary?
3. Why are the tablets dissolved in sulphuric acid instead of water?
4. How many moles of MnO4 were needed to react with 25 ml of Fe+2 solution?
5. How many moles of Fe+2 were there in all tablets of iron (II)?
6. What mass of a Fe+2 FeSO4, FeSO4H2O, was in one tablet?
7. What % of iron was there in one tablet of iron?
 PRACTICAL 6

Title: DETERMINATION OF THE FORMULA OF A COMPLEX ION

Aim
To investigate the stoichiometry of copper (II) / 1, 2 – diaminoethane complex.

Learning Objectives
By the end of this practical, you should be able to:
Use a colorimetric method to determine a formula of a complex ion

Introduction
Essentially the determination of the formula of a complex ion involves measurement of
the number of ligands complexing with one metal ion. This can be investigated by several
methods, the most common of which are:

a. Colorimetric methods requiring measurement of the colour intensity of the mixture

as the proportion of metal ion to ligand is varied.

b. Titration methods involving competitive complexing

The stoichiometry of a complex ion can be determined by colorimetry provided there is a

significant difference in colour between simple aqueous ions and the complex. When
aqueous Cu2+ ions react with 1,2–diaminoethane (H2NCH2CH2NH2), a deeply coloured
complex ion is formed. We can write an equation for this reaction as

Cu2+ (aq) + X H2NCH2CH2NH2 (aq) [Cu(H2NCH2CH2NH2)X]2+ (aq)

In order to determine the stoichiometry of the complex, we must first of all find the value
of X. This can be done using the method of continuous variation described below.

Materials
9 test tubes
CuSO4
1,2–diaminoethane (H2NCH2CH2NH2)
UV-VIS spectrophotometer
Procedure
1. Take nine test tubes and number them 1 to 9. Using these test tubes, make up
mixtures of 0.05 M CuSO4 and 0.05 M of 1,2–diaminoethane (H2NCH2CH2NH2)
with the compositions shown below.

1 2 3 4 5 6 7 8 9
Test tube number
Volume of 0.05 M CuSO4 (ml) 0.0 2.0 3.0 4.0 6.0 8.0 9.0 10.0 12.0
Volume of 0.05 M 1,2–diaminoethane 12.0 10.0 9.0 8.0 6.0 4.0 3.0 2.0 0.0

2. Shake each test tube to ensure that the solutions are thoroughly mixed. Notice that
each tube contains a total of 12 ml.

3. Follow the normal procedure to obtain zero absorbance (100% transmission) when
tube 1, containing only 1,2–diaminoethane solution, is placed in the colorimeter.
Now measure the absorbance of the other mixtures relative to this zero reading and
record the values in the table below.

1 2 3 4 5 6 7 8 9
Test tube number
Volume of 0.05 M CuSO4 (ml) 0.0 2.0 3.0 4.0 6.0 8.0 9.0 10.0 12.0
Volume of 0.05 M 1,2– 12.0 10.0 9.0 8.0 6.0 4.0 3.0 2.0 0.0
diamminoethane
Absorbance read

4. Plot a graph of absorbance (vertical axis) against the volume of 0.05 M CuSO4 from
left to right and, on the same horizontal scale, the volume of 0.05 M 1,2–
diaminoethane solution reading from right to left.

Questions

1. What is the colour of the copper (II) / 1, 2 – diaminoethane complex?

2. What are the volumes of the two solutions which on mixing give the same
maximum colour intensity?

3. In what molar proportions do Cu2+ ions and (H2NCH2CH2NH2) react to form the
complex?

4. Write an equation for the formation of the complex

5. Draw the structural formula you would predict for the complex ion and relate this
structure to that of [Cu(NH3)4]2+.
 PRACTICAL 7

COMPETITION FOR METAL CATION BETWEEN LIGANDS IN

COMPLEXING REACTIONS
Aim
To compare the relative strengths of different ligands for the metal cation Fe3+.

Learning Objectives
By the end of this practical, you should be able to:
(a). Carry out complexing displacement reactions
(b). Arrange ligands in order of increasing strength for Fe3+
(c). Determine experimentally the position of a ligand in the displacement series for
a given metal
(d). Predict whether or not displacement reaction would occur if a ligand were
added to a solution of a complex.

Introduction
A complex ion is an ion in which the central metal cation is bonded with a number of
anions or neutral molecules. The anion and molecules bound to the central metal cation
in a complex are called ligands. An example of a complex ion is hydrated copper ion, [Cu
(H2O)4]2+. The structure of the ion is shown in Figure 1.

H H

H O O H

Cu2+

H O O H

H H
Figure 1: The structure of a hydrated copper ion complex,
[Cu(H2O)4]2+.

A given metal cation forms complexes with different ligands. The strength of the
coordinate bonds between the cation and the ligand is different for different ligands. In
complexing reactions ligands, which form weaker bonds with the cations, are readily
displaced from the complex by those ligands, which form stronger bonds with the cation.
Since complexing reactions can easily be detected by observing colour changes when a
complex has been formed. In this experiment you will study some displacement reactions
of ligands from Fe3+ ion.

Materials
8 Test tubes in a rack,
The following solutions in dropper bottles:
1. 0.1 M Na2 (C2O4) solution of a 1.0 litre volume
2. 0.1 M EDTA (disodium salt) (16.8 g [CH2N(CH2COOH)CH2COONa]2 in 0.5 dm3)
solution
3. 0.1 M ammonia solution of a 1 litre volume
4. 0.1 M iron III Chloride (8.1g FeCl3 in 0.5 dm3 solution

Procedure
Follow the instructions below carefully. Write down your observations in the space
opposite each step and identify the ligand before moving on to the next step.

Instructions Observations Formula of Ligands

present

Place 15 drops of FeCl3

solution in a test tube.
Note the colour of the
solution.

Add ammonia to the test

tube until there is no
further change

Take 12 drops of the

mixture and place in a
clean test tube. Add to it a
solution of EDTA drop by
drop until there is no
further change

Questions
1. What do you understand by the term ligand?
2. What must a ligand posses in order to coordinate with the metal cation?

3. How is a coordinate bond formed?

4. From your results write the ligands EDTA, water and ammonia in order of increasing
strength of co-ordination with Fe3+

5. Design and carry out an experiment to find the position of the ligand ethanedioate
(C2O42-) in the series you have compiled.

6. Summarise the features of transition metal elements that can be learnt from this
practical.
 PRACTICAL 8

DETERMINATION OF THE CONCENTRATION OF CHLORIDE IONS

IN THE RIVER WATER

Aim
To determine the concentration of the chloride ions (Cl- ) in river water.

Learning Objective
By the end of the practical you should be able to:
Analyze chloride ions in drinking water

Chemical Equation:

Ag+ (aq) + Cl- (aq)  AgCl (s)

2Ag+ (aq) + CrO-2 (aq)  Ag2CrO4 (s)

Materials
Burette,
Burette stand,
Pipette (10 cm3),
4 conical flasks, (100 cm3)
Potassium Chromate (VI) solution,
0.05 M AgNO3
River water

Introduction
River water contains a certain amount of dissolved salts though the amount varies
accordingly to locality. Many different ions are present in river water the commonest
cation is Na+ while the commonest anion is Cl-. The method used is the standard one for
determining the concentration of chloride ions titration with silver nitrate solution of
known concentration. Silver ions form insoluble silver chloride when added to a solution
containing chloride ions.
By adding silver ions until silver chloride is no longer precipitated the amount of chloride
ions in a solution can be found.
Potassium chromate (VI) is used to indicate the end point of the titration- The point at
which all chloride ions have been precipitated, see chemical equations.

Procedure
In this titration, you will use 0.05M AgNO3 as a titrant. Pipette 10 cm3 of river water into
a 100ml volumetric flask and dilute to the mark with distilled water. Pipette 20ml of the
diluted river water into a conical flask and add about 10 drops potassium chloride (VI)
indicator. Rinse a burette with silver nitrate solution, then fill it with the solution. Titrate
the river water in the conical flask against the silver nitrate solution from the burette until
a reddish tinge colour just begins to appear.

Repeat the titration 4 more times and record the volumes of the titrant used.

Observations
Run 1st Run 2nd Run 3rd Run 4th Run 5th Run
Initial volume of 0.05M
AgNO3( m )
Final Volume of 0.05M
AgNO3( m )
Volume of 0.05M
AgNO3 used( m )

Precautions: AgNO3 is very corrosive avoid to contact with skin.

Questions
1. Find the average volume of AgNO3 used.
2. How many moles of silver ions are there in this volume of 0.05M AgNO3?
3. How many moles of chloride ions must there have been in the 10ml of river water
in the conical flask?

4. How many moles of chloride ions must have been in 1 dm3 of the original undiluted
water?

5. What is the concentration in gdm3, of the chloride ions in this sample of river water?

6. What are the possible sources of chloride ions observed in the river water?
7. Mention three biological roles that chloride ions play