_____________________________

Laboratory Manual
DMK 10023
BACIS PHYSICAL CHEMISTRY
_____________________________

NAME :
REGISTRATION NO. :
CLASS :
SESSION :
SESSION :

DIPLOMA IN CHEMICAL TECHNOLOGY (OIL & FAT)

DEPARTMENT OF CHEMICAL AND FOOD TECHNOLOGY
 CONTENTS

PRACTICAL TOPIC PAGE

General Laboratory Rules 3

Format & Marking Scheme of Laboratory Report 4

1 Separating the Components of a Mixture 5

2 Determination of the Formula of a Hydrate 7

3 Calculation of Concentration and Preparation of Solutions 9

4 Acid-base Titration 15

5 Determination of the Molarity of a given Sodium 17

Carbonate solution

6 Investigate the Degree of Ionisation of Ethanoic Acid in 19

aqueous solution

7 Preparetion of Buffer Solution 22

8 Investigate the effect of Catalyst and Temperature on Rate 25

of Reaction between Oxalic acid (Ethanedioic acid) and
Potassium manganate(VII)

9 Investigate Reversible Reactions and the Effectsof 27

Temperature and Acidity on Chemical Equilibrium

2
 GENERAL LABORATORY RULES

1. Students are NOT ALLOWED to enter the laboratory without the supervision of the laboratory
attendant or lecturer.

2. On entering the laboratory, before beginning any laboratory activity, all students are required
to wear their laboratory coats (buttoned up completely).

3. Students are required to wear shoes in the laboratory. Sandals, slippers and other such
footwear are prohibited in the laboratory.

4. Do not run, joke or banter in the laboratory. Do not carry out any activity that may endanger
self or friend.

5. Long sleeved clothing should be worn neatly buttoned or with sleeves rolled up to the elbows.

6. Female students with long hair, who do not wear head scarves must have their hair tied up.

7. Experiments can be started upon receiving instructions from the lecturer or laboratory
assistant. Students should not begin if still unclear or doubtful about the experimental
procedure.

8. Concentrate on what you are doing, when handling chemicals or laboratory equipment.
Follow ALL prescribed steps carefully, including safety procedures to prevent accidents.

9. Do not light a Bunsen burner if there is inflammable material nearby.

10. Unfinished or leftover chemical sand samples should be kept in a properly prepared container
for recycling or disposal.

11. After use, all equipment or glassware must be cleaned and returned to its proper place. Do
not leave dirty apparatus in the sink.

12. Report to the lecturer or laboratory assistant there is any breakage of glass equipment or
apparatus. Do not throw any broken glass into the sink.

13. Wash hands and any other part of the body that have been exposed to poisonous or dangerous
chemicals, with soap and plenty of water, especially if any itchiness is felt.

14. Before leaving the laboratory make sure all equipment, lights, air conditioning, water taps and
gas taps are turned or switched off. Wash your hands thoroughly with soap and water before
leaving the laboratory.

15. Students are not to eat and drink in the laboratory. Laboratory apparatus are not to be used
as food containers.

16. In the event of fire or other emergency, act calmly and do not rush for the laboratory exits.

17. Do not enter the laboratory to conduct any experiment if you are not feeling well. Ask the
lecturer’s permission to be exempted from the practical session and take arest.

3
 FORMAT & MARKING SCHEME OF
LABORATORY REPORT

Each laboratory report must be handed in latest by one week after the day the practical session is
held. The report should contain the following:

Front Page
A. Student’s identity
Name, Registration No., Class and names of group members.

B. Details of Practical
Practical No., date on which it is carried out and actual date of report submission.

Inside the Report

C. Practical No., Title and Objective(s)(5marks)

D. Introduction(10marks)
This section explains the theoretical and conceptual aspects of the practical. You are NOT
allowed to copy from the explanation given in the practical manual. If you do that, 2 marks
will be deducted from your mark for the whole report.

E. Apparatus, chemicals and samples (5 marks)

This section lists all the apparatus, reagents and samples used in the practical.

F. Method (5 marks)
This section explains the steps followed in the practical. All the steps should be shown in the
form of an organisational chart, in the active voice.

G. Results (30marks)
All results and observations are to be recorded in this part of the report. The results should
be presented in the form of tables which are appropriate to the need of the particular
practical.

H. Discussion (30marks)
This is a very important section. You have to refer to other texts before you can write it. This
is where you discuss the observations and results that you have obtained. Were you successful
in achieving your stated objective(s) or not? Are your results in agreement with the
theoretical basis of the practical? If not you need to suggest plausible reasons why not. Were
there mistakes in methodology made and resulting experimental errors caused? If so, state
the corrective measures that should have been taken. If the results are in full agreement with
their theoretical basis, you should explain the mechanisms or how the results were derived.
This means that you must prove your results theoretically.

I. Conclusion (10marks)
This section should be concise. It shows the results obtained based on the stated
objective(s) of the practical.

J. References (5marks)
Record all the reference materials that you have used in writing the report here, in the
recommended format.

K. Questions (Marks given here are included in the marks for discussion.
If questions are given, answer them here.

4
 PRACTICAL 1

1.0 AIM : SEPARATING THE COMPONENTS OF A MIXTURE

2.0 OBJECTIVES

At the end of the session, students should be able to:

1. Use the correct techniques of physical separation such as heating, filtration and
distillation
2. Separate the components of a mixture of salt and sand, using the abovementioned
techniques.
3. Determine the percentage of salt in the given mixture of salt and sand.

3.0 THEORY

A mixture is a physical combination of two or more different components. Mixtures are

different from compounds because the formation of a compound involves a combination of
elements through a chemical process.The components of a mixture can be separated using
physical processes such as heating, filtration and distillation. Heating is carried out to dissolve
one of the components in a suitable solvent. Filtration is then carried out to remove the other
component which is not dissolved. Recrystallisation then serves to recover the dissolved
component.

4.0 MATERIALS AND SAMPLES

Materials : Distilled water

Sample : A mixture of sand and salt

5.0 APPARATUS
Digital balance, 150 ml beaker, retort stand and clamp, filter funnel and paper, tripod stand,
wire gauze and Bunsen burner.

6.0 PROCEDURE

A. Heating

1. Weigh about 10 gof the given mixture in a 250 ml beaker (label it A).
2. Add about 50 ml distilled water to the mixture in the beaker and stir to
dissolve the salt.
3. Heat the beaker on the tripod stand until all the salt is dissolved.

B. Filtration

1. Fold the filter paper into quarters and put it in the filter funnel.
2. Label a 250 ml beaker B and weigh it (empty).

5
 3. Pour the hot mixture into the filter funnel and collect the filtrate in
beaker B.

C. Recrystallisation
1. Heat the filtrate in beaker B to evaporate all the water.
2. Weigh the beaker and contents.
3. Examine the crystals obtained and take note of their appearance and
texture.

7.0 RESULTS

Table 4.0 : Calculating the mass of salt after recrystallisation

Mass (g)

Mass of empty beaker A (x)

Mass of beaker A and mixture (y)

Mass of mixture (y – x)

Mass of empty beaker B (a)

Mass of beaker B + Mass of salt after recrystallisation (b)

Mass of salt (b - a)

Percentage salt content= Mass of salt___ x 100% = (b – a) X 100%

Mass of mixture (y – x)

= ………………………%

Table 5.0 : Appearance of salt crystals formed

Colour Texture (feel with hand)

6
 PRACTICAL 2

1.0 AIM: DETERMINATION OF THE FORMULA OF A HYDRATE

2.0 OBJECTIVES

At the end of the session, students should be able to;

1. Determine the percentage by mass of water in a hydrated salt

2. Establish the formula of a hydrated salt

3.0 THEORY

Many salts occurring in nature or purchased are hydrated; that is, a number of water
molecules are chemically bound to the ions of the salt in its crystalline structure. These water
molecules are referred to as waters of crystallisation.

The number of moles of water crystallization per mole of salt is usually a constant. For
example, hydrated iron (III) chloride has the formula of FeCl3.6H2O. 6 moles of water are found
in each mole of the hydrated salt.

For some salts, the water molecules are so loosely bound to the ions that heating the salts will
drive out the water, forming the anhydrous salts. When blue copper(II) sulphate
pentahydrate is heated gently, the white anhydrous salt, copper sulphate, is formed, as shown
in the equation below:

CuSO4.5H2O CuSO4 + 5H2O

In this experiment, the percent by mass of water in a hydrated salt is determined. The
formula of the hydrated salt can then be found. The sample is first weighed and then heated
to drive off the water molecules. The mass of remaining sample is measured again. Cycles
of heating and measuring of the sample’s mass are continued until the mass is constant.

4.0 MATERIALS DAN SAMPLES

Samples : Hydrated magnesium sulphate (MgSO4.xH2O)

5.0 APPARATUS
Crucible with lid, clay triangle, tongs, asbestos sheet and digital balance.

6.0 PROCEDURE

1. Obtain a clean crucible and lid. Support them on a clay triangle and heat
intensely for 5 minutes. Let the crucible and lid cool to room temperature on
the clay triangle.

2. Determine the mass (+ 0.001g) of the cooled crucible and lid and record. Handle
the crucible and lid with the crucible tongs, not your fingers – oil from the
7
 fingers can contaminate the crucible and lid.

3. Add about 3g of the hydrated magnesium sulphate provided to the crucible.

Weigh and record immediately.

4. Return the crucible with sample to the clay triangle. Set the lid just off the lip of
the crucible to allow the water to escape on heating.

5. Heat the sample slowly, then gradually intensify the heat. Do not allow the
crucible to become red hot. Maintain the high temperature for 10 minutes.

6. Close the crucible and cool to room temperature. Weigh the crucible, lid and
anhydrous salt using the same balance.

7. To make sure all the water has been removed, reheat the sample for 2 minutes.
Weigh again after cooling to room temperature.
If this second weighing gives a reading that is different by more than + 0.01g
from the previous reading, repeat step 7.

11. RESULTS

Mass of crucible and lid, a

Mass of crucible and lid with hydrated magnesium sulphate, b

Mass of hydrated magnesium sulphate, c (b-a)

Mass of crucible and lid with anhydrous salt, d

Mass of anhydrous salt, e (d-a)
Mass of water (H2O), c-e

Based details on the table, calculate the mole of H2O.

8
 PRACTICAL 3

1.0 AIM : CALCULATION OF CONCENTRATION AND PREPARATION OF SOLUTIONS

2.0 OBJECTIVES

At the end of the session, students should be able to :

1. Calculate the quantity of chemical substance either solid or liquid required to
prepare a solution.
2. Prepare solution of a known concentration using a solid chemical substance or
liquid.
3. Calculate concentration of a solution in molarity, normality and percentage (%)

3.0 THEORY

Solution is a mixture of a solute and a solvent where the quantity of the solvent is usually
more than quantity of the solute in a mixture.

Concentration is defined as the amount of solute in a certain volume of a solution. It can be

expressed as:

(a) molar concentration or molarity (M)

= number of moles of solute (mol) found in 1litre (l or dm3) of solution.

Molarity = Number of moles of solute (mol)

Volume of solution (l)

RMM H2SO4 = 98.08 g/mol

= 0.5 mol
1l
Mass = 49.04 g
= 0.5 M

(b) normality (N)

No. of mole = mass = 49.04 g = 0.5 mol
= number of equivalent weights of a solute in 1 liter(l)
RMM of solution
98.08 g/mol

One normal is one equivalent weight of a solute dissolved in 1 litre of solution

N= number of equivalent weights of solute

volume of solution

1 equivalent weight= __RMM _

Valence

9
 For ionic compounds the valence can be found from
the number of cations or anions in the formula of the
compound, whichever is higher.

Example: H2SO4
Cation Anion
H+ SO42-
No. of H+ :2 No. of SO42- :1

Example 1
Calculate the normality of LiOH solution that contains 24g LiOH in 1 of solution

RMM LiOH = (7+16+1) g/mol [ LiOH → Li+ + OH- ]:Valence = 1

1 equivalent weight = RMM = 24 = 24 g

Valence 1

Number of equivalent weights in 24 g LiOH = 24 g = 1

24 g

normality(N) = number of equivalent weights

volume of solution

= 1 = 1N
1

Example 2
What is the normality of sulphuric acid (H2SO4) solution obtained by dissolving 0.98g in 2L of
solution?

RMM of H2SO4 = (2[1] +32+ 4[16]) =98

[H2SO4→2H+ + SO42-] This means valence = 2

Equivalent weight = 98 = 49
2
No. of equivalent weights in 0.98g =0.98 = 0.02
49

Normality (N) = Number of Equivalent weight = 0.02

Volume of solution 2L

= 0.01N

Concentration can be expressed in physical units such as :

A. Weight percentage (% w/w)

= percentage of quantity of solute (in weight unit ) in a solution(weight unit)

10
 % w/w = mass of solute x 100
mass of solution

• mass of solution = mass of solute + mass of solvent

• mass of solution can also be determined using the relationship between

volume of solution and density.

• To change volume to mass:

mass of solution = volume of solution xdensity of solution

Example : Calculate percentage in weight for a solution prepared by dissolving 10 g

calcium nitrate in 650 g water.

% w/w = mass of calcium nitrate x 100

mass of solution

= 10 g x 100 = 1.5 %
10 + 650

Remember : Volume of solution is NOT same as volume of solvent.

B. Percentage of weight per volume (% w/v)

= percentage of quantity of solute (in weight unit) in a volume of solution (volume

unit)

% w/v = mass of solute x 100

volume solution

Example :Concentration of aqueous calcium nitrate is 25 % w/w. If the density of the

solution is 1.2 g/cm3, what is the concentration of solution in % w/v?

% w/w = mass calcium nitrate x 100 = 25 %

mass of solution

density of solution = mass solution = 1.2 g/cm3

volume of solution

If the mass of solution is 100 g, then

mass of calcium nitrate = 25 x mass of solution = 25 x 100 = 25g

100 100

Volume of solution = mass solution = 100 = 83. 3 cm3

density of solution 1.2

% w/v = mass of calcium nitrate x 100 = 25 x 100 = 30 %

volume of solution 83.3

11
 C. Percentage of volume per volume (% v/v)
= percentage of quantity of solute (volume unit) in a volume of solution (volume
unit)

% v/v = volume of solute x 100

volume of solution

volume of solution = volume of solute + volume of solvent

Example:Calculate percentage by volume for a solution prepared by dissolving 25 cm3

ethanol in 250 cm3 water.

% v/v = volume of ethanol x 100

volume of solution

= 25 x 100 = 9.1 %
25 +250

D. Parts per Million (PPM)

1 ppm is 1 part in 1 million (100000).

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 (𝑔)

𝑝𝑝𝑚 = × 1000000
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 (𝑔)

* Concentration measured in mg/L is equivalent to ppm.

Example:You add 11 mg of sulfuric acid to 2,000 grams of water. What is the resulting
concentration of sulphuric acid, in ppm?

11
11 mg = g = 0.011 g
1000
Concentration of sulphuric acid = 0.011g × 1000000 = 5.5 ppm
(2000 + 0.011) g

A chemical solution can be prepared by using a solute that is either in the form of a solid or a liquid.

A. Preparation of solutions of solid solutes.

A solution can be made using a solid solute by direct weighing. The amount of solute required must
first be calculated, using the formula:

Mass of Volume of solution to Concentration of solution Relative Molecular

= X X
solute(g) be prepared (dm3) to be prepared (M) Mass (RMM)

Note : 1 dm3≡ 1 litre≡ 1000 ml≡ 1000 cm3

Example

Prepare 1dm3 of 0.5M sodium thiosulphate solution. (RMM of sodium thiosulphate is 158.)

12
 Step 1 Calculate the amount of solute required

Mass of sodium thiosulphate required = 1 dm3 x 0.5 M x158

= 74 g

Step 2 Prepare the solution

Weigh 74 g solid sodium thiosulphate in a beaker.Dissolve in a little distilled water

and transfer completely to a clean 1 dm3 volumetric flask. Make up to 1 dm3
solution by carefully adding distilled water until the level of solution exactly reaches
the calibration mark on the flask. Close the flask, shake thoroughly and label the
flask clearly.

B. Preparation of dilute solutions from liquid solutes (usually supplied as concentrated

solutions).

Most acid and alkali such as sulfuric acid, nitric acid, hydrochloric acid, methanoic acid, ethanoic acid,
ammonium hydroxide and other organic substances such as formalin and ethanol do not exist in solid
state but in concentrated solution. Dilute solutions of such substances can be prepared by measuring
the volume of the concentrated solution, and not by weighing the solution. Use the following formula
to prepare a dilute solution from the concentrated solution.

Volume Mass of 1 mole of substance (g) Volume of Molarity of

of = specific gravity X % of concentrated X solutionrequired X solution
concentrated of concentrated solution (dm3) required (M)
solution solution(S.G) 100
needed (cm3)

Note : 1 dm3 ≡ 1 L≡ 1000 ml ≡ 1000 cm3

Example
A bottle of concentrated sulphuric acidcarries a label with the following information :

M.W ( relative molecular mass ) = 98

S.G ( specific gravity ) = 1.84
Concentration = 97%

From the acid provided, prepare 500cm3 of 2M sulphuric acid solution.

Step 1 Calculate the amount of solute required

Volume of (cm3) = 98 x 1 x2 cm3

concentrated acid 1.84 x 97% 2
required

98 x 0.5x 2
= 1.84 x 97/100 cm3 = 54.9cm3

13
 Step 2 Prepare the solution

Prepare about 100 cm3 distilled water in a clean beaker. Using a pipette, measure54.9 cm3
concentrated sulphuric acid and release slowlywhile stirring, into the distilled water. Transfer
all the solution to a clean 500 cm3 volumetric flask. Add distilled water to reach the calibration
mark exactly, making1dm3 solution. Close the flask, shake thoroughly and label it clearly.

CAUTION :
When diluting concentrated acid, add concentrated acid slowly to distilled water while
stirring. DO NOT add water to concentrated sulphuric acid; spattering of the acid will occur
due to sudden heat buildup.

The following are several examples of concentrated acids used in the chemistry laboratory :

M.W. S.G. Concentration

Concentrated sulphuric acid. 98 1.84 97%
Concentrated hydrochloric acid. 36.46 1.19 37%
Concentrated nitric acid. 63 1.42 72%
Concentrated ethanoic acid. 60 1.048 99.5%
Concentrated ammonium 17 0.91 25%
hydroxide
Formaldehyde 30 1.075 37%

H Cl
M = 36.46 g/mol Fuming Hydrochloric acid 37 %
1l = 1.19 kg

4.0 MATERIALS AND SAMPLES

4.1 Concentrated sulphuric acid (compound B)

4.2 Sodium chloride (compound A)
4.3 Distilled water

5.0 APPARATUS

5.1 100 cm3and 250 cm3 beakers

5.2dropper
5.3graduated pipettes and filler
5.4 spatula

6.0 PROCEDURE
A. Refering to the labels on the reagent bottles, write down the appropriate
information on compounds A, B and C (student’s choice) in the table provided in
Section G.

B. Prepare solutions of A and B following the specifications stated in the tables in

Section F.

14
 PRACTICAL 4

1.0 AIM : ACID-BASE TITRATION

2.0 OBJECTIVES

At the end of the session, students should be able to:

2.1 Describe a chemical reaction using chemical symbol for the reactants and products
2.2 Calculate the molarity of solution using titration method
2.3 Calculate the molecular mass of an element using titration results

3.0 THEORY

Acid-base titrations involve neutralization reactions between acids and bases to form salts and
water. Examine the neutralization reaction between acid A and base B shown below:

aA + bB salt + water

stoichiometry coefficients

The quantitative relationship between acid A and base B is:

MA VA = a
Stoichiometry ratio
MB VB b

MA , VA and MB , VB are molarity and volume for acid and base respectively. By using that relationship,
the molarity acid and base can be determined.

Example: In a titration, 16 cm3 aqueous NaOH solution was required to neutralize 20 cm3 H2SO4 with
a concentration of 0.25 M. Calculate the molarity of the NaOH.

H2SO4 + 2NaOH → Na2SO4 + 2H2O

(acid) (base) (salt) (water)

mole ratio of acid to base is 1:2

this can be expressed as

number of moles of acid = 1

number of moles of base 2

MA VA = a
MB VBb

0.25 M x 20 cm3 = 1
MB x 16 cm32

15
 MB = 0.625 M
= 0.63 M

4.0 MATERIALS AND SAMPLES

4.1 150 ml solution B (sodium hydroxide, NaOH)

4.2 100 ml solution A (0.55 ml of concentrated sulphuric acid (H2SO4) was used to prepare
100 ml solution)
4.3 Phenolphthtalein indicator solution

5.0 APPARATUS
5.1 200 cm3 conical flasks
5.2 50 cm3 burette
5.3 250 cm3 beaker
5.4 Dropper
5.5 20 cm3 pipette

6.0 PROCEDURE
6.1 Weigh 8.0 g sodium hydroxide (NaOH) and dissolve in water to prepare 100 cm3 of
solution B.
6.2 Pipette 20 cm3 solution B into a conical flask.
6.2 Using a filter funnel, fill the burette with solution A to reach the zero mark exactly.
6.3 Add 3 to 4 drops of phenolphthalein indicator solution to the conical flask containing
solution B and titrate with solution A. Stop the titration immediately when the
solution in the conical flask is almost colourless. Record the trial titration results.
6.4 Repeat the titration 3 times to get accurate results.

7.0 RESULT
Table 15 : Volume (cm3) of solution A required to neutralize 20 cm3of solution B
Titration No. Trial 1 2 3

Burette readings
Initial burette
reading (cm3)

Final burette
reading (cm3)

Volume of acid
used (cm3)

* Complete your laboratory report and hand in before you leave the laboratory.

16
 PRACTICAL 5

1.0 AIM : DETERMINATION OF THE MOLARITY OF A GIVEN SODIUM CARBONATE

SOLUTION

2.0 OBJECTIVES

At the end of the session, students should be able to:

Determine the molarity of the given sodium carbonate solution.

3.0 THEORY
Acid – baseindicators (pH indicators) like methyl orange and phenolphthalein are substances
which change colour according to hydrogen ion concentration or solution to which they are
added. The indicators are weak organic acids or weak organic bases which dissociate partially
in aqueous solutions. The indicators are able to change the colour because the ions have
different colour from the undissociated molecules.

Generally, most of the indicators can represented as follows

H indicator H ++ indicator -
colour A colour B

Addition of acid (excess of H+) shifts the equilibrium to the left, thus the solution has colour A.
With the addition of alkali (OH -) H+ ions are removed . As a result, the equilibrium shifts to the
right and the solution has colour B.

KH indicator is known as the indicator dissociation constant

KH indicator = [H+] [indicator-]

[H indicator]

Therefore the pH at which the indicator changes colour is different for different indicators.

Table 10.0: Indicator dissociation constant (pKa = lg KH indicator)

Indicator pKa pH range Colour

Acid Neutral Alkali
Methyl Orange 3.1 3.2 – 4.4 Red Orange Yellow
Methyl Red 5.1 4.2 – 6.3 Red Orange Yellow
Bromocresol Blue 7.0 6.0 – 7.6 Yellow Green Blue
Phenolphthalein 9.3 8.2 – 10.0 Colourless Almost Pink
Colourless

The table 10.0 shows that the indicator dissociation constant (pKa = lg KH indicator) varies greatly.
Different indicators show colour change over a different pH range. The pH range in which an
indicator changes colour is called the indicator range. For methyl orange, the indicator is
yellow in a solution of pH 4.4. If acid was added to the solution, the colour changes through
several orange tones. At pH 3.1 the indicator changes to red and after that no further colour
change is observed.

17
4.0 MATERIALS AND SAMPLES

Materials: 0.1M hydrochloric acid (HCI), methyl orange indicator, distilled water.

Samples: Anhydrous sodium carbonate (Relative molecular mass: 106) (Q)

5.0 APPARATUS

Droppers, 20 ml pipette, conical flasks, 250 ml volumetric flask and burette

6.0 PROCEDURE
1. Weigh 2.00 g solid Q and dissolve in distilled water.
2. Put the solution into a 250 ml volumetric flask and add distilled water till it reaches the
calibration mark.
3. Pipette 20.0 ml of solution Q into a conical flask and titrate with 0.1 M HCI. Use methyl
orange as indicator.
4. Run a trial and carry out the titration at least 3 times to get an accurate result.
5. Calculate the molarity of the solution Q.

7.0 RESULT

Mass of solid Q = ……………………. g

Table 11.0: Burette readings

Trial titration Titration 1 Titration 2 Titration 3

Initial reading / cm3

Final reading / cm3

Volume / cm3
(Final reading – Initial
reading) / cm3

Average volume of HCl used = ______________ ml

What is the molarity of solution Q?

18
 PRACTICAL 6

1.0 AIM: Investigate the Degree of Ionisation of Ethanoic Acid in Aqueous Solution
2.0 OBJECTIVES
At the end of the practical students will be able to:
a) determine the concentration of ethanoic acid used.
b) determine the degree of acid dissociation when the value of Ka is given.
c) compare the concentration (molarity)of ethanoic acid, the concentration of hydrogen
ions (H+) and the degree of dissociation for ethanoic acid.

3.0 THEORY
The degree of ionisation or degree of acid dissociation isa fraction of the total number of
moles of an acid or base or electrolyte that dissociates into ions in an aqueous solution when
equilibrium is reached.
HA + H2O H3O+ + A-
Acid base hydrozonium ion anion
(Conjugate acid) (Conjugate base)

Water acts as a base in receiving protons and changes to its conjugate acid, H3O+. HA,as the
acid, donates protons and formsthe conjugate base A-.

The degree of dissociation(α) isexpressed as:

molarity of hydrogen ion [H+ ]

α (for HA acid) = =
molarity of acid [HA]

ion − ]
molarity of hydroxyl [OH
α (for B base) = =
molarity of base [B]

Strong acids and bases are assumed to be fully ionised in aqueous solution. The degree of
ionisation for strong acids and bases is unity (1). Weak acids and bases are not fully ionized
in aqueous solution. The value of the degree of ionisation for weak acids and bases is less
than unity (1).

Weak acids have a lower tendency to donate protons, so the equilibrium position for weak
acids is more to the left side in the equation, where most of the acid is still in the form of
covalent molecules and only a portion of it is dissociated to form ions.

CH3COOH + H2O CH3COO- + H3O+

Ethanoic acid water ethanoate ion hydrozonium ion
(acid) (base) (conjugate base) (conjugate acid)

covalent molecules ions

The relationship between concentration, degree of dissociation and dissociation constant for
weak acids and bases can be shown by Oswald’s law of dissociation.

19
 Ka = cα2
(1-α)
where,
c = concentration (mol dm-3)
α = degree of dissociation
Ka= acid dissociation constant

If the degree of dissociation is very small, then

(1-α ) ≈ 1, and cα2 = Ka or α = Ka
c

[H+] = cα = cKa = Ka.c

c

The degree of dissociation therefore depends on the concentration at a particular

temperature. The value of Ka is constant at a particular temperature and is not affected by
concentration.

4.0 MATERIALS AND SAMPLES

Materials: Distilled water, blue bromophenol indicatorsolution
Samples: 50 cm3 of 1M ethanoic acid solution

5.0 APPARATUS
50 cm3 volumetric flask, 1 cm3and 10 cm3 pipettes, test tubes and rack
6.0 PROCEDURE
1. Prepare 50 cm3 of 1M ethanoic acid.
2. Prepare 5 test tubes. Using a pipette, add 10 cm3 of the prepared ethanoic acid solution
into the first test tube. Then add 9 cm3 distilled water into the other 4 test tubes.
3. Transfer 1 cm3 acid solution from test tube 1to test tube 2.
4. Transfer 1 cm3 acid solution from test tube 2 to test tube 3 and so on for test tubes 4 and
5.
5. Test the solution in each test tube with universal pH paper and compare the resulting
colour with that on the provided scale to determine the pH of the solution.
6. Add 2 drops of blue bromophenol indicator to each test tube, record and observe the
changes in color.

Summary of series dilution:

1 cm3 1 cm3 1 cm3 1 cm3

Test tube 1 Test tube 2 Test tube 3 Test tube 4 Test tube 5

10 cm31 M 9 cm3 water 9 cm3 water 9 cm3 water 9 cm3 water

acid

20
7.0 RESULTS

Table 1 : Colour Changes with Bromophenol Blue and pH paper

Test tube
1 2 3 4 5
Changes of color

pH

8.0 DISCUSSION
1. Calculate the concentration of ethanoic acid, the concentration of H+ions and the degree
of dissociation, given that Ka of ethanoic acid at 25 °C is 1.80 x 10-5. Write your answer in
Table 2 below.

Table 2 : Molarity of acid, hydrogen ions and Degree of Dissociation (α)

Test tube pH value Molarity (M)of Molarity (M)of H+ Degree of
acid ions Dissociation
( [H+] = Kac ) α = Ka
c
1
2
3
4
5

2. By referring to your answers in Table 2, compare the acid concentration, hydrogen ion
concentration and degree of dissociation for ethanoic acid and explain your
observations.

3. If this experiment is repeated with hydrochloric acid (HCl), would the same resultsbe
obtained? Explain your answer.

21
 PRACTICAL 7

1.0 AIM : PREPARETION OF BUFFER SOLUTION

2.0 OBJECTIVES

At the end of the session, students should be able to:

4. to prepare buffer solutions from weak acid and it salt

5. to test the effects of added acid or base upon the pH to buffer solution.

3.0 THEORY

A buffer solution is a solution the pH of which does not change significantly on the addition
of a little acid or base. This property of resisting changes in pH is crucial for living organisms
as well as industrial processes. Without buffers, when 1cm³ of 1.0 M hydrochloric acid is
added to 1 dm³ of water, the pH changes from 7.0 to 3.0, a change of 4 units. If this happens
to the biological systems of living organisms, the organism would perish instantly.

Buffers are also important in many industrial processes. Certain processed foods have to be
prepared in a buffered form so that when consumed it does not cause undue change in pH.
A buffered solution must contain a relatively large quantity of acid to react with any OH¯
ions that might be added to it, and must also contain a relatively large quantity of base to
react with any H+ ions that might be added to it. The acid and base components of the
buffer solution must not neutralize one another.

The Henderson-Hasselbalch equation describes the derivation of pH as a measure of acidity

(using pKa, the acid dissociation constant) in biological and chemical systems. The equation
is also useful for estimating the pH of a buffer solution and finding the equilibrium pH in
acid-base reactions.

pH = pKa – log "[Acid]" /"[Salt]"

4.0 MATERIALS AND SAMPLES

Materials : Distilled water, acetic acid, sodium acetate, 1M HCl, 1 M NaOH

5.0 APPARATUS

Digital balance, 150 ml beaker, pH meter, glass rod, stirrer

22
6.0 PROCEDURE

A. Preparation of acidic buffer solution

4. Add about 50 mL of distilled water to a 100 mL beaker.

5. Use a volumetric pipette to add 5.0 mL of 0.30 M acetic acid to the beaker.
6. Accurately weigh a small beaker, add about 0.3 g sodium acetate (NaC2H3O2), and
weigh the beaker again. Record these masses in your notebook to all the sig figs
possible.
7. Insert a previously calibrated pH meter into the beaker.
8. Add a little bit of the sodium acetate at a time, stirring with a glass rod to dissolve
(do NOT stir with the pH probe!) until the pH is 5.0. In theory, this will take 0.216 g
of sodium acetate.
9. Weigh the beaker with the remaining sodium acetate.
10. Quantitatively transfer the buffer solution to a 100 mL volumetric flask.
11. Add distilled water up to the mark. Cap and invert the flask twice to mix. Heat the
beaker on the tripod stand until all the salt is dissolved.

B. Testing pH of Buffer Solution

1. The buffer solution was added into 100ml beaker and the pH was measured using
the pH electrode.
2. 50ml deionized water was added into two different beakers and the pH was
measured. The first beaker was added with 1.0 ml of 1M HCL and the second
beaker was added with 1.0 ml of 1M NaOH. The pH of each solution was
measured.
3. The above steps were repeated but by using buffer solution instead of deionized
water. The pH of each solution was measured.

23
7.0 RESULTS

Solution pH

Initial After adding HCl After adding NaOH

Deionised water

Buffer

24
 PRACTICAL 8

1.0 AIM : INVESTIGATE THE EFFECT OF CATALYST AND TEMPERATURE ON RATE OF

REACTION BETWEEN OXALIC ACID (ETHANEDIOIC ACID) AND POTASSIUM
MANGANATE(VII)

2.0 OBJECTIVES
At the end of practical student will be able to:
a) determine the relationship between temperature and rate of reaction.
b) determine the effect of a catalyst on the rate of reaction
c) Write the equation for the reaction

3.0 THEORY
When the temperature of reaction is increased, the rate of reaction increases. This happens
because at a high temperature, the molecules become more reactive and undergo more
collisions. Effective collisions increase because the frequency of molecular collisions
increases. These collisions produce enough energy for the formation of the reaction product.

A catalyst is a substance that increases the rate of reaction when added to the reaction
mixture. It does not react with the reactants in the mixture. The presence of a catalyst does
not change the concentrations of components in the mixture. It only increases the rate of
reaction.

4.0 MATERIALS AND SAMPLES

Materials: 50 cm³ sulphuric acid 1 M solution and distilled water

Samples: 25 cm³ 0.02 M potassium manganate (VII) solution and 25 cm³ 0.5 M oxalic acid
solution and 10 cm³ manganese (II) sulphate (10%) solution

5.0 APPARATUS
25 cm³, 10 cm³ and 50 cm³ volumetric flasks, 250cm³ beaker, test tube / boiling tube,
5 cm³ pipette, thermometer, bunsen burner and tripod stand

6.0 PROCEDURE
1. Prepare 25 cm³ of 0.02 M potassium manganate(VII) solution, 25 cm³ of 0.5 M oxalic
acid solution, 50 cm³ of 1M sulphuric acid solution and 10 cm³ of 10% w/v manganese
(II) sulphatesolution.

2. Prepare a water bath by half-filling a 250ml beaker with distilled water.

3. Prepare 2 pairs of test tubes, each pair labelled A and B

25
 4. To each test tube A, add 2 cm³ potassium manganate (VII) solution and 4 cm³ sulphuric
acid solution. To each test tube B add 2 cm³oxalic acid.

5. Put all the test tubes into the water bath. Insert a thermometer into one of the test
tubes. Heat the water bath gradually with a Bunsen flame.

6. When the temperature inside the test tube reaches 60 °C, mix the contents of 1 pair of
test tubes A and B and immediately start the stopwatch. Record the time taken for the
color of potassium manganate (VII) to disappear.

7. Repeat step 6 with the other pair of test tubes (A and B). This time add 1 drop of
manganese (II) sulphate solution to the mixture.

8. Repeat the experiment at the temperatures shown at the Table 1 below.

Table 1 : Time taken for manganate (VII) to be decolorized by oxalic acid.

Temperature (°C) Reaction without MnSO4 Reaction with MnSO4
Time (s) 1 -1 Time (s) 1
Time
(s ) Time
(s-1)
60
50
40
__ °C(Room
Temperature)

7.0 DISCUSSION
a) Write balanced equations for the reactions that occurred.

1
b) On the same paper, plot against temperature for the two reactions (with catalyst
Time
and without catalyst). (Use graph paper.)Compare and explain the differences between
the two graphs.

c) What is the effect of temperature on the rate of reaction?

26
 PRACTICAL 9

1.0 AIM : INVESTIGATEREVERSIBLE REACTIONS AND THE EFFECTS OF TEMPERATURE AND

ACIDITY ON CHEMICAL EQUILIBRIUM

2.0 OBJECTIVES
At the end of practical students should be able to:
a) Write the equation for the reversible reaction studied in this practical.
b) Identify the oxidising and reducing agents in the reaction.
c) Determine the effects of temperature and acidity changes on a chemical reaction in
equilibrium.

3.0 THEORY
In the reaction represented by:
Fe (p) + 4H2O (steam) Fe3O4+ 4H2 (g)

When steam is passed through hot iron filings, hydrogen gas and iron(III) oxide are
produced. Conversely, if hydrogen gas is passed through hot iron(III) oxide, the reaction is
reversed, producing steam and iron. This is an example of a reversible reaction.
If in the reaction represented above, the hydrogen gas produced is removed or consumed as
soon as it is produced, the forward reaction speeds up, forming hydrogen gas and iron(III)
oxide at a higher rate, while the reverse reaction slows down.

Fe(p) + 4H2O (gas) Fe3O4+ 4H2 (g)

Nett reaction from left to right

On the contrary, if the steam is removed, iron(III) oxide and hydrogen gas will react faster
produce more iron and steam. This means the nett reaction will move from right to left.

Fe (p) + 4H2O (steam) Fe3O4+ 4H2 (g)

Nett Reaction from right to left

In a chemical system that is at equilibrium, both forward and reverse reactions take place
simultaneously and at the same rate. A change in any of several factors in the environment
would trigger a change in the rates of the forward and reverse reactions. Therefore, the
nett direction of the reaction depends on the prevailing condition of the system.

4.0 MATERIALS AND SAMPLES

Materials: 6 M sodium hydroxide solution, 3 M and 0.01 M sulphuric acid solutions, 0.1M
potassium iodide solutionand distilled water

Samples: 0.1 M potassium dichromate(VI) (K2Cr2O7) solution, 0.1 M lead nitrate solution and
saturated bromine water

27
5.0 APPARATUS
50 cm³ volumetric flask, 50 cm³ burette, 5 cm³ pipette, 250 cm³ beaker, test tube, dropper,
bunsen burner and 100°C thermometer

6.0 PROCEDURE

6.1 Effect of Acidity on Equilibrium

6.1.1 To a test tube add about 4 cm³ 0.1M K2Cr2O7solution.
6.2.2 Tothe test tube add 1M sulphuric acid(CAUTION: CORROSIVE) using a
dropper, until a change in colour is observed. Record your observations.
6.2.3 Add 2M NaOH solution(CAUTION: CORROSIVE) to the mixture,until its
colour changes again. Record your observations.

6.2 Identifying the Oxidising Agent and Reducing Agent

6.2.1 Put 5 cm³ distilled water in a test tube.
6.2.2 Add 10 dropsof saturated bromine water.
6.2.3 Add distilled waterusing a dropper until changes are observed. Record
your observations.
6.2.4 Add 1M H2SO4solution using a dropper until changes are observed. Record
your observations.

6.3 Effect of change of temperature on equilibrium

6.3.1 To 3 cm³ 0.1M Pb(NO3)2solution in a test tube, add about the same amount
of KI solution.
6.3.2 Heat the mixture over a Bunsen flameand keep it boiling for 1 minute.
Record your observations.
6.3.3 Let the mixture cool quickly under a running tap. Observe if any further
changes take place.

7.0 RESULTS
Procedure 6.1 Potassium dichromate (K2CrO7) equilibrium
Experiment Observations
Add 1M H2SO4

Add 2M NaOH

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 Procedure 6.2 Bromine water equilibrium
Experiment Observations
Add 2MNaOH

Add 1M H2SO4

Procedure 6.3 Lead nitrate equilibrium

Experiment Observations
0.1M Pb(NO3)2

Add KI solution.

Heat mixture over bunsen

burner to boil vigorously.

Cool mixture under a

running tap.

8.0 DISCUSSION
1. Write the chemical equation for the reaction that occurred in Procedure 6.1.
2. What is the role of sulphuric acid and sodium hydroxide in the reaction in 6.1?
3. Write the chemical equation for the reaction that occurred in Procedure 6.2.
4. Is bromine water the oxidising or reducing agent? Explain your answer.
5. How does a change in temperature affect the equilibrium in Procedure 6.3?

29