Semester September 2017

CONTENTS

Introduction 2
Laboratory Safety Guidelines 3

Safety Declaration From 6

Laboratory Report Format 7

Experiment 1 :

Determination of Reaction Heat 8

Experiment 2 :

Determination of Dissociation Constant for a Weak Acid using 11

Spectrophotometer

Experiment 3 :

Determination of Reaction Rate 18

Experiment 4 :

Determination of Initial Rates & Activation Energy of Iodine Clock 22

References 25

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 INTRODUCTION

This manual provides the laboratory guidelines, safety declaration form, lab report format and
experimental procedures for subject Physical Chemistry (CLB 10703). The manual also contains
specific instructions for completing the experiments and general information covering laboratory
conducts and safety rules.

Students are compulsory to read and understand all the laboratory guidelines provided in the manual.
The safety declaration form should be submitted to the lecturer/instructor before starting the
experiment works.

In the laboratory report format, there are report writing guidelines and requirements that should be
followed to produce a good quality of lab report.

Laboratory Jotter Notes are required for each of the experiment. In the jotter note, the basic
information of the experiment, the procedure and all primary data and observations during the
experiment should be clearly written. The jotter note has to be prepared BEFORE coming to the lab
and need to be verified by the lecturer/instructor BEFORE leaving the lab on the day of experiment.
Then the jotter note of each group member MUST be attached to the lab report during submission.

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 LABORATORY SAFETY GUIDELINES

General Guidelines

1. Conduct yourself in a responsible manner at all times in the laboratory.

2. Be familiar with your lab experiment before you come to the lab. Follow all written and
verbal instructions carefully. If you do not understand a direction or part of a procedure, ask
the lecturer/instructor before proceeding.
3. No student may work in the laboratory alone. The lab instructor/lecturer grants exceptions
on a case by case basis.
4. When first entering a laboratory, do not touch any equipment, chemicals or other materials
in the laboratory area until you are instructed to do so.
5. Do not eat, drink beverages or chew gum in the laboratory. Do not use laboratory glassware
as containers for food or beverages.
6. Smoking is strictly not allowed in any indoor area.
7. No music allowed in the laboratory.
8. No cellular phone is allowed in the laboratory.
9. Perform only those experiments authorized by the lecturer/instructor. Never do anything in
the laboratory that is not called for the laboratory procedures or by your lecture/instructor.
Carefully follow all instructions, both written and oral. Unauthorized experiments are
prohibited.
10. Observe good housekeeping practices. Work areas should be kept clean and tidy at all times.
11. Horseplay, practical jokes, and pranks are dangerous and prohibited.
12. Bring only your laboratory manual, worksheets and report to the work area. Other
materials (books, purses, backpacks, etc) should be stored in the cabinet.
13. Know the locations and operation procedures of all safety equipment including the first aid
kit, eyewash station, safety shower, spill kit and fire extinguisher.
14. Be alert and proceed with caution at all times in the laboratory. Notify the
lecturer/instructor immediately of any unsafe condition you observe.
15. Label and equipment instructions must be read carefully before use. Set up and use the
prescribed apparatus as directed in the laboratory instructions provided by your
lecturer/instructor.
16. Experiments must be personally monitored at all times. You will be assigned a laboratory
station at which to work. Do not wander around the room, distract other students or
interfere with laboratory experiments or others.

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17. Defeating safety devices or using equipment in a manner other than that which is intended
will be grounds for dismissal from the lab.

Clothing

1. Safety goggles and safety jacket must be worn whenever you work in lab.
2. Gloves should be worn whenever you use chemicals that cause skin irritations or need to
handle hot equipment.
3. Mask should be worn every time you prepare the chemicals.
4. Safety shoes and hard hat should be worn at all times while in the laboratory.
5. Dress properly during a laboratory activity.
6. Long hair, dangling jewellery and loose or baggy clothing are a hazard in the laboratory.
Long hair must be tied back and dangling jewellery and loose or baggy clothing must be
secured.
7. Sandal, open-toed shoes, high heels or shoes with holes in the sols will not be worn in the
lab.
8. Shorts and skirts are not permitted.
9. Instructor and laboratory assistant have a right dismiss to you from the laboratory if they
found that you are not wearing proper safety clothing.

Handling of Chemicals

1. Treat chemicals with respect and understand the chemicals you are using with Material
Safety Data Sheet (MSDS). The MSDS are available in the analytical room.
2. All chemicals in the laboratory are to be considered dangerous. Do not touch, taste or smell
any chemical unless specifically instructed to do so.
3. Check the label on chemical bottles before removing any of the contents. Take only much
chemical are you need. Smaller amounts often work better than larger amounts.
4. Label all containers and massing papers holding dry chemicals.
5. Never return unused chemicals to their original containers.
6. Never use mouth suction to fill a pipette. Use pipette bulb or pipette filler.
7. Acids must be handled with extreme care. Always add acids slowly to water, with slow
stirring and swirling, being careful of the heat produced, particularly with sulfuric acid.
8. Handle flammable hazardous liquid over a pan to contain spills. Never dispense flammable
liquids anywhere near a flame or source of heat.

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9. Never take chemicals or other materials from the laboratory area.
10. Take good care when transferring acids and other chemicals from one part of the laboratory
to another. Hold them securely and in the method demonstrated by the instructor as you
walk.
11. All wastes generated during the course of an experiment must be disposed of according to
the lab instructors directions.
12. Never mix chemicals in sink drains.
13. Sinks are to be used only for water and those solutions designated by the instructor.
14. Solid chemicals, metals, matches, filter paper, and all other insoluble materials are to be
disposed of in the proper waste containers, not in the sink.
15. Checks the label of all waste containers twice before adding your chemicals waste to the
container.
16. Cracked or broken glass should be placed in the special container for broken glass.
17. Keep hands away from your face, eyes, mouth and body while using chemicals. Wash your
hands with soap and water after performing all experiments.

Accidents and Injuries

1. Report any accidents (spill, breakage, etc) or injury (cut, burn, etc) to the instructor
immediately, no matter how trivial it may appear.
2. If you or your lab partners are hurt, immediately tell to the instructor.
3. If a chemical should splash in your eye(s), immediately flush with running water from the
eyewash station for at least 20 minutes. Notify the instructor immediately. Spills should be
cleaned up immediately.

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 SAFETY DECLARATION FORM

The Dean/Head of Campus

Universiti Kuala Lumpur
Malaysian Institute of Chemical and Bioengineering Technology
Lot 1988, Vendor City Industrial Area
Taboh Naning, 78000 Alor Gajah
Melaka.

Dear Sir,

SAFETY DECLARATION (Subject : PHYSICAL CHEMISTRY CLB 10703)

I................................................................................................
ID No ......... declare that I have read and understood the safety rules and
regulations in UniKL MICET. I hereby agree to abide by all the rules and regulations stated in the
safety guidelines.

2. I hereby understood the contents and will disciplinary action will be taken against me, if I do
not abide by the stated rules.

3. I am fully responsible for all my actions during laboratory sessions.

Thank you.

Yours faithfully,

.
Name:
Matrix No:
Date:

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 Laboratory Report Format

The lab report should be :

- In hand writing of all group members
- Legible and neat
- No spelling error
- Free from any plagiarism. Some of the data and observations might be similar from one group
to another, but the interpretation should not be written identically. Therefore, please avoid
copying another student lab report or otherwise all the involved parties will lose points or share
the total marks.

Contents of the lab report should be addressed to the items below :

Front Page Include the title of experiment, your name and ID No, your partners name and ID No
and the date of experiment.

Objective State the objectives of the experiment in point form.

Summary / Abstract Briefly review on the experiment as a whole including the results and
conclusion.

Introduction State the background or theory of the experiment.

Materials and Procedure Include list of chemicals and equipment used and the experimental
procedure.

Results and Discussion Summarize the data collection in tables, figures or plots form. After clearly
presenting results of the experiments, either as tables or figures, it is necessary to discuss the scientific
and technical reasons of those results. The discussion section of the report should be objective. The
results of the experiment should be interpreted and (where appropriate) compared with each other.

Conclusion and Recommendations - The conclusion should begin with a restatement of the results.
The results should be compared with literature values and theory whenever possible. Any error in the
results should be addressed, for example why a plot that according to theory; should be linear but the
plot is not. Any possible sources of error should be identified. Suggest recommendation (s) for the
improvement of the experiment.

Laboratory Question Answer all questions for each of the experiment.

References List down all the references in proper format.

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EXPERIMENT 1: DETERMINATION OF REACTION HEAT

Introduction

The energy involved in a chemical reaction is expressed in terms of the amounts of heat released or
absorbed during the reaction. This heat or reaction (H) is measured in kilojoules per mole. H of an
exothermic reaction (heat is released) has a negative sign; H of an endothermic reaction (heat is
absorbed) has a positive sign.

In this experiment, three related exothermic reactions involving sodium hydroxide (NaOH) has to be
studied. In the first reaction, solid NaOH will dissociate into water (H 2O). The heat produced by the
reaction (H1) is called the heat of NaOH solution. In the second reaction, an aqueous solution of
NaOH will react with an aqueous solution of hydrochloric acid (HCl). The heat of this reaction (H 2)
is called the heat of NaOH neutralization. In the third reaction, solid NaOH will be reacted with an
aqueous solution of HCl. This reaction is the combination of the both previous reactions. The solid
NaOH will dissociate into its ions as it dissolves in the acid solution before being neutralized by the
acid. Thus, the heat of the reaction (H 3) could be equal to (H1+ H2). By using the calculations of
data collection in the experiment, the additive nature of reaction heat might be verified.

Objective
a) To determine the enthalpy change (H) of three exothermic reactions.
b) To relates the three exothermic reactions with Hess Law.

Materials
1. Sodium Hydroxide (NaOH) solid
2. 1 M NaOH solution
3. 0.5 M and 1M Hydrochloric Acid (HCl)
4. Distilled water (H2O)

Equipment / Apparatus
1. Analytical Balance
2. Pipette 25 ml
3. Spatula
4. Thermometer
5. Erlenmeyer Flask 50 ml
6. Small Beaker
7. Glass Rod

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Procedure

Part A: Heat of NaOH Solution (Solid NaOH + Distilled water)

1. Pipette 25 ml of distilled water into a 50 ml Erlenmeyer flask and allow it reaches the room
temperature.
2. Measure the temperature of the distilled water in the Erlenmeyer flask and record the temperature
as Ti.
3. Use a spatula to weigh exactly 0.5 g of sodium hydroxide (NaOH).
4. Add the NaOH into the Erlenmeyer flask. Use a glass rod to stir the mixture until the NaOH has
completely dissolved. Observe the changes of the temperature in the flask while stirring. Record
the highest temperature as Tf.
5. Discard the solution. Rinse off the thermometer.

Part B: Heat of NaOH Neutralization (NaOH Solution + HCl Solution)

1. Pipette 25 ml of 1 M hydrochloric acid (HCl) into a 50 ml Erlenmeyer flask. Allow the acid to
stand until it reaches the room temperature. Record the temperature as Ti.
2. Add exactly 25 ml of 1 M NaOH solution into the flask. Stir using a glass rod and observe the
changes of the temperature. Record the highest temperature as Tf.
3. Discard the solution. Rinse off the thermometer.

Part C: Heat of NaOH Solution (Solid NaOH + HCl Solution)

1. Pipette 25 ml of 0.5 M HCl into a 50 ml Erlenmeyer flask. Allow it to stand until it reaches the
room temperature. Measure the temperature of the HCl solution in the flask and record as Ti.
2. Use a spatula to weigh exactly 0.5 g NaOH and transfer it into the Erlenmeyer flask.
3. Use a glass rod to stir the mixture until the NaOH has completely dissolved. Observe the changes
of the temperature in the flask while stirring.
4. Record the highest temperature as Tf.
5. Discard the solution. Rinse off the thermometer and keep it safely.

Observation and Data

State all the temperatures (Ti and Tf) obtain from Part A, Part B and Part C in a proper table.

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Calculation
Calculate the H1, H2 and H3 by using the data obtained.
[Specific heat capacity of water, swater = 4.184 J/g.C]

Part A: Heat of NaOH Solution (Solid NaOH + Distilled water)

1. Find the heat (q) absorbed by the water (released by the NaOH).
2. Find the heat (q) released per gram of NaOH.
3. Find the enthalpy change, H1 in kJ/mole.

Part B: Heat of NaOH Neutralization (NaOH Solution + HCl Solution)

1. Find the heat (q) produced by the reaction of NaOH solution and HCl solution.
2. Find the enthalpy change, H2 in kJ/mole.

Part C: Heat of NaOH Solution (Solid NaOH + HCl Solution)

1. Find the heat (q) absorbed by the HCl solution (released by the NaOH).
2. Find the heat (q) released per gram of NaOH.
3. Find the enthalpy change, H3 in kJ/mole.

Pre-lab Questions
1. Define the term calorimeter.
2. State the units of energy normally used to measure heat.
3. Explain the concept of Hess Law.

Post-lab Questions

1. Write all ionic equations for the three reactions in the experiment.
2. List down all possible sources of error in the experiment.

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EXPERIMENT 2: DETERMINATION OF DISSOCIATION CONSTANT FOR A WEAK ACID
USING SPECTROPHOTOMETER

Introduction

Methyl red (4-dimethylaminobenzene-2-carboxylic acid) is a commonly used indicator for acid-base

titrations. In this experiment, the visible absorption spectra of the acidic and basic forms of this
compound will be measured. Then, a series of buffered solutions of methyl red will be prepared at
known pH. By following the change in absorbance as a function of pH and the acid dissociation
constant, the pKa of the methyl red can be determined. Methyl red provides a particularly good system
in the study of acid-base equilibrium since [HMR] and [MR-] have strong absorption peaks in the
visible portion of the spectrum.

The equilibrium reaction of methyl red is shown as :

HMR + H2O MR- + H3O+

The equilibrium constant of methyl red is equal to the acid dissociation constant, Ka .
[H3O+][ MR-]
Ka =
[HMR]
It is convenient to use this equation in form of :-
[ MR-]
pKa = pH log
[HMR]

The pKa values can be determined by varying the pH of methyl red solutions and calculate the value
of [MR-]/[HMR]. Acetic acid-acetate is used as a buffer to control pH since the Ka value for acetic
acid is in the same range as the Ka value for methyl red. The absorption spectra of methyl red in acidic
and basic solutions are determined and two wavelengths are selected for analyzing mixtures of the two
forms. These two wavelengths, 1 and 2, are chosen because the acidic form has a very large
absorbance index compared with the basic form. Therefore a reverse situation is expected to take
place.

Several concentrations of HMR and MR- at different wavelength will be used to indicate the
absorbance values of the compounds. The absorption of light is governed by the Beer-Lambert Law
as follows :
A= bc
Where, A = absorbance
= molar absorptivity (L. cm-1. mol-1)
b = path length of the cell (cm)

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 c = concentration of the absorbing species (mol. L -1)
The absorption spectrum of HMR and MR - is shown in Figure 1. The curve shows the changes in the
spectrum for the system with the changes in the pH. The absorbance values of HMR and MR - cannot
be differentiated if the molar extinction of both is similar at certain wavelengths. The absorption for
the overall system will be constant if the concentration for both of the HMR and MR - is constant,
regardless of the concentration ratio. This point is known as the isosbestic point. This point is
identified as all the curves are intersected (Figure 1).

Figure 1: Changes in the absorption spectrum of HMR and MR- with pH

Objective
To measure the pKa value of the methyl red through its absorbance spectra as a function of pH.

Materials
1. Methyl Red Stock Solution (1000 ppm)
2. Ethanol (95 %)
3. Hydrochloric Acid, HCl (0.1 M)
4. Sodium Hydroxide, NaOH (1.0 M)
5. Sodium Acetate (0.2 M)
6. Acetic Acid (0.2 M)

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Equipment / Apparatus
1. Ultraviolet Visible Spectrophotometer with Sample cell (10 mm)
2. pH meter
3. Volumetric Flask (12 x 50 ml)
4. Pipette (1 ml, 5 ml and 10 ml)
5. Beaker (50 ml and 100 ml)
6. Dropper

Procedure

Part A: Preparation of Methyl Red Standard Solution

1. Pipette 5 ml of methyl red (MR) stock solution into a 100 ml volumetric flask.
2. Add 50 ml of Ethanol (95%) into the flask and dilute with distilled water until mark level.

Part B: Preparation of Methyl Red Acidic and Basic Solutions

i) Acidic Solution of Methyl Red (pH 1)

1. Pipette 6 ml of MR standard solution (from part A) into a 50 ml volumetric flask.
2. Add 10 ml of hydrochloric acid (0.1 M) into the flask.
3. Dilute the solution in the flask with distilled water until the mark level.
4. Check the pH of the solution by using a pH meter.
5. Label the pH of the solution and observe its colour.
6. Record the absorption spectrum for the solution in the wavelength range of 350-600 nm.

ii) Basic Solution of Methyl Red (pH 13)

1. Pipette 5 ml of MR standard solution into a 50 ml volumetric flask.
2. Add 10 ml of sodium hydroxide (1.0 M) into the flask.
3. Dilute the solution in the flask with distilled water until the mark level.
4. Check the pH of the solution by using a pH meter.
5. Label the pH of the solution and observe its colour.
6. Record the absorption spectrum for the solution in the wavelength range of 350-600 nm.

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Part C: Absorption Spectrum of Methyl Red at various pH
1. Prepare a series of methyl red standard solutions (A H) in 50 ml volumetric flask.
(Refer Table 1 below)
Table 1: The volume of the mixed solution

Volume of MR Volume of 0.2 M Volume of 0.2 M

Solution
standard solution (ml) acetic acid (ml) sodium acetate (ml)

A 6 12 8
B 6 10 10
C 6 8 12
D 6 6 14
E 6 4 16
F 6 3 17
G 6 2 18
H 6 1 19

2. Dilute the mixture in each volumetric flask with distilled water until the mark level.
3. Shake the volumetric flasks and measure pH of the standard solutions by using a pH meter.
4. After that, the lab instructor will brief on the standard operating procedure of Ultraviolet Visible
Spectrophotometer. Perform the wavelengths scan for all solutions including the acidic and basic
solutions of methyl red (from Part B).
5. Record the absorption spectrum for each solution on a different paper. Recording should be
carried out immediately after preparing the solutions.

**REMINDER The accuracy of volume measurements for each solution is VERY IMPORTANT during the
preparation.

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Observation and Data

1. From the UV Vis Spectrophotometer Spectrum, record data required by the Table 2 below.

Table 2 : Absorbance of all solutions at various wavelength

Absorbance at wavelength
Solution
350 nm 375 nm 400 nm 600 nm
Acidic
A
B

H
Basic

Then, plot a graph of absorbance values against the wavelength for the acidic and basic solutions
of methyl red and solution A-H. Determine the isosbestic point and the wavelength where the
maximum absorption occurs on the left and right of the isosbestic point.

2. Determine the absorbance value at maximum wavelength ( max) for all solutions and record it in
Table 3 below.
Table 3 : pH and absorbance of all solutions
Solution pH Absorbance at max
Acidic
A
B

H
Basic

Plot a graph of absorbance at max against pH for the respective solutions. The graph obtain will
have the shape as in Figure 2. Draw a straight line corresponding to the absorption at pH 1 (Line
I) and pH 13 (Line II).

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 Figure 2: Graph of Absorbance (at maximum wavelength) against pH

3. Calculate concentration of [MR-] and [HMR] for each solution by using the following formula.

[MR-] = Abs at max of Solution X Abs at max of Basic Solution

[HMR] = Abs at max of Acidic Solution Abs at max of Solution X

Record the data in the table below.

Table 4 : Concentration of [MR-] and [HMR] for each solution.
Absorbance
Solution pH [MR-] [HMR] log [MR-]/[HMR]
at max
Acidic
A

H
Basic

Then, plot a graph of log [MR -]/[HMR] against pH of the solutions. The intersection point at the
X-axis is where the methyl red concentration in the acidic medium is the same as the
concentration in the basic medium. At the pH where the intersection occurs, determine the pKa
value of the methyl red.

Pre-lab Questions
1. Define pKa. Differentiate between pKa and pH.
2. Describe about max.

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Pre-lab Questions
1. Discuss the straight line in the graph of log [MR-]/[HMR] against pH.
2. Calculate pH of the prepared buffer solution (please use one example from any of the solutions).
Compare the calculated pH value with the true pH that measured by pH meter.
3. Discuss the weakness of the experiment.

EXPERIMENT 3: DETERMINATION OF REACTION RATE

Introduction

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Chemical kinetics is the area of chemistry concerned with the speeds or rates of a chemical reaction.
Kinetics refers to the reaction rate which is the change in the concentration of a reactant or a product
with time (M/s). Knowledge of reaction rates is useful in drug design, in pollution control and in food
processing. Industrial chemists often place more emphasis on speeding up the rate of a reaction rather
than on maximizing its yield.

The reaction can be represented by the general equation.

Reactants Products

From the equation, the reactants are consumed while products are formed. As a result, the progress of
a reaction is obtained by monitoring the concentration of the products. Besides, the temperature,
catalyst and physical state of a reaction also affects the rate of chemical reaction.

Chemical reactions occur at different rates. In this experiment, some of the key factors that influence
the rate of a reaction will be considered; there are temperature, concentration and catalysts. According
to the collision theory, the rate of a reaction depends on the frequency of collisions between reacting
particles. The more frequent the collisions in a reaction, the higher the rate will be.

However, in order for the collisions to be effective, the particles must collide with sufficient energy
(activation energy). Furthermore, the particles must collide with the proper orientation. The factors
that will be examined in this lab influence reaction rate by either increasing how often collisions occur
or by making collisions more effective.

Objective
To determine the effects of concentration, temperature and catalyst on reaction rate.

Materials
Part A: Effect of Concentration on Reaction Rate
1. Sodium thiosulphate, Na2S2O3 (0.15 M)
2. Hydrochloric Acid, HCl (6 M)
3. Distilled water

Part B: Effect of Temperature and Catalyst on Reaction Rate

1. Oxalic acid, H2C2O4 (0.25 M)
2. Potassium Permanganate, KMnO4 (0.02 M)

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 3. Sulfuric acid, H2SO4 (2 M)
4. Manganese (II) sulphate, MnO2 (10 %)
5. Distilled water

Equipment
Part A: Effect of Concentration on Reaction Rate
1. Beaker 250 ml
2. Stirring rod / Glass rod
3. Pipette 10 ml & 50 ml
4. Timer / Stopwatch
5. White paper

Part B: Effect of Temperature and Catalyst on Reaction Rate

1. Beaker 250 ml
2. Test tube (20 test tubes per group)
3. Water bath set - 30C, 40C, 50C, 60C and 70C
4. Timer / Stopwatch
5. Thermometer
6. Wooden tong

Procedure

Part A: Effect of Concentration on Reaction Rate

1. Obtain five 250 ml beakers and label each of the beakers accordingly.
2. Add sodium thiosulphate solution and distilled water to each beaker. Refer Table 5 below.

Table 5 : The composition of Na2S2O3 solution and distilled water for beaker 1-5

Beaker No. Volume of Na2S2O3 solution (ml) Volume of distilled water (ml)

1 25 0

2 20 5

3 15 10

4 10 15

5 5 20
* Note : The total volume in each of the beaker is 25 ml.
3. On a sheet of white paper, draw a small X mark with a marker. Place beaker 1 over the X
mark. Add 5 ml of HCl solution into the beaker and start the timer once the acid touches the
sodium thiosulphate solution. Stir the mixture at a constant rate throughout the reaction.

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4. Stop the timer when the X mark under the beaker is no longer visible through the solution.
Record the time in a proper table. Repeat step 3 for beaker 2, 3, 4 and 5.

Part B: Effect of Temperature and Catalyst on Reaction Rate

1. Obtain 20 test tubes and label the test tubes with A1 (5 test tubes), A2 (5 test tubes), B1 (5 test
tubes) and B2 (5 test tubes). Add oxalic acid solution, sulphuric acid solution, manganese (II)
sulphate and potassium permanganate solution into the test tubes as in Table 6.

Table 6: The amount of chemicals in each test tube

T/C Test Tube Volume of Volume of Volume of Volume of
H2C2O4 H2SO4 KMnO4 MnSO4
(ml) (ml) (ml)

A1 10
A2 10
30
B1 10 5
B2 10 5 5 drops
A1 10
A2 10
40
B1 10 5
B2 10 5 5 drops
A1 10
A2 10
50
B1 10 5
B2 10 5 5 drops
A1 10
A2 10
60
B1 10 5
B2 10 5 5 drops
A1 10
A2 10
70
B1 10 5
B2 10 5 5 drops

2. Stir the mixture in test tube B1 and B2 with glass rod.

3. Heat the test tubes A1 and B1 in the water bath at the temperature of 30C, 40C, 50C, 60C and
70C.

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4. Measure the temperature in test tube A1 and B1. Continue heating until the temperature of the
test tubes are exactly the same as the temperature of the water bath.
5. After that, transfer solution in test tube A1 into the test tube B1.
6. Start the timer once the reaction begins until the solution become colourless while stirring.
Record the time in a proper table.
7. Repeat steps 3 6 for test tube A2 and B2 for each water bath.

**REMINDER - Concentrated HCl solution will burn skin or damage clothing; AVOID skin contact with the
acid. Reaction should be carried out in a fume cupboard because some poisonous SO 2 gas is produced. Students
should be cautioned against leaning over the reaction vessel too closely as they observe the X mark under the
beaker. LAB SAFETY MASK and GOGGLES should be worn throughout the experiment.

Observation and Data

1. For Part A, plot a graph of reaction rate (per time, s -1) on the y-axis against volume of sodium
thiosulphate stock solution (in ml) on the x-axis.
2. For Part B, plot two graphs of reaction rate (per time, s -1) for samples without catalyst and
samples with catalyst on the y-axis against temperature of the mixture (in C) on the x-axis.
Compare the graphs.

Pre-lab Questions

1. Define reaction rate by giving an appropriate example.

2. State all factors that will influence reaction rate.

Post-lab Questions

1. Explain the relationship between volume of sodium thiosulphate solution and time of reaction.
State the trend of the reaction rate.
2. Explain the effects of temperature on the reaction time and the reaction rate.
3. Name the catalyst used in the experiment. Describe the functions.

EXPERIMENT 4: DETERMINATION OF INITIAL RATE AND ACTIVATION ENERGY

FOR IODINE CLOCK

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Introduction
Peroxydisulphate ions (or persulphate) are powerful oxidizing agents, and react with iodide ions to
form iodine via the overall reaction:
S2O82- + 2I- 2SO42- + I2
The rate of reaction is dependent on the concentrations of the peroxydisulphate and iodide ions. If the
concentration of iodide is higher than peroxydisulphate, the concentration of iodide will hardly change
during the experiment. The reaction rate will then appear to depend only on the concentration of
peroxydisulphate ions. The rate law is written as follows:-

d[S2O82- ]
k '[S2O2-8 ] ........... (1)
dt

Where k , which includes any dependence on iodide concentration, is known as the pseudo first
order rate constant for the reaction. Consider such an experiment, where the iodide ion concentration
is in excess. Suppose that the initial concentration of S 2O8 - is ao and that by time is has fallen to a.
2-
[S2O8 ]
a t

a 0 [S2 O8 ]
k ' dt
0
2-
........... (2)

Integration of this equation leads to:

a0 ........... (3)
ln k' t
a

In principle, the change in concentration of S 2O82- with time can be monitored. Then the rate constant
can be calculated. The rate constant is not directly measured, but it use an indicator to show how fast
the reaction is proceeding. Suppose that is the time taken for a fraction of the S2O82- to be used up.
i.e. the concentration of S2O82- will fall from aO to aO (1- ). Substitution into Equation (3) gives:

........... (4)

The rate constant is inversely proportional to the time for a fraction of the reaction to occur. Thus
by varying the reaction condition (e.g. temperature) and monitoring the time taken for a fixed amount
of peroxydisulphate to react, the rate constant changes can be determined.

The rate constant (k) for any reaction varies with absolute temperature (T) according to Arrhenius
Equation:

........... (5)

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 ........... (6)

Where E is the activation energy of the reaction, R is the molar gas constant (8.314 J/mol.K) and A is
known as the A-factor, which is related to the frequency of collision between the reacting molecules.
Remember that k is proportional to 1/ , so if the Arrhenius Equation holds, a plot of ln 1/ against 1/T
will give a straight line of slope (E/R), from which E may be readily determined.

Materials
1. 0.2 M Potassium Iodide (KI)
2. 0.05 M Sodium Thiosulphate (Na2S2O3)
3. 0.1 M Potassium Peroxydisulphate (K2S2O8)
4. Iodine Indicator
5. Beaker
6. Pipette
7. Test Tube (10 test tubes)
8. Water Bath (set at 30C, 40C, 50C, 60C and 70C)
9. Thermometer
10. Glass rod
11. Wooden tong

Procedure

1. Part A : Obtain five test tubes and label them as A-30C, A-40C, A-50C, A-60C and A-70C.
Pipette 5 ml of 0.05 M sodium thiosulphate (Na 2S2O3) and 10 ml of 0.2 M potassium iodide (KI)
into each of the test tube.
2. Part B : Obtain another five test tubes and label them as B-30C, B-40C, B-50C, B-60C and
B-70C. Pipette 10 ml of 0.1 M potassium peroxydisulphate (K 2S2O8) and 5 drops of iodine
indicator in each of the test tube.

3. Heat all the test tubes (from part A and B) in the respective water baths. Allow the contents of the
test tubes to reach the temperature of the water bath. Use a thermometer to monitor the
temperature. (Note: Do not transfer the thermometer from one test tube to the other or it will be
contaminated.)

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4. Pour the contents of test tube in Part A into the test tube in Part B once the temperatures reached
the point. Start the timer immediately after mixing. Stir the mixture using glass rod until the
colourless solution turn to dark yellow. Record the time in a proper table.

Observation and Data

1. Plot a graph of ln 1/ against 1/T (T is absolute temperature). Calculate the activation energy (E)
for the reaction.

Pre-lab Questions
1. Define the terms below :
a) Initial rate
b) Activation energy
2. Explain the purpose of using water baths in this experiment.

Post-lab Questions
1. Discuss the methodology needs to remain the iodide concentration. Use evidence from the
experimental method as well as the obtained results to justify the argument.

References

1. Monk, P., (2004), Physical Chemistry, John Wiley & Sons.

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 2. Chang, R., (2000), Physical Chemistry for Chemical and Biological Science, University
Science Book.
3. Atkins, P. and De Paula, J., (2006), Physical Chemistry, 1st Edition, Oxford University
Press.
4. Ball, D. W, (2003), Physical Chemistry, Pacific Grove, Thomson Brook/Cole.
5. Steven, B., (1970), Chemical Kinetics, Chapman Hall.
6. Smith, J. M., (1981), Chemical engineering Kinetics, 3rd Edition, MacGraw Hill.
7. Ramette, R. W., (1981), Chemical Equilibrium and Analysis, Addison-Wesley, Reading, MA.
8. Masterton, W., Slowinski, E., and Walford, E., (1980), Chemistry in the Lab, Rinehart and
Winston, New York.

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