MINISTRY OF EDUCATION

MATRICULATION DIVISION

CHEMISTRY
LABORATORY MANUAL

SK015 &
SK025
13th EDITION
 MATRICULATION DIVISION
MINISTRY OF EDUCATION MALAYSIA

CHEMISTRY
LABORATORY MANUAL
SEMESTER I & II
SK015 & SK025

MINISTRY OF EDUCATION MALAYSIA

MATRICULATION PROGRAMME

THIRTEENTH EDITION
First Printing, 2003
Second Printing, 2004
Third Printing, 2005 (Sixth Edition)
Fourth Printing, 2006 (Seventh Edition)
Fifth Printing, 2007 (Eighth Edition)
Sixth Printing, 2011 (Ninth Edition)
Seventh Printing, 2013 (Tenth Edition)
Eighth Printing, 2018 (Eleventh Edition)
Ninth Printing, 2020 (Twelfth Edition)
Tenth Printing, 2022 (Thirteenth Edition)
Copyright © 2022 Matriculation Division
Ministry of Education Malaysia

ALL RIGHTS RESERVED. No part of this publication may be reproduced or

transmitted in any form or by any means, electronic or mechanical, including
photocopying, recording or any information storage and retrieval system, without
the prior written permission from the Director of Matriculation Division, Ministry
of Education Malaysia.

Published in Malaysia by

Matriculation Division
Ministry of Education Malaysia,
Level 6 – 7, Block E15,
Government Complex Parcel E,
Federal Government Administrative Centre,
62604 Putrajaya,
MALAYSIA.
Tel: 603-8884 4083
Fax: 603-8884 4028
Website: www.moe.gov.my

Printed in Malaysia by

Malaysia National Library

Chemistry Laboratory Manual
Semester I & II
SK015 & SK025
Thirteenth Edition

e ISBN 978-983-2604-63-1

i
 NATIONAL EDUCATION PHILOSOPHY

Education in Malaysia is an on-going effort towards

further developing the potential of individuals in a
holistic and integrated manner, so as to produce
individuals who are intellectually, spiritually and
physically balanced and harmonious based on a firm
belief in and devotion to God. Such an effort is designed
to produce Malaysian citizens who are knowledgeable
and competent, who possess high moral standards and
who are responsible and capable of achieving a high
level of personal well-being as well as being able to
contribute to the betterment of the family, society and
the nation at large.

NATIONAL SCIENCE EDUCATION

PHILOSOPHY

In consonance with the National Education Philosophy,

science education in Malaysia nurtures a science and
technology culture by focusing on the development of
individuals who are competitive, dynamic, robust and
resilient and able to master scientific knowledge and
technological competency.

ii
 FOREWORD

I am delighted to write the foreword for the Laboratory Manual,

which aimed to equip students with knowledge, skills, and the
ability to be competitive undergraduates.

This Laboratory Manual is written in such a way to emphasise

students’ practical skills and their ability to read and understand
instructions, making assumptions, apply learnt skills and react
effectively in a safe environment. Science process skills such as
making accurate observations, taking measurement in correct
manner, using appropriate measuring apparatus, inferring,
hypothesizing, predicting, interpreting data, and controlling
variables are further developed during practical session. The
processes are incorporated to help students to enhance their
Higher Order Thinking Skills such as analytical, critical and
creative thinking skills. These 21st century skills are crucial to
prepare students to succeed in Industrial Revolution (I.R.) 4.0.

The manipulative skills such as handling the instruments, setting

up the apparatus correctly and drawing the diagrams can be
advanced through practical session. The laboratory experiments
are designed to encourage students to have enquiry mind. It
requires students to participate actively in the science process
skills before, during and after the experiment by preparing the pre-
report, making observations, analysing the results and in the
science process skills before, during, after the experiment by
preparing the pre-report, making observations, analysing the
results and drawing conclusions.

It is my hope and expectation that this manual will provide an

effective learning experience and referenced resource for all
students to equip themselves with the skills needed to fulfil the
prerequisite requirements in the first-year undergraduate studies.

DR HAJAH ROSNARIZAH BINTI ABDUL HALIM

Director
Matriculation Division

iii
 CONTENTS

Page
Students Learning Time (SLT) v
Learning Outcomes v
Laboratory Safety viii
Ethics In The Laboratory xi
Preparation For Experiment xi

Semester I
Experiment Title
1 Determination of the formula unit of a compound 1
Acid Base Titration – Determination of the
2 5
concentration of hydrochloric acid solution
3 Determination of the molar mass of a metal 10
4 Charles’ Law and the ideal gas Law 15
5 Chemical Equilibrium 22
6 pH measurement and its applications 29

Semester II
Experiment Title
1 Rate of reaction 36
2 Determining the heat of reaction 40
3 Electrochemical cells 44
4 Reactions of aliphatic and aromatic hydrocarbons 49
5 Reactions of hydroxy compounds 54
6 Aldehydes and ketones 58

References 62
Acknowledgements 63

iv
 Chemistry Lab Manual

1.0 Student Learning Time (SLT)

Students will be performing the experiment within the time allocated

for each practical work.

Face-to-face Non face-to-face

2 hour 0

2.0 Learning Outcomes

2.1 Matriculation Science Programme Educational Objectives

Upon a year of graduation from the programme, graduates

are:

1. Knowledgeable and technically competent in science

disciplines study in-line with higher educational
institution requirement.

2. Able to apply information and use data to solve

problems in science disciplines.

3. Able to communicate competently and collaborate

effectively in group work to compete in higher
education environment.

4. Able to use basic information technologies and engage

in life-long learning to continue the acquisition of new
knowledge and skills.

5. Able to demonstrate leadership skills and practice

good values and ethics in managing organisations.

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 Chemistry Lab Manual

2.2 Matriculation Science Programme Learning Outcomes

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

1. Acquire knowledge of science and mathematics as a

fundamental of higher level education.
(MQF LOC i – Knowledge and understanding)

2. Apply logical, analytical and critical thinking in

scientific studies and problem solving.
(MQF LOC ii – Cognitive skills)

3. Demonstrate manipulative skills in laboratory works.

(MQF LOC iii a – Practical skills)

4. Collaborate in group work with skills required for

higher education.
(MQF LOC iii b – Interpersonal skills)

5. Deliver ideas, information, problems and solution in

verbal and written communication.
(MQF LOC iii c – Communication skills)

6. Use basic digital technology to seek and analyse data

for management of information.
(MQF LOC iii d – Digital skills)

7. Interpret familiar and uncomplicated numerical data to

solve problems.
(MQF LOC iii e – Numeracy skills)

8. Demonstrate leadership, autonomy and responsibility

in managing organization.
(MQF LOC iii f – Leadership, autonomy and
responsibility)

9. Initiate self-improvement through independent

learning.
(MQF LOC iv – Personal and entrepreneurial skills)

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 Chemistry Lab Manual

10. Practice good values attitude, ethics and accountability

in STEM and professionalism.
(MQF LOC v – Ethics and professionalism)

2.3 Course Learning Outcome

2.3.1 Chemistry 1

At the end of the course, student should be able to:

1. Explain the fundamental concepts in chemistry.

(C2, PLO 1, MQF LOC i)

2. Solve problems with analytical and critical thinking

using chemistry facts and principles.
(C4, PLO 2, MQF LOC ii)

3. Apply the appropriate scientific laboratory skills in

chemistry experiments.
(P3, PLO 3, MQF LOC iii a)

4. Analyse numerical problems in chemistry.

(C4, PLO 7, MQF LOC iii e)

2.3.2 Chemistry 2

At the end of the course, student should be able to:

1. Explain the fundamental concepts in chemistry.

(C2, PLO 1, MQF LOC i)

2. Solve problems with analytical and critical thinking

using chemistry facts and principles.
(C4, PLO 2, MQF LOC ii)

3. Apply the appropriate scientific laboratory skills in

chemistry experiments.
(P3, PLO 3, MQF LOC iii a)

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 Chemistry Lab Manual

2.4 Objectives of Practical Sessions

The main purpose of the experiment is to give the student a

better insight of the concepts of Chemistry discussed in the
lectures by carrying out experiments. The aims of the
experiments are to enable students to:

1. Learn and practise the necessary safety precautions in

the laboratory.

2. Plan, understand and carry out the experiment.

3. Use the correct techniques in handling the apparatus.

4. Acquire scientific skills in measuring, recording and

analysing data.

5. Observe, measure and record data by giving

consideration to the consistency, accuracy and units
of the physical quantities.

6. Determine the errors in various physical quantities

obtained in the experiments.

7. Deduce logically and critically the conclusion based

on observation and data analysis.

3.0 Laboratory Safety

The Science Matriculation Programme requires the students to

attend practical classes two hours a week to complete six
experiments each semester.

In order for the laboratory to be a safe place to work in, students

should learn laboratory rules and regulations, including the correct
way of using laboratory apparatus and handling of chemicals before
starting any experiments.

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 Chemistry Lab Manual

Laboratory rules and regulations.

1. Attendance is COMPULSORY. If you are unable to attend any

practical class, you should produce a medical certificate or a
letter of exemption.

2. Read, understand and plan your experiment before pre-lab

sessions and practical classes.

3. Wear shoes, lab coats and safety goggles at all times in the
laboratory.

4. Tie long hair or tuck head scarf under your lab coat

5. Do not wear contact lenses during experiments.

6. Foods and drinks are not allowed in the laboratory.

7. Do not perform any unauthorised experiments! Understand

and follow the specified procedures for each experiment.

8. Do not waste chemicals. Take only sufficient amount of

chemicals needed for your experiments.

9. Replace the lids or stoppers on the reagent bottles or

containers immediately after use.

10. Do not remove chemicals from the laboratory.

11. Handle volatile and hazardous compounds in the fume

cupboard. Avoid skin contact with all chemicals, wash off any
spillages.

12. Clean up spillages immediately. In case of a mercury spillage,

do not touch the mercury. Notify your instructor immediately.

13. Ensure there are no flames in the vicinity before working with
flammable chemicals

14. NEVER leave an ongoing experiment unattended.

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 Chemistry Lab Manual

15. Be aware or familiar with the location and proper way of

handling safety equipment, including eyewash, safety shower,
fire blanket, fire alarm and fire extinguisher.

16. Turn off bunsen flames when not in use. Notify your
instructor immediately of any injury, fire or explosion

17. Do not throw any solid wastes into the sink. Dispose any
organic substances in the waste bottles provided.

18. Wash all glassware after use and return the apparatus to its
appropriate places.

19. Keep your work area clean and tidy.

20. Notify your instructor immediately of any injury, fire or

explosion

I have read and understood the laboratory rules and regulations

as stated above. I agree to abide by all these rules, follow the
instructions and act responsibly at all times.

Signature: Date:

Name: Practicum:

Matric number:

Signature Instructor: Date:

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 Chemistry Lab Manual

4.0 Ethics in the laboratory

1. Follow the laboratory rules.

2. Students must be punctual for the practical session. Students

are not allowed to leave the laboratory before the practical
session ends without permission.

3. Co-operation between members of the group must be

encouraged so that each member can gain experience in
handling the apparatus and take part in the discussions about
the results of the experiments.

4. Record the data based on the observations and not based on

any assumptions. If the results obtained are different from
the theoretical value, state the possible reasons.

5. Get help from the instructor or the laboratory assistant

should any problems arise during the practical session.

5.0 Preparation for experiment

5.1 Pre-lab Sessions.

1. Read and understand the objectives and the theory of

the experiment.

2. Think and plan the working procedures properly for

the whole experiment. Make sure you have
appropriate table for the data.

3. Complete and submit the pre-lab questions provided.

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 Chemistry Lab Manual

5.2 Practical Sessions

1. Check the apparatus provided.

2. Conduct the experiment carefully.

3. Record all measurements and observations made

during the experiment.

4. Keep the work area clean and tidy.

5.3 Post-lab Sessions

1. Explain what has been carried out and discuss the

findings of the experiment.

2. Introduce the format of report writing as below:

Objective ▪ state clearly

▪ write concisely in your own words
Theory
▪ draw and label diagram if necessary
▪ write in passive sentences about all the
Procedure
steps taken during the experiment
▪ data tabulation with units and
uncertainties
Results/
▪ data processing (plotting graph,
Observation
calculation to obtain the results of the
experiments and its uncertainties)
▪ give comments about the experimental
results by comparing it with the standard
value.
Discussion ▪ state the source of mistake(s) or error(s)
if any as well as any precaution(s) taken
to overcome them.
▪ answer all the questions given
▪ state briefly the results with reference to
Conclusion
the objectives of the experiment
Reminder: NO PLAGIARISM IS ALLOWED.

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CHEMISTRY 1
SK015
 Chemistry Lab Manual – SK015

EXPERIMENT 1: DETERMINATION OF THE FORMULA UNIT

OF A COMPOUND

Objectives

At the end of this lesson, students should be able to:

i. synthesise a zinc chloride compound; and
ii. determine the formula unit of zinc chloride.

Introduction

One of the main properties of a compound is its chemical composition which

can be identified by determining the elements present. A quantitative
analysis can be used to determine the composition of an unknown
compound. Once the composition of the compound is known, it’s formula
unit can be determined. For example, a compound containing 0.1 mol of
silver and 0.1 mol of bromine will have a formula unit, AgBr.

In this experiment, a simple compound composed of zinc and chlorine will

be prepared. Once the mass of zinc and the mass of the compound are
known, the mass of chlorine can be determined. Using these masses, the
percentage composition of the compound can be calculated and the formula
unit can be deduced.

Apparatus Chemical Reagents

Hot plate 6 M HCl

Glass rod Zinc powder
White tile
Crucible tongs
50 mL crucible
Analytical balance
Measuring cylinder (10 mL)

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 Chemistry Lab Manual – SK015

Procedure

1. Weigh the crucible and record the exact mass.

2. Place approximately 0.25 g of zinc powder into the crucible and

determine the exact mass of zinc powder.

3. Carefully add in 10 mL of 6 M HCl solution into the crucible

containing the zinc powder and stir gently with a glass rod. A vigorous
chemical reaction will occur and hydrogen gas will be released.

Carry out this step in a fume cupboard. Do not

CAUTION ! work near a fire source. Wet hydrogen gas can
cause explosions.

4. If the zinc powder does not dissolve completely, continue adding the
acid, 5 mL at a time until all zinc is dissolved. The amount of acid to be
used must not exceed 20 mL.

5. Place the crucible on a hot plate in the fume cupboard and heat the
content slowly so that the compound does not splatter during the
heating process.

6. Heat the compound gently until it is completely dry. Remove the

crucible from the hot plate immediately to avoid the compound from
melting.
(Precaution: Avoid from overheating)

7. Cover the crucible and allow it to cool to room temperature. Then

weigh the crucible and the compound. Record the mass.

8. Reheat the crucible to dry the compound. Let it cool to room

temperature and then weigh it again. Repeat the procedure until the
difference in mass does not exceed 0.02 g.

9. Determine the mass of zinc chloride from the final weight of the
sample (the smallest value). Calculate the mass of chlorine in the zinc
chloride.

10. Determine the formula unit of zinc chloride.

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 Chemistry Lab Manual – SK015

POINT TO DISCUSS

1. Explain why the content is not weighed while it is still hot.

2. Explain why the crucible needs to be covered during cooling.

3. Write a balanced equation for the reaction between zinc and

hydrochloric acid.

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 Chemistry Lab Manual – SK015

DATA SHEET

EXPERIMENT 1: DETERMINATION OF THE FORMULA UNIT

OF A COMPOUND

RESULTS

No. Item Mass (g)

1. Mass of empty crucible

2. Mass of crucible + zinc powder

3. Mass of zinc powder

4. Mass of crucible + zinc chloride:

i) First heating

ii) Second heating

iii) Third heating

5. Mass of zinc chloride

6. Mass of chlorine

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 Chemistry Lab Manual – SK015

EXPERIMENT 2: ACID-BASE TITRATION − DETERMINATION

OF THE CONCENTRATION OF
HYDROCHLORIC ACID SOLUTION

Objectives

At the end of this lesson, students should be able to:

i. prepare a standard solution of oxalic acid.
ii. standardise 0.2 M NaOH solution.
iii. determine the concentration of HCl solution.
iv. acquire the correct techniques of titration

Introduction

Titration is a laboratory technique used to determine the concentration of a

solution using another solution with a known concentration.

Standards in acid-base titrations

One of the solutions involved in a titration is used as a standard solution.

The standard solution can be classified as either primary or secondary. A
primary standard solution is prepared by dissolving an accurately weighed
pure solid of a known molar mass in a known volume of distilled water.

A primary standard is used to determine the molarity of the other standard

solution, known as a secondary standard. For example, oxalic acid,
H2C2O4, and potassium hydrogen phthalate, KHC8H4O4, are two common
primary standards used to determine the concentration of bases (secondary
standard).

The NaOH solution used in titrations need to be standardized because they

contain impurities. Solid NaOH is hygroscopic (it absorbs moisture). Thus, it
is difficult to obtain its accurate mass. The standardized NaOH becomes the
secondary standard and can then be used to determine the concentration of
other acids such as HCl acid.

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 Chemistry Lab Manual – SK015

Equivalence point and end point

An equivalence point is the point in a titration at which the added titrant

reacts completely with the electrolyte according to stoichiometry.To detect
this equivalence point, an indicator which produces a change in colour is
often used. The point at which the indicator changes colour is called the end
point. The end point and equivalence point should ideally be the same.

Chemical equations

In this acid-base titration, the neutralisation reactions involved are:

H2C2O4(aq) + 2NaOH(aq) → Na2C2O4(aq) + 2H2O(l) . . .(1)

HCl(aq) + NaOH(aq) → NaCl(aq) + H2O(l) . . .(2)

Apparatus Chemical Reagents

Burette x M HCl
Dropper 0.2 M NaOH
Glass rod Distilled water
White tile Phenolphthalein
Retort stand Hydrated oxalic acid, H2C2O4.2H2O
Filter funnel
50 mL beaker
25 mL pipette
Analytical balance
250 mL conical flask
250 mL volumetric flask
50 mL measuring cylinder

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 Chemistry Lab Manual – SK015

Procedure

(A) Preparation of standard solution

1. Weigh to the nearest 0.0001 g about 3.00 g of hydrated oxalic

acid, H2C2O4.2H2O in a 50 mL beaker.

2. Add approximately 30 mL of distilled water to dissolve the

oxalic acid.

3. Transfer the solution into a 250 mL volumetric flask. Rinse the

beaker and pour the content into the flask. Add distilled water
up to the calibrated mark of the volumetric flask.

4. Stopper and shake the flask to obtain a homogeneous solution.

5. Calculate the concentration of the standard oxalic acid solution.

NOTE: Use this solution to standardize the NaOH solution in

Part (B).

(B) Standardisation of 0.2 M NaOH solution

1. Rinse a burette with a given NaOH solution to be standardized.

2. Fill the burette with the NaOH solution. Ensure there are no air
bubbles trapped at the tip.

3. Record the initial burette reading to two decimal places.

4. Pipette 25 mL of oxalic acid solution from Part (A) into a 250

mL conical flask. Add 2 drops of phenolphthalein to the oxalic
acid solution.

5. Place a white tile underneath the flask so that any colour

change can be clearly observed.

6. Titrate the acid with the NaOH solution from the burette.
During the titration, swirl the flask continuously.

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 Chemistry Lab Manual – SK015

7. Rinse the unreacted solutions at the inner wall of the conical

flask with distilled water.

8. Upon reaching the end point, a temporary pink solution appears

but fades when the solution is swirled. Continue titrating until a
pale pink colour persists for more than 30 seconds. This is the
end point.

9. Record the final burette reading to two decimal places.

10. Repeat the titration three times.

11. Calculate the molarity of the NaOH solution.

(C) Determination of the molar concentration of HCl solution.

1. Pipette 25 mL of a given HCl solution into a 250 mL conical

flask.

2. Add two drops of phenolphthalein.

3. Repeat steps 5-9 as in Part (B).

4. Calculate the concentration of HCl.

POINT TO DISCUSS

Does the addition of water in step 7 (Part B) affect the result of the
titration? Explain.

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 Chemistry Lab Manual – SK015

DATA SHEET

EXPERIMENT 2: ACID-BASE TITRATION − DETERMINATION

OF THE CONCENTRATION OF
HYDROCHLORIC ACID SOLUTION

RESULTS

(A) Preparation of standard oxalic acid solution

i. Exact mass of hydrated oxalic acid =

ii. Moles of hydrated oxalic acid =
iii. Molarity of oxalic acid =

(B) Standardisation of 0.2 M NaOH solution

Burette reading / mL Gross I II III

Final reading
Initial reading
Volume of NaOH used /
mL

Average volume of NaOH used =

Calculate the molarity of the NaOH solution.

(C) Determination of the molar concentration of HCl solution

Burette reading / mL Gross I II III

Final reading
Initial reading
Volume of NaOH used /
mL

Average volume of NaOH used =

Calculate the molarity of the HCl solution

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 Chemistry Lab Manual – SK015

EXPERIMENT 3: DETERMINATION OF THE MOLAR MASS OF

A METAL

Objectives

At the end of this lesson, students should be able to:

i. standardize the hydrochloric acid solution.
ii. determine the molar mass of an alkaline earth metal by back- titration
method.

Introduction

A reactive metal, for example an alkaline earth metal, would readily react
with a strong acid such as hydrochloric acid. The general reaction between a
metal, M and an aqueous hydrochloric acid, HCl is as follows:

M(s) + 2HCI(aq) → MCl2(aq) + H2(g)

The molar mass of M can be determined by a back-titration. A back

titration is a two-stage analytical technique. The first stage involves the
reaction of a metal with an excess amount of acid of a known concentration.
In the second stage, the unreacted acid is titrated with a standardized base
solution to determine the amount of the remaining excess reactant.

In this experiment, the concentration of the acid is initially determined by the

normal titration before the reaction with metal M is carried out. M reacts
completely according to stoichiometric equation and if the amount of acid
used exceeds the amount of metal in terms of equivalence, then the resulting
solution would be acidic.

The excess acid can be determined by performing back-titration with sodium

hydroxide solution. The amount in moles of the reacted metal is determined
by comparing the moles of acid before and after the reaction.

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 Chemistry Lab Manual – SK015

Apparatus Chemical Reagents

Scissors Distilled water

Dropper Phenolphthalein
White tile x M Hydrochloric acid, HCl
Pipette filler 1.0 M Sodium hydroxide, NaOH,
Filter funnel An unknown alkaline earth metal, M
Retort stand
50 mL beaker
50 mL burette
25 mL pipette
Analytical balance
250 mL conical flask
Abrasive cloth no.3 (36) / sandpaper
Aluminium oxide

Procedure

(A) Standardization of HCl solution

1. Rinse a clean burette with 1.0 M NaOH.

2. Fill the burette with 1.0 M NaOH solution.

3. Record the initial burette reading to two decimal places.

4. Pipette 25 mL HCl solution into a 250 mL conical flask. Add 2

drops of phenolphthalein to the acid.

5. Place a piece of white tile underneath the flask.

6. Titrate the acid with the NaOH solution. Swirl the flask
continuously.

7. Upon reaching the end point, a temporary pink solution will

appear but the colour will fade when it is swirled. Continue
titrating until the pale pink colour remains for more than 30
seconds. This is the end point.

8. Record the final reading of the burette.

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 Chemistry Lab Manual – SK015

9. Repeat the titration three times.

10. Calculate the concentration of the HCI solution.

(B) Determination of the molar mass of a metal

1. Pipette 25 mL of HCl solution into 2 separate conical flasks.

2. Clean two pieces of metal M, each of approximately 4 cm long,

with a piece of abrasive cloth.

3. Weigh accurately the mass of each sample.

4. Cut each sample into smaller pieces. Place the samples

separately into the HCl solution. Swirl occasionally until the
metal is completely dissolved.

5. Add 2 drops of phenolphthalein.

6. Record the initial burette reading.

7. Titrate the unreacted HCl with the NaOH solution.

8. Record the final burette reading.

9. Repeat titration with the other sample.

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DATA SHEET

EXPERIMENT 3: DETERMINATION OF THE MOLAR MASS OF

A METAL

RESULTS

1. Titration of standard HCl solution

Concentration of NaOH = ___________ M

Volume of HCl = ___________ mL

Burette reading / mL Gross I II III

Final reading
Initial reading
Volume of NaOH /
mL

Average volume of NaOH =

2. Reaction of metal and HCl

Mass of metal (sample I) (g)

Mass of metal (sample II) (g)

3. Titration of unreacted HCl

Burette reading / mL Sample I Sample II

Final reading
Initial reading
Volume of NaOH (mL)

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 Chemistry Lab Manual – SK015

CALCULATION

1. Calculate the molarity of the standard HCl solution.

2. Determine the number of moles of HCl in 25 mL of the standard

solution.

3. Calculate the number of moles of the unreacted HCl solution.

Sample I:

Sample II:

4. Calculate the number of moles of the reacted metal.

Sample I:

Sample II:

5. Determine the molar mass of metal in each sample.

Sample I:

Sample II:

Average molar mass of metal = _______

6. By comparing the results with elements in the periodic table,

determine the metal M.

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 Chemistry Lab Manual – SK015

EXPERIMENT 4: CHARLES’ LAW AND THE IDEAL GAS LAW

Objectives

At the end of this lesson, students should be able to:

i. verify Charles’ Law.
ii. determine the molar mass of a volatile liquid.

Introduction

Charles’ Law states that the volume of a fixed mass of a given gas is
directly proportional to its absolute temperature at constant pressure. The law
is written as

V  T (n, P constant)

In this experiment, a quantity of air is trapped between the sealed end of a

thick-walled glass tube (with a small cross-sectional area) and a movable
plug of mercury. If the glass tube is held upright, the plug of mercury will
move to a position where the pressure of the air in the tube is equal to the
atmospheric pressure and a small pressure exerted by the plug. Thus, the
pressure of the trapped air is constant.

The volume, V, of the trapped air is obtained by multiplying the cross-

sectional area of the tube, A, with the height of the air column, h.

V= A x h

Assuming that the cross-sectional area is constant, the volume is directly

proportional to the height, i.e., V  h. Therefore, the height of the air column
can be used as a measure of the volume in this experiment. By measuring
this height at different temperatures we can determine the relationship
between the volume of the trapped air and its temperature at constant
pressure.

Ideal Gas Equation:

By combining the relationships govern by the gas laws, a general equation

known as the ideal gas equation can be obtained.

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 Chemistry Lab Manual – SK015

Boyle’s Law
Volume of a fixed mass of a given gas is inversely proportional to its
pressure at constant temperature.
1
V  (n, T constant)
p

Avogadro’s Principle
All gases of equal volume will contain the same number of molecules at the
constant temperature and pressure.

V  n (T, P constant)
Charles’ Law
Volume of a fixed mass of a given gas is directly proportional to its absolute
temperature at constant pressure.

V  T (n, P constant)

Thus, combining the three laws, we get

nT
V 
p

The above expression can be written as

RnT
V = or PV = nRT ...........(1)
P

This is the ideal gas equation and R is called the gas constant. The number of
moles, n,
mass
n =
Molar mass, Mr

Therefore, the ideal gas equation can also be written as

RT
PV = m ( ) ..........(2)
Mr

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Apparatus Chemical Reagents

Needle Ice
Wire gauze Methanol
Tripod stand Unknown liquid
Rubber band
Thermometer
Bunsen burner
Aluminum foil
Analytical balance
Barometer
Retort stand and clamp
Charles’ law apparatus
600 mL beaker
100 mL conical flask
100 mL measuring cylinder
Stopwatch

Procedure

(A) Charles’ Law

1. Tie a thermometer to a glass tube containing a plug of

mercury with a rubber band. The bulb of the thermometer is
placed approximately half-way up the column of the trapped
air as shown in Figure 4.1.

Figure 4.1
Charles’ law apparatus

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2. Fill a 100 mL measuring cylinder with tap water. Place the

tube and the thermometer into the water until the air column
in the tube is immersed.

3. Leave for 5 minutes to ensure that the temperature of the

trapped air is equivalent to the temperature of the tap water.

4. Record the temperature and measure the height of the air

column.

5. Repeat Steps 2 until 4 using:

i. warm water (40 – 50°C)

ii. a mixture of ice and water
iii. a mixture of ice and 5 mL methanol

NOTE: Ensure that the mercury plug does not split into small
droplets.

(B) Determination of the molar mass of a gas

1. Cover a 100 mL conical flask with a piece of aluminium foil

and tie it loosely around the neck with a rubber band as shown
in Figure 4.2.

Figure 4.2 Figure 4.3

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2. Prick a tiny hole in the middle of the foil with a needle.

3. Weigh the apparatus accurately.

4. Remove the foil and place 5.0 mL of the unknown liquid into
the flask.

5. Replace the foil and tie it with a rubber band.

6. Clamp the neck of the flask and immerse it into a 600 mL

beaker containing water as shown in Figure 4.3.

7. Heat the water until all of the unknown liquid in the flask has
vaporised.

8. Record the temperature of the water bath when all the

unknown liquid has evaporated.

9. Take out the flask immediately by using the clamp.

10. Wipe the outer wall of the flask and the aluminium foil when
the flask is cooled.

11. Weigh the flask with the aluminium foil, rubber band and the
condensed unknown liquid.

12. Discard both the foil and the condensed liquid. Fill the flask
up to the brim with water and pour it into a measuring
cylinder. Record the volume of water.

13. Record the barometric pressure.

14. Calculate the molar mass of the unknown liquid using the
ideal gas equation.

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DATA SHEET

EXPERIMENT 4: CHARLES’ LAW AND THE IDEAL GAS LAW

RESULT

(A) Charles’ law

TABLE 1

Volume
Temperature
Condition (Height of gas column)
(0C)
(mm)
Warm water
Tap water
Ice-water
Ice-methanol

1. Complete TABLE 1.

2. Plot the height of the column, h, against temperature, T, in celsius on a

graph paper. Based on the graph, state the relationship between volume
and temperature.

3. Extrapolate the line until h = 0, to obtain the absolute zero temperature.

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(B) Determination of the molar mass of the gas

TABLE 2

No Item Reading
1. Mass of flask + rubber band + cover (g)
Mass of flask + rubber band + cover + condensed
2.
liquid (g)
3. Mass of condensed liquid (g)
4. Temperature of water bath (oC)
5. Barometric pressure (mm Hg)
6. Volume of flask (mL)

4. Complete TABLE 2.

5. Calculate the molar mass of the unknown liquid.

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EXPERIMENT 5: CHEMICAL EQUILIBRIUM

Objectives

At the end of this lesson, students should be able to:

i. study the effect of concentration and temperature on chemical
equilibrium.
ii. determine the equilibrium constant, Kc, of a reaction.

Introduction

There are two types of chemical reactions, namely irreversible and

reversible. A reversible reaction will reach a dynamic equilibrium when the
rate of the forward reaction is equal to the rate of the reverse reaction. At this
stage, one cannot observe any changes in the system as the concentration of
reactants are constant. This does not mean that the reactions have stopped,
instead, the reactions are still occurring but at the same rate.

The factors that influence chemical equilibrium are:

i. concentration
ii. temperature
iii. pressure (for reactions that involve gases)

A change in one of the factors on a system that is already at equilibrium, will

cause the reaction to move to the direction that minimizes the effect of
change. The direction of the change can be determined by applying Le
Chatelier’s Principle.

Le Chatelier’s Principle states that if a system at equilibrium is disturbed by

a change in temperature, pressure or concentration of one or more
components, the system will shift its equilibrium position in such a way so as
to counteract the effect of the disturbance.

The effect of concentration

According to the Le Chatelier’s principle, the change in concentration of any

substance in a mixture at equilibrium will cause the equilibrium position to
shift in the forward direction or reverse direction to re-attain the equilibrium.

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Consider a general reaction as follows:

A + B C + D

If substance A or B is added to a mixture at equilibrium, the reaction will

shift forward to reduce the concentration of A or B until equilibrium is re-
established.

On the other hand, if substance C or D is added, the equilibrium will shift in

the direction that will reduce the concentration of C or D, i.e. from right to
left until equilibrium is re-established.

The effect of temperature

The effect of temperature on an equilibrium system depends on whether the

reaction is exothermic or endothermic. Consider the following system:

E + F G + Heat

If the forward reaction is exothermic, then the heat released is considered as

one of the products. Heating the system will cause the equilibrium to shift in
the reverse direction so as to reduce the excess heat. Thus, the concentrations
of E and F increase while the concentration of G decreases. However, when
the system is cooled, the equilibrium will move forward to increase the heat
in the system. The same principle can be applied to explain an endothermic
system.

In this experiment, you will study the effect of changes in concentration and
temperature on two equilibrium systems. You can notice the shift in
equilibrium through changes in colour or phases such as precipitation or
dissolution.

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Apparatus Chemical Reagents

Burette 6 M HCl
Ice bath 0.2 M CoCl2
Test tube 2.5 M NaOH
Water bath 0.1 M KSCN
10 mL pipette 0.1 M Fe(NO3)3
100 mL beaker 0.5 M SbCl3 in 6 M HCl
100 mL conical flask
10 mL measuring cylinder
100 mL measuring cylinder

Procedure

(A) The effect of concentration in the formation of thiocyanoiron(III)

complex ion

The thiocyanoiron(III) complex ion is formed when iron(III) ion, Fe3+,

is added to the thiocyanate ion, SCN-. The equation for the reaction is

Fe3+ (aq) + 2SCN- (aq) [Fe(SCN)2]+(aq)

(Yellowish brown) (blood-red)

1. Place 2 mL of 0.1 M Fe(NO3)3 solution and 3 mL of 0.1 M

KSCN solution in a 100 mL beaker.

2. Add 50 mL of distilled water to reduce the intensity of the blood

red solution.

3. Place approximately 5 mL each of this solution into four test

tubes.

(a) To the first test tube, add 1 mL of 0.1 M Fe(NO3)3.

(b) To the second test tube, add 1 mL of 0.1 M KSCN.
(c) To the third test tube, add 6-8 drops of 2.5 M NaOH.
(d) The fourth test tube serves as a control.

4. Tabulate the observations.

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(B) The Effect of Temperature

The reaction between hexaaquocobalt(II) complex ion with chloride

ion produces tetrachlorocobalt(II) ion. The equation for the reaction is
given below:

[Co(H2O)6]2+(aq) + 4Cl-(aq) [CoCl4]2-(aq) + 6H2O(l)

(pink) (blue)

1. Place 2 mL of 0.2 M CoCl2 solution into a conical flask.

2. Add 20 mL of 6 M HCl and swirl the flask.

3. A purple solution should form, indicating a mixture of pink and

blue. If the solution appears pink, add more HCl; if it is blue, add
more distilled water.

4. Divide the purple solution into 3 separate test tubes.

(a) Leave one test tube at room temperature.

(b) Place the second test tube in an ice bath.
(c) Place the third test tube in a water bath at 80 – 90 °C.

5. Record the colour of the solution in each test tube. Remove the
second and the third test tubes and leave them at room
temperature. Observe the change in colour.

POINT TO DISCUSS

Determine whether the forward reaction is exothermic or endothermic.

Discuss.

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(C) Determination of the equilibrium constant.

The following reaction is an example of a heterogenous system:

SbCl3(aq) + H2O(l) SbOCl(s) + 2HCl(aq)

The expression for the equilibrium constant is:

[HCl]2
Kc =
[SbCl 3 ]

1. Pipette 5.0 mL of 0.5 M SbCl3 in 6 M HCl into a conical flask.

2. Carefully add distilled water from a burette into the conical flask
while swirling until a faint white precipitate is obtained.

3. Record the volume of water added.

4. Calculate the value of the equilibrium constant, Kc.

POINT TO DISCUSS

Explain why the concentration of pure liquid and solid are excluded from the
equilibrium constant expression for a heterogeneous system.

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DATA SHEET

EXPERIMENT 5: CHEMICAL EQUILIBRIUM

RESULT

(A) The effect of concentration in the formation of thiocyanoiron(III)

complex ion

Test
Experiment Observation
tube
Addition of 1 mL of 0.1M
I
Fe(NO3)3

Addition of 1 mL of 0.1M
II
KSCN

Addition of 6-8 drops of

III
10% NaOH

(B) The Effect of Temperature

Test
Experiment Observation
tube

I At room temperature

II 0 ⁰C (in ice bath)

III 80- 90 ⁰C

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When left at room temperature:

Test Observation
tube

II

III

(C) Determination of the equilibrium constant

Burette reading / mL Observation

Initial reading

Final reading

Volume of water

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EXPERIMENT 6: pH MEASUREMENT AND ITS APPLICATIONS

Objectives

At the end of this lesson, students should be able to:

i. use various methods to measure the pH of acids, bases and salts.
ii. determine the dissociation constant, Ka, of acetic acid.

Introduction

pH is a measure of acidity or basicity of a solution. pH is defined as the

negative logarithm of hydrogen ion concentration, [H+].

pH = − log [H+] ……….(1)

The pH scale ranges from 0 to 14. At 25°C, a neutral solution has a pH of 7.

An acidic solution has a pH of less than 7 while a basic solution has a pH
greater than 7.

There are two methods to determine pH in the laboratory. The first method
involves the use of indicators such as pH paper and the universal indicator.
The second method is using the pH meter.

Acids or bases which ionise completely are called strong acids or strong
bases. An example of a strong acid is HCl and a strong base is NaOH. Weak
acids and weak bases do not ionise completely. An example of a weak acid is
acetic acid, CH3COOH, and that of a weak base is ammonia, NH3.

Consider the ionisation of a weak acid, HA.

HA(aq) H+(aq) + A-(aq) ……….(2)

The equilibrium constant expression for the above reaction is written as:

[H + ][A − ]
Ka = ……….(3)
[HA]
where [H+], [A−] and [HA] represent the molar concentrations of species that
exist at equilibrium. Kais the dissociation constant for acid HA. A similar
expression of Kb can be written for weak bases.

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One of the methods to determine Ka is by adding a weak acid solution to its

conjugated base solution. The product of this process is an acidic buffer
solution. The conjugated base is obtained from the salt produced using the
titration method.

In this method, a known weak acid, HA is divided into two equal portions, X
and Y. The first portion, X is titrated with NaOH solution using
phenolphthalein as an indicator to detect the formation of a salt solution. A
change in colour, from colourless to light pink, indicates the end point. The
equation for the reaction is:-

OH−(aq) + HA(aq) A−(aq) + H2O(l) ……….(4)

In this reaction, HA reacts with NaOH to form NaA and H2O. NaA ionises
completely to form A− and Na+. The number of moles of A− formed is the
same as the number of moles of HA in the second portion, Y, which has not
been titrated.

The second portion of the weak acid HA is added to the conical flask
containing the salt NaA. In this mixture, the concentration of HA is equal to
the concentration of A− from the salt.

Since [A−] = [HA], and from Equation 3,

Ka = [H+]

The value of [H+] is obtained by measuring the pH; hence the value of Ka can
be calculated.

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Apparatus Chemical Reagents

Burette Methyl red
Test tube Methyl orange
pH meter Alizarin yellow
25 mL pipette Phenolphthalein
250 mL conical flask Universal indicator
0.1 M NaCl
0.1 M NH4NO3
0.1 M CH3COONa
0.1 M and 1.0 M NH3
0.01 M and 1.0 M HCl
0.1 M and 1.0 M CH3COOH
0.1 M, 0.2 M and 1.0 M NaOH

Procedure

(A) Determination of pH of acidic and basic solutions

1. (a) Place 2 mL of the following solutions into separate

test tubes.

i. 0.01 M HCl
ii. 1.0 M HCl
iii. 0.1 M CH3COOH
iv. 1.0 M CH3COOH
v. 0.1 M NaOH
vi. 0.1 M NH3

Use pH paper to determine the pH of the solutions.

(b) Use a pH meter to determine the pH of the following

solutions:

i. 0.01 M HCl
ii. 1.0 M HCl
iii. 0.1 M CH3COOH
iv. 1.0 M CH3COOH

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2. Fill the test tubes with 2 mL of each of the following solution:

i. 0.01 M HCl
ii. 0.1 M CH3COOH
iii. 0.1 M NH3

Add two drops of methyl red to each test tube. Record the
observation. Determine the pH range by comparing the colour
of the solutions with the chart provided.

Repeat step 2 with methyl orange.

3. Fill the test tubes with 2 mL of each of the following solution:

i. 0.1 M NaOH
ii. 1.0 M NaOH
iii. 0.1 M NH3
iv. 1.0 M NH3

Add two drops of alizarin yellow to each test tube. Record the
observation. Determine the pH range by comparing the colour
of the solutions with the chart provided.

(B) Determination of pH of salt solutions

1. Fill the test tube with 2 mL of each of the following solution:

i. 0.1 M NaCl
ii. 0.1 M CH3COONa
iii. 0.1 M NH4NO3

Using pH paper and universal indicator, determine the pH and

state whether the salt solutions are acidic, basic or neutral.

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(C) Determination of the dissociation constant of a weak acid, Ka

1. Pipette 25 mL of 0.1 M CH3COOH into two conical flasks, X

and Y.

2. Add 2 - 3 drops of phenolphthalein into the conical flask X

and titrate it with 0.2 M NaOH. When the volume of base
reaches 10 mL, add the titrant drop by drop. The end point is
reached when the solution becomes pink. Record the initial
and the final readings of the burette.

3. Mix the solution in step 2 with 25 mL of 0.1 M CH3COOH in

the conical flask Y. Determine the pH of this mixture using a
pH meter.

4. Calculate Ka from the value of pH obtained in step 3.

POINT TO DISCUSS

1. Calculate the percentage of ionisation of 0.1 M and 1.0 M acetic acid.

How does the percentage of ionisation change with its concentration?

2. Refer to the pH value of acetic acid in Part (A). Calculate its Ka and
compare this value to that obtained from Part (C).

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DATA SHEET

EXPERIMENT 6: pH MEASUREMENT AND ITS APPLICATIONS

RESULT

(A) pH measurements of acid and base solutions

Indicator
Solution
pH pH Methyl Alizarin Methyl
paper meter red Yellow orange
0.01 M -
HCl
1.0 M - - -

0.1 M -
CH3COOH
1.0 M - - -

0.1 M - - -
NaOH
1.0 M - - - -

0.1 M -
NH3
1.0 M - - - -

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(B) pH measurements of salt solutions

Universal Acidic/ Basic/

Salt solution pH paper
Indicator Neutral

NaCl 0.1 M

CH3COONa 0.1 M

NH4NO3 0.1 M

(C) Dissociation constant of a weak acid, Ka

Burette reading / mL Data

Final reading

Initial reading

Volume of NaOH used / mL

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CHEMISTRY 2
SK025
 Chemistry Lab Manual – SK025

EXPERIMENT 1: RATE OF REACTION

Objectives

At the end of this lesson, students should be able to study the effect of
concentration, temperature, and catalyst on the reaction rate.

Introduction

The reaction rate is the change in concentration of the reactants or products

per unit time. The factors that influence the rate of reaction are
temperature, pressure, catalyst, size of particles and concentration of
reactants.

The rate of a reaction can be studied by observing the change in the

chemical or physical properties of species involved in the reaction. The
reaction rate is inversely proportional to the time of the reaction, i.e., the
faster the reaction occurs, the shorter is the time for the reaction to
complete.

Apparatus Chemical Reagents

Glass rod 0.1 M HCl
Water bath 10% MnSO4
Stopwatch 2.0 M H2 SO 4
Boiling tube 0.02 M KMnO4
Thermometer 0.2 M Na2S2O3
10 mL pipette 0.25 M H2C2O4
50 mL burette
10 mL measuring cylinder
100 mL conical flask
Laminated white paper with ‘X’ mark

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Procedure

(A) The effect of concentration on the reaction rate

1. Place 50 mL of 0.2 M sodium thiosulphate, Na2S2O3using a

burette into a 100 mL conical flask. Put the conical flask on the
white paper with ‘X’ mark.

2. Pipette 10 mL of 0.1 M HCl into the conical flask and

immediately start the stopwatch. Stir continuously with a glass
rod until the mark is no longer visible and record the time.

Note: The ‘X’ mark should be observed from the top of the
conical flask.

3. Repeat steps 1 till 2 with the addition of distilled water to the

sodium thiosulphate as instructed in Table 1.1.

Table 1.1
Concentration of reactant

Volume of Volume of 1
Volume of Concentration
distilled 0.1 M HCI Time
0.2 M Na2S2O3 of Na2S2O3 𝑡
water solution (s)
solution (mL) (M) (s-1)
(mL) (mL)
50.00 0.00 10.00
40.00 10.00 10.00
30.00 20.00 10.00
20.00 30.00 10.00
10.00 40.00 10.00

4. Calculate the concentration of the sodium thiosulphate solution

1
after the dilution and the value of 𝑡 .

1
5. Plot a graph of 𝑡 against the concentration of sodium
thiosulphate solution.

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7. Based on the graph, state the relationship between the

concentration of the sodium thiosulphate solution with time
and the rate of reaction.

(B) The effect of temperature and catalyst on the reaction rate

1. Label 4 boiling tubes as A1, A2, B1 and B2.

2. Place 10 mL of 0.25 M oxalic acid, H2C2O4 solution into boiling

tubes A1 and A2.

3. Fill boiling tubes B1 and B2 with 5 mL of 0.02 M KMnO4

solution. Then add 10 mL of 2.0 M H2SO4 solution to both tubes.

4. Add 5 drops of 10% MnSO4 solution to B2. Stir the mixture.

5. Place tubes A1 and B1 in a water bath at temperature of 30°C for

about 3 minutes.

6. While tube A1 is still in the water bath, pour the solutions from
tube B1 into tube A1. Start the stopwatch immediately.

7. Record the time taken for the mixture to turn colourless.

8. Repeat Steps 5 till 7 for tubes A2 and B2.

9. Follow Steps 2 till 7 for the temperatures of 35°C, 40°C and

50°C. Record yourresults in Table 1.2.

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Table 1.2
Effect of temperature and catalyst on reaction rate

Without catalyst MnSO4 With catalyst MnSO4

Temperature (A1 + B1) (A2 + B2)
(°C) 1 1
t (s) (s-1) t (s) (s-1)
𝑡 𝑡

30
35
40
50

1
10. Plot 𝑡 against the temperature for the mixture of (A1 + B1) and
(A2 + B2) solutions on the same graph.

11. Based on the graph, deduce the relationship between:

i. temperature and rate of reaction;

ii. catalyst and rate of reaction.

POINT TO DISCUSS

1. What is the function of the catalyst in the above reactions?

1
2. What does 𝑡 represent?

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EXPERIMENT 2: DETERMINING THE HEAT OF REACTION

Objectives

At the end of this lesson, students should be able to:

i. determine the heat capacity of a calorimeter; and
ii. determine the heat of neutralisation of HCl and NaOH.

Introduction

Heat released or absorbed during chemical reactions can be measured by

using a calorimeter. A calorimeter is a container that is thermally isolated
from the environment. Heat released by the chemical reaction, −q is absorbed
by the solution and the calorimeter.

−qrxn = qs + qc ….. (1)

where qs = heat absorbed by solution

qc = heat absorbed by calorimeter

The heat absorbed by a calorimeter is proportional to the change in

temperature. The proportionality constant, C, is known as the heat capacity
of a calorimeter. Heat capacity is defined as the amount of heat required to
increase the temperature of the calorimeter by 1°C.

qc = C∆T ….. (2)

For a solution, the heat absorbed is proportional to the mass of the

solution and the change in temperature. The constant, c, is known as the
specific heat capacity of solution per unit mass. The specific heat capacity
of a very dilute solution is equivalent to the specific heat capacity of
pure water, 4.18 J g−1 °C−1. The mass of the solution can be calculated by
assuming the density of the solution is the same as the density of water.

qs = mscs∆T ….. (3)

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Heat released can be determined by measuring the temperature before and

after the reaction:

−qrxn = CT + mscsT ….. (4)

where ∆T = final temperature of system – initial

temperature of system
ms = mass of solution
Cc = heat capacity of calorimeter
cs = specific heat capacity of solution

Apparatus Chemical Reagents

25 mL pipette 1.0 M HCl
100 mL beaker 1.0 M NaOH
Thermometer
Calorimeter or styrofoam cup

Procedure

(A) Determination of the heat capacity of a calorimeter

1. Set up a simple calorimeter as shown in Figure 2.1.

Figure 2.1
A simple calorimeter (Chang, 2005)

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2. Measure the temperature, T1, of an empty calorimeter.

3. Pipette 50 mL of distilled water into a 100 mL beaker.

4. Heat the beaker to a temperature between 50 − 60°C.

5. Pour the hot water into the calorimeter. Close the lid
immediately and measure the initial temperature of the hot
water, T2.

6. Observe the decrease in temperature every 10 seconds for 2

minutes. Record the temperature that remains constant, T3.

7. Determine the heat capacity of the calorimeter.

(B) Determination of the heat of neutralisation of 1.0 M HCl and 1.0 M

NaOH

1. Pipette 25 mL of 1.0 M NaOH solution into the calorimeter

and 25 mL of 1.0 M HCl solution into a beaker. Record the
initial temperature of each solution.

2. Without removing the thermometer, lift the lid slightly and

quickly pour the HClsolution into the calorimeter.

3. Quickly replace the lid of the calorimeter.

4. Stir the solution and record the maximum temperature reached.

5. Calculate the heat of neutralisation.

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DATA SHEET

EXPERIMENT 2: DETERMINING THE HEAT OF REACTION

RESULTS

(A) Determination of the heat capacity of a calorimeter

i. Temperature of calorimeter, T1 = ________ °C

ii. Initial temperature of the hot water used, T2 = ________ °C

Time
Interval (s) 10 20 30 40 50 60 70 80 90 100 110 120
Temperature
(°C)

iii. Constant temperature of water, T3 = ________ °C

iv. Mass of water (assume ρwater = 1.0 g/mL) = ________ g

(B) Determination of the heat of neutralisation of 1.0 M HCl and 1.0 M

NaOH

Initial temperature of HCl (°C) =

Initial temperature of NaOH (°C) =

Average initial temperature (°C) =

Maximum temperature (°C) =

T =

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EXPERIMENT 3: ELECTROCHEMICAL CELLS

Objectives

At the end of this lesson, students should be able to:

i. arrange Al, Zn, Mg, Fe and Cu in an electrochemical series; and
ii. determine the Faraday’s constant by electrolysis of CuSO4 solution.

Introduction

Electrochemistry is a study of the relationship between electricity and

chemistry. Generally, there are two types of electrochemical cells, namely
galvanic and electrolytic cells. A galvanic cell is an electrochemical cell in
which redox reaction occurs spontaneously to generate electricity. For a
galvanic cell, oxidation occurs at the anode and electrons flow to the
cathode where reduction occurs.

A standard reduction potential is defined as a reduction potential obtained

at a standard condition where the concentration of solution is 1.0 M, the
gas partial pressure is 1 atm and temperature is 25°C. The standard
reduction potential values are arranged in a certain order and the list is
known as the Standard Reduction Potential Table or the emf Series.

The potential difference between the two half cells in an electrochemical

cell is called cell potential. The cell potential or the cell voltage at the
standard condition can be written as:

E°cell = E°cathode − E°anode

The cell potential at non-standard condition can be calculated by using the

Nernst equation.
0.0592
Ecell = E°cell − log Q
𝑛

In this experiment, the cell potential is obtained from the voltmeter

reading. By inserting the value and the concentration of the electrolyte in
the Nernst equation, the standard cell potential, E°cell can be determined.

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An electrolytic cell uses electricity to produce chemical changes in an

electrolyte. The cell is made up of two electrodes connected to a battery
which functions as a source of direct current. During electrolysis, cations
are reduced at the cathode while anions are oxidised at the anode. The
amount of substance formed at each electrode can be predicted based on
Faraday’s first law.

Apparatus Chemical Reagents

Tons 0.1 M CuSO4
Ammeter 0.1 M ZnSO4
Hair dryer 0.1 M FeSO4
Voltmeter 0.1 M MgSO4
Stopwatch 0.1 M Al(NO3)3
Transformer Zinc strip
Sandpaper or abrasive cloth Copper strip
Crocodile clips Magnesium strip
50 mL beaker Aluminium strip
Analytical balance Carbon rod
Salt bridge Saturated KNO3 or KCl
50 mL measuring cylinder

Note:
1. Clean the electrodes with sandpaper or abrasive cloth before use.

2. Ensure that the filter paper to be used as salt bridge is completely soaked
insaturated KNO3 or KCl solution. Avoid handling the salt bridge with
bare hands.

Procedure

(A) Galvanic cell

1. Clean the metal strips with sandpaper or abrasive cloth.

2. Fill a 50 mL beaker with 35 mL of 0.1 M CuSO4 and the other

beaker with 35 mLof 0.1 M ZnSO4.

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3. Set up the apparatus as shown in Figure 3.1.

Zn Cu
Salt bridge

ZnSO4 CuSO4

Figure 3.1
Galvanic cell

4. Record the cell potential.

5. Repeat Steps 1 till 4 by replacing Zn2+/Zn half cell with a

(a) magnesium strip in 0.1 M MgSO4

(b) aluminium strip in 0.1 M Al(NO3)3
(c) iron strip in 0.1 M FeSO4
6. Arrange the metals in ascending order of strength as reducing
agents.

7. Verify the above order by calculating the standard reduction

potential, E°reduction of each electrode.

(B) Determination of Faraday’s constant

1. Clean a copper electrode with a piece of sandpaper or abrasive

cloth.

2. Weigh the copper electrode accurately.

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3. Set up apparatus as show in Figure 3.2. Fill a 50 mL beaker

with 35 mL 0.1 MCuSO4.

+ DC
−

Carbon Copper
(anode) (cathode
)

0.1 M CuSO4

Figure 3.2
An electrolytic cell

4. Complete the circuit by connecting the wires from each

electrode to the ammeter and transformer. Set the transformer to
supply the direct current with a voltage of 3 V.

5. Run the electrolysis for 15 minutes.

6. Record the ammeter reading and your observation of each

electrode.

7. Disconnect the circuit and record the exact time of electrolysis.

8. Dry the copper strip using a hair dryer.

9. Weigh again the copper strip.

10. Calculate the mass of copper deposited. Determine the

Faraday’s constant.

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DATA SHEET

EXPERIMENT 3: ELECTROCHEMICAL CELLS

RESULTS

(A) Galvanic cell

Galvanic Cell Cell Potential, Ecell (V)

(B) Determination of Faraday’s number

Electrode Observation
Cathode
Anode

Final mass of Cu electrode (g) =

Initial mass of Cu electrode (g) =
Mass of Cu deposited (g) =
Moles of Cu (mol) =
Ammeter reading (A) =
Time (s) =
Quantity of charge, Q (C) =

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EXPERIMENT 4: REACTIONS OF ALIPHATIC AND AROMATIC

HYDROCARBONS

Objectives

At the end of this lesson, students should be able to:

i. study the chemical properties of an alkane, alkene and arene; and
ii. differentiate an alkane from an alkene and arene.

Introduction

Hydrocarbons are organic compounds that contain only carbon and

hydrogen. Alkanes which are also known as paraffins are saturated
hydrocarbons. They do not contain double or triple bonds. Hence, alkanes
are relatively inert to chemical reactions.

Example of alkanes:

H H H
H C H H C C H
H H H
Methane Ethane Cyclohexane

Alkanes undergo free radical substitution reaction.

CH2Cl2
CH4 + Br2
uv
CH3 Br + HBr
Alkenes are unsaturated hydrocarbons with at least one double bond
between two carbonatoms.

Example of alkenes:

H2C CH2

Ethene Cyclohexene

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Alkenes undergo electrophilic addition reactions at the C=C bond. For

example, alkenes undergo hydrogenation and halogenation to form alkanes
and dihalides, respectively.

CH2Cl2
CH3CH CH2 + Br2 CH3CHCH3 + HBr

Br

Alkenes also react with potassium permanganate solution in two different

conditions:

a) In basic medium to form a diol.

H H
KMnO4, OH-
H2C CH2 H C C H
cold, dilute
OH OH

b) In hot acidic medium to form a carboxylic acid.

H3C CH3 O
KMnO4, H+
C C 2 CH3 C OH
Δ
H H

Arenes are aromatic hydrocarbons with stable molecular structures.

Example of aromatic hydrocarbons:

CH3

Toluene Naphthalene Anthracene

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Although arenes have a very high degree of unsaturation, they are

relatively inert towards all addition reactions except at a very high pressure
and temperature.

Ni
+ H2
high pressure, 200°C

Arenes undergo electrophilic aromatic substitution reactions in the

presence of a Lewis acid catalyst.

Br
FeBr3
+ Br2 + HBr

Apparatus Chemical Reagents

Dropper Toluene
Test tube Cyclohexane
Rubber band Cyclohexene
Labeling paper Dichloromethane
Test tube rack 0.01 M KMnO4
Black sugar paper (6 cm × 12 cm) 4% bromine in dichloromethane

Procedure

(A) Reaction with bromine in dichloromethane

1. Label 6 dry, clean test tubes, A to F.

2. Place 1 mL of cyclohexane in test tubes A and B, 1 mL of

cyclohexene in test tubes C and D, and 1 mL of toluene in test
tubes E and F.

3. Wrap test tubes A, C and E with black sugar papers.

4. Add 4 to 5 drops of 4% bromine in dichloromethane into each

test tube.

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5. Keep test tubes A, C and E in a dark place, and test tubes

B, D and F in the sunlight. Leave them for 15 minutes.

6. Record the observations.

(B) Oxidation with cold alkaline solution of KMnO4 (Baeyer’s Test)

1. Label dry, clean test tubes, G, H and I.

2. Place 1 mL each of cyclohexane, cyclohexene and toluene in

test tubes G, H and I, respectively.

3. Add a few drops of alkaline KMnO4 solution into each test tube
and shake.

4. Record the observations.

POINT TO DISCUSS

1. Write the mechanism for the reaction of cyclohexane with bromine.

2. State the function of sunlight in Part (B).

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DATA SHEET

EXPERIMENT 4: REACTIONS OF ALIPHATIC AND AROMATIC

HYDROCARBONS

RESULTS

Test Bromine in dichloromethane Oxidation with

alkaline KMnO4
Under sunlight In the dark (Baeyer’s test)
Hydrocarbons

Cyclohexane

Cyclohexene

Toluene

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EXPERIMENT 5: REACTIONS OF HYDROXY COMPOUNDS

Objectives

At the end of this lesson, students should be able to:

i. identify classes of alcohols; and
ii. study the chemical properties of alcohols and phenol.

Introduction

Alcohols are organic compounds containing hydroxyl group, −OH, as the

functional group.Alcohols can be classified into:

H H R
R C OH R C OH R C OH
H R R
Primary Secondary Tertiary
alcohol (1o) alcohol (2o ) alcohol (3o)

Lucas reagent, a mixture of concentrated hydrochloric acid and anhydrous

zinc chloride, can be used to differentiate the three classes of alcohols.
Tertiary alcohols turn cloudy or appear in two layers almost immediately.
Secondary alcohols turn cloudy within 5 to 10 minutes whereas primary
alcohols do not show any changes.

Alcohol can be oxidised to aldehyde, ketone or carboxylic acid. The product

formed depends on the class of alcohol used. Various oxidizing agent such
as KMnO4, Na2Cr2O7 and H2CrO4 can be used.

Phenol, an example of aromatic alcohol can be distinguished from aliphatic

alcohol through reactions with FeCl3 solution or bromine water.

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Apparatus Chemical Reagents

Stopper Ethanol
Dropper 1-Butanol
Test tube 2-Butanol
Stopwatch Alcohol X
Water bath Lucas reagent
10 mL measuring cylinder 2-Methyl-2-propanol
Concentrated H2SO4
0.04 M Na2Cr2O7
Glacial acetic acid
Phenol
Bromine water

Procedure

(A) Lucas test

1. Place approximately 1 mL of 1-butanol, 2-butanol, 2-methyl-2-

propanol, and alcohol X in 4 separate test tubes.

2. Add 2 mL of Lucas reagent into the test tube.

3. Stopper and shake the test tube.

Note: If no change occurs within 10 minutes, place the test tube

in a water bath at 70°C – 80°C

4. Record the observation and the time taken for the reaction to
occur.

5. Deduce the class of alcohol X.

(B) Oxidation

1. Place 5 mL of 0.04 M Na2Cr2O7 solution in 4 separate test tube.

2. Add 2 to 3 drops of concentrated H2SO4 to the Na2Cr2O7

solution in the fume cupboard.

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3. Add 3 drops of 1-butanol, 2-butanol, 2-methyl-2-propanol, and

alcohol X to each of the mixture accordingly and heat in a water
bath at 70°C – 80°C.

4. Record the colour change.

(C) Confirmatory test for phenol

1. Place approximately 1.0 ml of phenol solution in a test tube.

2. Add bromine water dropwise until precipitate is formed.

3. Record the observation.

Note: Carry out this test in a fume cupboard.

POINTS TO DISCUSS

1. Explain the formation of the two layers in the Lucas test.

2. Write the equations for all reactions.

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DATA SHEET

EXPERIMENT 5: REACTIONS OF HYDROXY COMPOUNDS

RESULTS

Observation
Hydroxy (B)
compound (A)
Oxidation with sodium
Lucas Test
dichromate

1-butanol

2-butanol

2-methyl-2-propanol

Unknown
(Alcohol X)

(C) Confirmatory test for phenol

Compound Observation

Phenol

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EXPERIMENT 6: ALDEHYDES AND KETONES

Objectives

At the end of this lesson, students should be able to differentiate between

aldehydes andketones using qualitative analysis:

Introduction

Aldehydes and ketones are organic compounds containing carbonyl group:

O

C
R OH

A carbonyl compound forms an orange or a yellow precipitate with Brady’s

reagent, 2,4-dinitrophenylhydrazine.

Aldehydes can be differentiated from ketones by using Fehling’s, Schiff’s, or

Tollens’ reagents. An aldehyde gives a positive result with the above
reagents whereas a ketone does not. The Iodoform test is used to determine
whether a carbonyl compound contains any methyl carbonyl structure. The
formation of a yellow precipitate indicates the presence of the methyl
carbonyl group, R C CH 3

Apparatus Chemical Reagents

Stopper Ethanal
Dropper Benzaldehyde
Test tube Propanone
Boiling tube Unknown Y
Water bath 5% NH3
themometer 10% NaOH
5 mL measuring cylinder 0.3 M AgNO3
2,4-dinitrophenylhydrazine
Fehling’s solution
I2 in KI solution

Note: Use distilled or ANALAR grade for propanone

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Procedure

(A) Brady’s test

1. Place approximately 1 mL of 2,4-dinitrophenylhydrazine into 4

separate test tubes.

2. Add 5 drops of ethanal, benzaldehyde, propanone, and unknown

Y into the 4 test tubes accordingly.

3. Shake the test tubes.

4. Observe the formation of a precipitate.

Note:
If there is no precipitate, add 2 mL of distilled water and heat it
in a water bath at 60 – 70°C.

(B) Fehling’s test

1. Place approximately 1 mL of ethanal, benzaldehyde,

propanone, and unknown Y in 4 separate test tubes.

2. Add 2 mL of Fehling’s solution in each test tube.

3. Shake the test tubes gently.

4. Heat the mixture in the hot water bath for 15 - 20 minutes.

5. Record the observations.

(C) Tollens’ test

1. Prepare Tollens’ reagent by adding one drop of 10% NaOH

to 2 mL of 0.3 MAgNO3 in a boiling tube.

2. Add 5% NH3 dropwise until the precipitate dissolves.

3. Place approximately 1 mL of ethanal, benzaldehyde,

propanone, and unknown Y in separate test tubes.

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4. Add 1 mL of Tollens’ reagent to each test tube and shake the

mixtures gently.

5. Allow the mixtures to stand for 3 minutes. If there is no

change, warm themixture in a water bath at 60 – 70°C for 5
minutes.

6. Record the observations.

(D) Iodoform test

1. Place 10 drops of I2 in KI solution into 3 mL of distilled water

in a boiling tube.

2. Add 5 drops of ethanal into the boiling tube and shake gently.

3. Add 10% NaOH to the boiling tube drop by drop until the
colour of the I2 fades.

4. Allow it to stand for 2 to 3 minutes. If no precipitate forms,

warm the boiling tubein a water bath at 60 – 70oC.

5. If the colour of I2 disappears, add more I2 in KI solution

until the colour of I2 isretained. Repeat Step 4.

6. Record the observations.

7. Repeat the above steps with benzaldehyde, propanone, and

unknown Y.

POINT TO DISCUSS

1. Deduce the structure of an unknown based on the following

observations:
(a) A yellow precipitate with 2,4-dinitrophenylhydrazine.
(b) Silver mirror formed with Tollens’ reagents.
(c) A yellow precipitate with a solution of iodine in sodium
hydroxide.

2. State the tests that show the reducing property of an aldehyde and a
ketone.

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DATA SHEET

EXPERIMENT 6: ALDEHYDES AND KETONES

RESULTS

Unknown
Test Ethanal Benzaldehyde Propanone
Y
Brady’s
test

Fehling’s
test

Tollens’
test

Iodoform
test

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 REFERENCES

Ali, R. (1995) Panduan Amali Kimia Asas, Kursus Pengajian Tinggi Fajar
Bakti, Selangor.

Baum, S.J., Sandwick, R.K. (1994) Laboratory Exercises in Organic and

Biological Chemistry. Prentice Hall. New Jersey. United States of
America.

Beran, J.A. (1996) A Study of Chemical and Physical Changes, 2nd

Edition. John Wiley & Sons Inc. United States of America.

Brown, T. E., LeMay, H. E., Bursten, B. E., Murphy, C., Woodward, P. &
Stoltzfus, M. E. (2018). Chemistry: The Central Science (14th ed.).
Pearson Education

Chang, R & Overby, J. (2019). Chemistry (13th ed.). McGraw-Hill. United

States of America.

Chemistry Department of University Malaya. (2001) Laboratory Manual

Organic Chemistry (SCES1220). Universiti Malaya. Malaysia.

Ritchie, R. (2000) Revise AS Chemistry. Letts Educational Ltd. United

States of America.

Seager, S.L., Slabaugh, M.R. (2000) Introductory Chemistry for Today, 4th
Edition. Thomson Learning. California. United States of America.

Silberberg, M. & Amateis, P. (2021). Chemistry: The Molecular Nature of

Matter and Change (9th ed.). McGraw-Hill

Stanley, A.J. et.al (2000) Discovering Chemistry : A Year-12 Chemistry

Text Book. Openbook Publishers. South Australia, Australia.

Universiti Teknologi Malaysia (2001) Amali Kimia Am, Jawatankuasa

Penerbitan dan Penulisan Fakulti Sains UTM. Penerbit UTM.
Malaysia.

Ware, G., Deretic, G. (1995) Senior Chemistry : Practical Manual,

Heinemann. Victoria.

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 ACKNOWLEDGEMENTS

The Matriculation Division, Ministry of Education Malaysia wish to thank

everyone who has contributed in shaping and writing this CHEMISTRY
LABORATORY MANUAL (13th Edition) for the Two Semester
Matriculation Programme. Special thanks go to those for their many
valuable suggestions and conscientiousness in completing this manual.

Dr. Hajah Rosnarizah binti Abdul Halim

Director of Matriculation Division

Haji Mohd Yusof bin Samad

Deputy Director of Matriculation Division (Academic)

Mohd Junaidi bin Abd Aziz

Senior Principal Assistant Director

Siti Warda binti Selamat

Assistant Director

Reviewers for the 13th Edition:

• Prof. Dr. Zanariah binti Abdullah, UM

• Prof. Dr. Rosiyah binti Yahya, UM
• Norasyikin binti Ismail @ Chik, KMK
• Wan Zai Azlin binti Wan Aziz, KMPh
• Byron MC Michael Kadum, KML
• Zuraidah binti Ahmad, KMJ
• Fara Nur Hani binti Musa, KMP
• Fauziah binti Ismail, KMPk
• Sariah binti Ali, KMM
• Noor Fatihah binti Zulkeply, KMNS
• Wan Syafinas binti Wan Salim, KMKK
• Nur Afiqah binti Rosali, KMKPh
• Ahmad Farid bin Yang Abd Talib, KMSw
• Azfa Ilhamuna binti Ahmad Badri, KMPP

Cover designed by Syed Nassir bin Syed Ahmad, KML

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SK015 & SK025