Chemistry Lab Manual

MATRICULATION DIVISION

CHEMISTRY

LABORATORY MANUAL
SEMESTER I & II
DK014 & DK024

FOURTH EDITION

MATRICULATION DIVISION
MINISTRY OF EDUCATION MALAYSIA

CHEMISTRY

LABORATORY MANUAL
SEMESTER I & II
DK014 & DK024

FOURTH EDITION

First Printing, 2011 (First Edition)
Second Printing, 2015 (Second Edition)
Third Printing, 2018 (Third Edition)
Fourth Printing, 2020 (Fourth Edition)
Copyright © 2020 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 : 603-88844083
Fax : 603-88844028
Website : http://www.moe.gov.my/v/BM

Printed in Malaysia by

Malaysia National Library
Chemistry Laboratory Manual
Semester I & II
DK014 & DK024
Fourth Edition

eISBN: 978-983-2604-39-6

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,
emotionally 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.



CONTENTS

Learning Outcomes Page
Introduction i

 Laboratory Safety iii - iv
 Preparation For Experiment v
 Report Writing vi

Semester I 1
Experiment Title 3
6
1 Determination Of The Density Of Water 9

2 Standard Solution And Determination Of The 13
Concentration Of Acid Solution. 16
19
3 Quantitative Analysis Of Baking Soda 21
4 Molecular Geometry
23
Semester II 24
Experiment Title

1 Qualitative Analysis Of Organic Compounds
2 Saturated And Unsaturated Hydrocarbon
3 Reactions Of Alcohols
4 Aldehydes And Ketones

References
Acknowledgements

DK014 & DK024 Lab Manual

1.0 Learning Outcomes
1.1 Matriculation Science Programme Educational Objectives
Upon a year of graduation from the programme, graduates are:
1. Knowledgeable and technically competent in science disciplines
in-line with higher educational institution requirement.
2. Able to communicate competently and collaborate effectively in group
work to compete in higher education environment.
3. Able to solve scientific and mathematical problems innovatively and
creatively.
4. Able to engage in life-long learning with strong commitment to
continue the acquisition of new knowledge and skills.

1.2 Matriculation Science Programme Learning Outcomes
At the end of the programme, students should be able to:
1. Acquire knowledge of science and mathematics fundamental in higher
level education.
(PEO 1, MQF LOD 1)
2. Demonstrate manipulative skills in laboratory work.
(PEO 1, MQF LOD 2)
3. Communicate competently and collaborate effectively in group work
with skills needed for admission in higher education institutions.
(PEO 2, MQF LOD 5)
4. Apply logical, analytical and critical thinking in scientific studies and
problem solving.
(PEO 3, MQF LOD 6)
5. Independently seek and share information related to science and
mathematics.
(PEO 4, MQF LOD 7)

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1.3 Course Learning Outcome
13.1 Chemistry 1
At the end of the course, student should be able to:

1. Explain basic concepts and principles of physical chemistry in
novel and real life situations.
(C2, PLO1, MQF LOD1)

2. Demonstrate the correct techniques in handling laboratory
apparatus and chemicals when carrying out experiments.
(P3, PLO2, MQF LOD2)

3. Solve chemistry related problems by applying the basic concepts
and Principles in physical chemistry.
(C3, PLO4, CTPS3, MQF LOD 6)

13.2 Chemistry 2
At the end of the course, student should be able to:

1. Explain basic concepts and principles of organic chemistry in
novel and real life situations.
(C2, PLO1, MQF LOD1)

2. Demonstrate the correct techniques in handling laboratory
apparatus and chemicals when carrying out experiments.
(P3, PLO2, MQF LOD2)

3. Solve chemistry related problems by applying the basic concepts and
principles in organic chemistry.
(PLO4, CTPS3, MQF LOD 6)

1.4 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.

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2.0 Laboratory Safety

The Science Matriculation Programme requires the students to attend practical classes
two hours a week to complete four 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.

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.

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.

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18. Wash all glasswares 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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3.0 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.

4.0 Preparation for experiment
4.1 Pre-lab Sessions.
i. Read and understand the objectives and the theory of the experiment.
ii. Think and plan the working procedures properly for the whole
experiment. Make sure you have appropriate table for the data.
iii. Complete and submit the pre-lab questions provided.

4.2 Practical Sessions
i. Check the apparatus provided.
ii. Conduct the experiment carefully.
iii. Record all measurements and observations made during the
experiment.
iv. Keep the work area clean and tidy.

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4.3 Post-lab Sessions
i. Explain what has been carried out and discuss the findings of the
experiment.
ii. Introduce the format of report writing as below:

Objective  state clearly
Theory
Procedure  write concisely in your own words
Results/  draw and label diagram if necessary
Observation
 write in passive sentences about all the
Discussion steps taken during the experiment

Conclusion  data tabulation with units and uncertainties
 data processing (plotting graph, calculation

to obtain the results of the experiments and
its uncertainties)

 give comments about the experimental
results by comparing it with the standard
value.

 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 the
objectives of the experiment

Reminder: NO PLAGIARISM IS ALLOWED.

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CHEMISTRY 1
DK014

DK014 & DK024 Lab Manual

EXPERIMENT 1 DETERMINATION OF THE DENSITY OF WATER

Course Learning Objective
Demonstrate the correct techniques in handling laboratory apparatus and chemicals when carrying
out experiments. (P3, PLO 2, MQF LOD 2)

Learning Outcomes
At the end of this lesson, students should be able to:
i. Determine the density of water.
ii. Compare the accuracy of the density of water using different apparatus.

Student Learning Time (SLT)

Face-to-face Non face-to-face
2 hour 0

Introduction

Density is defined as mass per unit volume. It is dependent on the temperature. When
temperature increases, the density decreases. Volume of a liquid is measured by using
pipette, measuring cylinder and burette. However, to get accurate volume measurement,
pipette and burette are most commonly used. A top loading balance and an analytical
balance is used to measure mass of a substance. A top loading balance and an analytical
balance give a reading of two and four decimal places respectively.

Apparatus

Burette
Glass rod
Filter funnel
Beaker (50 mL)
Pipette (10 mL)
Analytical balance
Top loading balance
Measuring cylinder (20 mL)

Procedure

1. Write a procedure on how to determine the density of 10 mL of water using the
apparatus provided.

2. Based on the procedure suggested, determine the density of water.

3. Compare the density of water obtained using different apparatus.

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DATA SHEET

EXPERIMENT 1 DETERMINATION OF THE DENSITY OF WATER

RESULTS

Temperature of water : _________________________
_________________________
Atmospheric pressure: _________________________

Volume of water :

Data Burette Pipette Measuring cylinder
Mass of empty beaker / g
Mass of beaker + water / g
Mass of water transferred / g
Density of water / g mL-1

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EXPERIMENT 2 STANDARD SOLUTION AND DETERMINATION OF THE
CONCENTRATION OF ACID SOLUTION.

Course Learning Objective

Demonstrate the correct techniques in handling laboratory apparatus and chemicals when carrying
out experiments. (P3, PLO 2, MQF LOD 2)

Learning Outcomes

At the end of this lesson, students should be able to:
i. Prepare a standard solution of sodium carbonate.
ii Determine the concentration of HCl solution using the standard solution of sodium

carbonate.

Student Learning Time (SLT)

Face-to-face Non face-to-face
2 hour 0

Introduction

A solution of known concentration is called a standard solution. Concentrations are usually
measured as molL-1 or gL-1. The concentration of a standard solution is often determined by
using a primary standard i.e. a substance that can be accurately weighed and is pure. In its
pure form, the number of moles present can be accurately determined from the measured
weight and its molar mass. In this experiment, pure sodium carbonate is used as a primary
standard to determine the concentration of hydrochloric acid, a secondary standard. 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.

Apparatus Chemical reagents

Burette Methyl orange
Spatula Distilled water
Glass rod Sodium carbonate, Na2CO3
White tile Hydrochloric acid solution, HCl
Retorts stand
Analytical balance
Conical flask (250 mL)
Pipette filler
Filter Funnel
Pipette (25 mL)
Volumetric flask (250 mL)

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Procedure

(A) Preparation of a standard solution
1. Weigh accurately 1.3000 - 1.3500 g of pure sodium carbonate, Na2CO3 , in a clean

dry 50 mL beaker.

2. Add approximately 20 mL of distilled water to dissolve the solid.
3. Carefully transfer the solution into a 250 mL volumetric flask by using a filter funnel.
4. Rinse the beaker with distilled water and pour it into the flask.
5. Add distilled water up to the graduated mark of the volumetric flask.
6. Stopper and shake the flask until the solution is homogeneous.
7. Calculate the concentration of this standard solution.

(B) Standardisation of hydrochloric acid solution
1. Rinse a clean pipette with Na2CO3 solution
2. Pipette 25 mL of Na2CO3 solution into a clean 250 mL conical flask.
3. Add 3 drops of methyl orange as an indicator in the Na2CO3 solution.
4. Rinse a clean burette with HCl solution.
5. Fill the burette with HCl solution. Ensure that no air bubbles are trapped at the tip.
6. Record the initial burette reading to 2 decimal places.
7. Place a piece of white tile underneath the flask.
8. Titrate the Na2CO3 solution with HCl solution. During titration control the stopcock

with your left hand while swirling the conical flask with your right hand.

9. For the first titration,dispense the HCl solution slowly until the yellow solution
changes to orange colour permanently. This is the end point.

10. Record the final reading. The difference between the final and initial reading is gross
volume.

11. Repeat the titration 3 times. In the subsequent titrations, dispense the solution
quickly up to a few milliliters from the end point. Titrate a drop at a time until the end
point is reached.

12. Calculate the concentration of HCl solution.

Precaution: Rinse the unreacted solution at the inner wall of the conical flask once a while
with distilled water to ensure all the solution reacted.

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DATA SHEET

EXPERIMENT 2 STANDARD SOLUTION AND DETERMINATION OF THE
CONCENTRATION OF ACID SOLUTION

RESULTS AND CALCULATIONS
(A) Preparation of a standard solution

i. Mass of Na2CO3 = ___________________

ii. Moles of Na2CO3 = ___________________

iii. Molarity of Na2CO3 = ___________________

(B) Standardisation of hydrochloric acid solution

Burette reading / mL Gross I II III
Final reading
Initial reading
Volume of HCl used

Average volume of HCl = ____________mL

Note: Exculde the gross reading in determining the average volume of HCl.

Calculate the molarity of HCl solution.

EXERCISE
Does the addition of water in the precaution step affect the result of the titration? Explain.

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EXPERIMENT 3 QUANTITATIVE ANALYSIS OF BAKING SODA

Course Learning Objective

Demonstrate the correct techniques in handling laboratory apparatus and chemicals when carrying
out experiments. (P3, PLO 2, MQF LOD 2)

Learning Outcomes

At the end of this lesson, students should be able to:
i. Determine the percentage of sodium hydrogen carbonate, NaHCO3, in baking soda

sample.
ii. Acquire the correct techniques of titration.

Student Learning Time (SLT)

Face-to-face Non face-to-face
2 hour 0

Introduction

Titration is a laboratory technique used to determine the concentration of a solution using
another solution with a known solution.

Titration also can be used to determine the percentage of the content in any sample of a
solution such as baking soda solution.

The acid - carbonate reaction is

NaHCO3 (aq) + HCl(aq)  NaCl(aq) + H2O(l) + CO2 (g)
The reaction can be used to determine the amount of acid that reacts with a known amount
of carbonate. The end point is determined using a suitable indicator.

Apparatus Chemical Reagents

Burette Baking soda
Spatula methyl orange
Glass rod Distilled water
White tile Hydrochloric acid solution, HCl (used the same
Retort stand HCl solution prepared in experiment 2
Analytical balance
Conical flask (250 mL)
Pipette filler
Filter Funnel
Pipette (25 mL)
Volumetric flask (250 mL)

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Procedure

1. Weigh accurately 1.4500 - 1.500 g of baking soda sample in a clean dry 50 mL
beaker.

2. Add approximately 20 mL of distilled water into a the beaker. Stir until all solids are
dissolved.

3. Pour the resulting solution into a 250 mL volumetric flask.

4. Rinse the beaker with distilled water and pour it into the flask.
5. Add distilled water up to the graduated mark of the volumetric flask.
6. Stopper and shake the flask until the solution is homogeneous.
7. Pipette 25 mL of this solution into a 250 mL conical flask. Add 2 drops of methyl

orange.
8. Titrate the solution with the standard HCl solution.
9. For the first titration, dispense the HCl solution slowly until the yellow solution

changes to orange colour permanently. This is the endpoint.

10. Record the final reading. The difference between the final and initial reading is gross
volume.

11. Repeat the titration 3 times. In the subsequent titrations, dispense the solution
quickly up to a few milliliters from the end point. Titrate a drop at a time until the end
point is reached.

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DATA SHEET

EXPERIMENT 3 QUANTITATIVE ANALYSIS OF BAKING SODA

RESULTS
(A) Analysis of baking soda sample

Mass of baking soda = _____________

Burette reading / mL Gross I II III
Final reading
Initial reading
Volume of HCl used

Average volume of HCl = _____________

CALCULATIONS

1. Calculate the number of mole of HCl needed to react with 25 mL of baking soda
solution.

2. The active constituent of baking soda is sodium hydrogen carbonate NaHCO3. Write
the equation of the reaction between NaHCO3 and HCl.

3. Calculate the number of moles of NaHCO3 in

a) 25 mL of the baking soda solution
b) The original solution in the volumetric flask

4. Calculate the mass of NaHCO3 in the original solution.
5. Calculate the % of NaHCO3 in baking soda.

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EXPERIMENT 4 MOLECULAR GEOMETRY

Course Learning Objective
Demonstrate the correct techniques in handling laboratory apparatus and chemicals when carrying
out experiments. (P3, PLO 2, MQF LOD 2)

Learning Outcomes
At the end of this lesson, students should be able to:
i. View molecules in 3-dimensional structure
ii. Determine the shape of molecules using the VSEPR theory

Student Learning Time (SLT)

Face-to-face Non face-to-face
2 hour 0

Introduction

The first step toward visualizing the structure of a molecule is to convert its molecular
formula to its Lewis structure. A Lewis structure is a 2-dimensional structural formula that
shows how the atoms are attached to each other within a molecule. It does not reveal the
overall shape.
The Valence Shell Electron Pair Repulsion (VSEPR) theory is used to determine the
geometry of a molecule. In the VSEPR theory, the repulsion between two pairs of electrons
(i.e. bonding pairs or lone pairs) in the valence shell is the dominant factor that determines
the geometry of a molecule. The electron pairs around the central atom are oriented as far
apart as possible to reduce the repulsion between them. In this case, the lone pairs repel
more strongly than the bonding pairs.
The geometry of a molecule is determined by the position of the terminal atoms that are
bonded to the central atom. The lone pairs will influence the bond angles but do not
contribute to the shape.

Apparatus

3–D molecular model set (2 students per set)

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Procedure

(A) Basic geometry
1. Using a 3-D model set, construct structures with the following geometry:
i. Linear
ii. Trigonal planar
iii. Tetrahedral
iv. Trigonal bipyramidal
v. Octahedral
2. Draw the structures in Table 4.1

3. Determine the bond angles and write the general formulae to represent the
molecules. Use the symbol A as the central atom and X as the terminal atom.

(B) Molecular geometry

1. Draw Lewis structures and construct the molecular model for the following
molecules:
i. CO2
ii. BH3
iii. CH4
iv. PF5
v. SF6

2. Draw and name the molecular geometry of each molecule in Table 4.2.

3. State the bond angle(s).

4. Write the general formula of each structure.

EXERCISE

1. What is the most important factor in determining the geometry of a molecule?
2. List down the steps to determine the molecular shape of a compound.

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DATA SHEET

EXPERIMENT 4 MOLECULAR GEOMETRY

TABLE 4.1 Basic geometrical drawings and bond angles

Molecular Geometry Bond Angle General Formula

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TABLE 4.2 Molecular geometry and bond angle for particular compounds

Compound Lewis Molecular Bond Angle General
Structure Geometry Formula

CO2

BH3

CH4

PF5

SF6

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CHEMISTRY 2
DK024

DK014 & DK024 Lab Manual

EXPERIMENT 1 QUALITATIVE ANALYSIS OF ORGANIC COMPOUNDS

Course Learning Objective

Demonstrate the correct techniques in handling laboratory apparatus and chemicals when carrying
out experiments. (P3, PLO 2, MQF LOD 2)

Learning Outcomes

At the end of this lesson, students should be able to identify the elements in organic
compounds.

Student Learning Time (SLT)

Face-to-face Non face-to-face
2 hour 0

Introduction

All organic compounds contain carbon and hydrogen. However, some organic compounds

may also contain elements such as nitrogen, sulphur, oxygen and halogen. The presence of

carbon and hydrogen can be determined by using the combustion process. When organic

compounds are burnt in excess oxygen, the carbon will change to carbon dioxide and the

hydrogen to water.

CxHy + y xCO2 + y
( x + ) O2 H2O

4 2

Other elements can be identified by heating the organic compounds with sodium or a
mixture of magnesium and sodium carbonate. These elements are converted into various
anions that can be further tested.

N, S, C1, Br, I Na or Mg/Na2CO3 CN-, S2-, Br -, I-
∆

The presence of nitrogen in the form of CN- can be tested by using either the biuret test or
Nessler’s reagent while the S2- ion can be tested using lead acetate solution.

Apparatus Chemical reagents
Beaker Urea
Spatula
Test tube Sugar
Water bath Albumin
Boiling tube
Delivery tube Egg yolk
Bunsen Burner Lime water
Test tube holder Solid KClO3
Filter paper strips 2.5 M NaOH
Analytical balance 0.1 M CuSO4
Measuring cylinder (10 mL) 1.0 M Pb(CH3COO)2
Red and blue litmus paper

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Procedure
(A) Determination of carbon and hydrogen in sugar

1. Mix 0.20 g of sugar with 0.25 g of KClO3 in a boiling tube.
2. Heat the mixture and pass the gas released through lime water using a delivery

tube.
3. Record the observations of lime water and at the mouth of the boiling tube

(B) Determination of nitrogen in urea and albumin
(a) Urea
1. Heat one spatula of urea in a boiling tube until it melts. Take a whiff to identify
the gas emitted.
2. Immediately test the gas emitted with a dampened red litmus paper.
3. Allow the urea to cool and add 2 mL of 2.5 M NaOH.
4. Stir the mixture and add 3 drops of 0.1 M CuSO4.
5. Record the observations.

(b) Albumin
1. Place 1 mL of albumin in a test tube.
2. Add 2 mL of 2.5 M NaOH.
3. Stir the mixture and add 3 drops of 0.1 M CuSO4.
4. Record the observations.

(C) Determination of sulphur in albumin and egg yolk
1. Place 3 mL of albumin in a boiling tube.
2. Add 5 mL of 2.5 M NaOH and stir the mixture.
3. Place the boiling tube in a water bath at 30 C for 2 minutes.
4. Add two drops of Pb(CH3COO)2 solution. Record your observations.
5. Repeat steps 1 to 4 using egg york.

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EXERCISE
1. State the function of KClO3.
2. Compare the sulphur content in albumin and egg yolk.

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EXPERIMENT 2 SATURATED AND UNSATURATED HYDROCARBON

Course Learning Objective

Demonstrate the correct techniques in handling laboratory apparatus and chemicals when carrying
out experiments. (P3, PLO 2, MQF LOD 2)

Learning Outcomes

At the end of this lesson, students should be able to:
i. Distinguish between saturated and unsaturated hydrocarbon.
ii. Study the chemical properties of alkanes and alkenes.

Student Learning Time (SLT)

Face-to-face Non face-to-face
2 hour 0

Introduction

Hydrocarbons are organic compounds that contain only carbon and hydrogen. These
hydrocarbons can be divided into saturated and unsaturated. Alkanes which are also known
as paraffin are saturated hydrocarbons. They do not contain double or triple bonds. Due to
this reason, alkanes are relatively inert to chemical reactions.

Alkenes contain at least one C-C double bong which makes them chemically reactive. They
can be distinguished from alkanes throughout a few reactions

Example of alkane

H HH
HC H HCCH

H HH

Methane Ethane Cyclohexane

Alkanes undergo only free radical substitution reaction.

uv CH3Br + HBr
CH4 + Br2

Example of alkene:

H2C CH2 Cyclohexene
Ethene

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Alkenes can easily undergo addition reactions at the C=C bond. For example, alkenes
undergo hydrogenation and halogenation to form alkanes and dihalides, respectively.
Alkenes also react with potassium permanganate solution in two different conditions:

(a) In basic medium to form a diol.

H2C CH2 KMnO4/OH- HH + MnO2
room temp HC CH (brown precipitate)

OH OH

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

H3C CH3 KMnO4/H+ 2 H3C O
C C C

H H OH

Apparatus Chemical reagents
White tile Cyclohexane
Dropper Cyclohexene
Test tube Dichloromethane
Water bath Alkaline KMnO4, 0.01 M
Rubber band 4 % bromine in dichloromethane
Wood splint
Labeling paper
Evaporating dish
Black sugar paper (6 x 12 cm)
Measuring cylinder

Procedure
(A) Combustion

1. Place 1 mL of cyclohexane and cyclohexene in two separate evaporating dishes.
2. Ignite both compound simultaneously with a burning wood splint.
3. Compare the colour intensity of the flame and the soot given off.
4. Record the observations.

(B) Solubility

1. Add approximately 1 mL of cyclohexane into a test tube containing 2 mL of
distilled water.

2. Stopper and shake the test tube. Record the observation.

3. Repeat steps 1-2 using cyclohexene.

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(C) Reaction with bromine in dichloromethane
1. Label 4 dry, clean test tubes, A to D.
2. Place 1 mL of cyclohexane in test tubes A and B, 1 mL of cyclohexene in test
tubes C and D.
3. Wrap test tubes A and C with black sugar papers.
4. Add 4 to 5 drops of 4% bromine in dichloromethane into each test tube.
5. Keep test tubes A and C in a dark place, and test tubes B and D in the sunlight.
Leave them for 10 minutes.
6. Record the observations.

(D) Baeyer’s Test
1. Place approximately 1 mL of cyclohexane into a test tube.
2. Add 5 drops of 0.01 M alkaline potassium permanganate, KMnO4.
3. Shake the test tube and allow the mixture to stand for 10 minutes. Record the
observations.
4. Repeat step 1-3 using cyclohexene.

EXERCISE

1. Write the mechanism for the reaction of cyclohexane with bromine in the presence
of ultra violet.

2. Explain the function of sunlight in Part (C).
3. Write all the equations involved.

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DK014 & DK024 Lab Manual

EXPERIMENT 3 REACTIONS OF ALCOHOLS

Course Learning Objective

Demonstrate the correct techniques in handling laboratory apparatus and chemicals when carrying
out experiments. (P3, PLO 2, MQF LOD 2)

Learning Outcomes

At the end of this lesson, students should be able to:
i. Classify alcohols.
ii. Study the chemical properties of alcohols.

Student Learning Time (SLT)

Face-to-face Non face-to-face
2 hour 0

Introduction

Alcohol is a class of organic compound containing hydroxyl group, -OH, as the functional
group. Alcohol can be classified as:

H H R
R C OH R C OH
R C OH [R = alkyl]
H R R

Primary alcohol (1o) Secondary alcohol (2o ) Tertiary 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 alcohol turns cloudy or
appears in two layers almost immediately, secondary alcohol reacts within 5 to 10 minutes
whereas primary alcohol reacts very slowly.

Alcohol can be oxidised to aldehyde, ketone or carboxylic acid. The product formed depends
on the class of alcohol used. Various oxidising agents such as KMnO4, Na2Cr2O7 and
H2CrO4 can be used. The reaction between alcohols and carboxylic acids will produce
esters.

Apparatus Chemical reagents
Stopper Ethanol
Dropper 1-Butanol
Test tube
Stopwatch 2-Butanol
Water bath Alcohol X
Measuring cylinder (10 mL)
Lucas reagent
2-Methyl-2-propanol
Concentrated H2SO4
Acidified KMnO4 0.01 M
Glacial acetic acid

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DK014 & DK024 Lab Manual

Procedure
(A) Lucas test

1. Place 1 mL of 2-methyl-2-propanol in a test tube.
2. Add 2 mL of Lucas reagent into the test tube.
3. Stopper and shake the test tube.
4. Record the observation and the time taken for the reaction to occur.
5. Repeat the above steps using 2-butanol, 1-butanol and alcohol X. If no change

occurs within 10 minutes, place the test tube in a water bath at 70 – 80 C.

(B) Oxidation
1. Place 5 mL of 0.01 M acidified KMnO4 solution in a test tube.
2. Add 2 to 3 drops of concentrated H2SO4 to the solution in the fume cupboard.
3. Add 3 drops of 1-butanol to the mixture and heat it in a water bath at 70 – 80 C.
4. Repeat the above steps using 2-butanol, 2-methyl-2-propanol and alcohol X.
5. Record the colour change.

(C) Esterification
1. Place 2 mL of ethanol in a dry test tube.
2. Add 1 mL of glacial acetic acid and 3 drops of concentrated H2SO4 to the ethanol
in the fume cupboard.
3. Shake the mixture and warm it in a water bath at 60 C for 5 to 10 minutes.
4. Add 3 mL of distilled water and take a whiff of the vapour released. Describe the
smell.

EXERCISE
1. Write the equations and explain the formation of the two layers in the Lucas test.
2. Write the equations for the reactions in Part (B) and Part (C).

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DK014 & DK024 Lab Manual

EXPERIMENT 4 ALDEHYDES AND KETONES

Course Learning Objective

Demonstrate the correct techniques in handling laboratory apparatus and chemicals when carrying
out experiments. (P3, PLO 2, MQF LOD 2)

Learning Outcomes

At the end of this lesson, students should be able to differentiate between an aldehydes and
a ketone using qualitative analysis

Student Learning Time (SLT)

Face-to-face Non face-to-face
2 hour 0

Introduction

Aldehydes and ketones are organic compounds containing carbonyl group,

O R is alkyl or H
RR

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.

Apparatus Chemical reagents
Stopper Ethanol
Dropper Propanone
Test tube Benzaldehyde
Water bath An unknown
Boiling tube
Thermometer 5 % NH3
10 % NaOH
0.3 M AgNO3
2,4-dinitrophenylhydrazine

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DK014 & DK024 Lab Manual

Procedure
(A) Brady’s test

1. Place approximately 1 mL of 2,4-dinitrophenylhydrazine into a test tube and add
5 drops of ethanal.

2. Shake the test tubes and heat it in a water bath at 60 – 70C. Observe the
formation of a precipitate.
Note: If there is no precipitate, add 2 mL of distilled water.

3. Repeat step 1 and 2 by replacing ethanal with benzaldehyde, propanone and an
unknown.

(B) Tollens’ test
1. Prepare Tollens’ reagent by adding one drop of 2.5 M NaOH to 2 mL of 0.3 M
AgNO3 in a boiling tube.

2. Add 5 % NH3 drop by drop until the precipitate dissolves.

3. Place approximately 1 mL of ethanal, benzaldehyde, propanone and an unknown
in 4 seperate test tube.

4. Divide equally the Tollen’s reagent from steps 1 and 2 to each test tube and
shake the mixtures gently.

5. Allow the mixtures to stand for 3 minutes and observe whether a silver mirror
forms in any of the test tubes.

6. If there is no change, warm the mixture in a water bath at 60 – 70 C for 5
minutes.

7. Record the observations.

EXERCISE

1. Deduce the class of compound of an unknown based on the following
observations:
a) A yellow precipitate with 2,4-dinitrophenylhydrazine.
b) No precipitates are formed with Tollens’ reagents.

2. Write the equations for the positive results of the test in part A and part B.

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REFER ENCES

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.

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.

Ryan, L. (1996) Chemistry for You, Stanley Thorpes (Publishers) Ltd. England.

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

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.

Chang, R. (2005) Chemistry, 8th Edition. MacGraw Hill. United States of
America.

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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 (4th Edition)
for the Two Year 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

Dr. Shah Jahan bin Assanarkutty
Deputy Director of Matriculation Division (Academic)

Mohd Junaidi bin Abd Aziz
Senior Principal Assistant Director

Reviewers for the 4th Edition: Universiti Malaya
Universiti Malaya
Prof. Dr. Zanariah binti Abdullah Kolej Matrikulasi Negeri Sembilan
Prof. Dr. Rosiyah binti Yahya Kolej Matrikulasi Johor
Rusiati binti Md. Som Kolej Matrikulasi Melaka
Salwana binti Md. Ali Kolej Matrikulasi Perak
Norzalina binti Maarof Kolej Matrikulasi Selangor
Hamisah binti Abu Rashid Kolej Matrikulasi Negeri Sembilan
Fauziah binti Abdullah Bahagian Matrikulasi KPM
Ramanurbaya binti Mansor Bahagian Matrikulasi KPM
Isharae bin Abdul Mosamad Bahagian Matrikulasi KPM
Izyan Izdihar binti Shaarani
Siti Warda binti Selamat

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