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LABORATORY MANUAL
SKF1013
INTRODUCTION TO PHYSICAL CHEMISTRY
Department of Chemistry
Faculty of Science and Mathematics
UNIVERSITI PENDIDIKAN SULTAN IDRIS
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SKF1013: Introduction to Physical Chemistry
No Experiment Pages
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SKF1013: Introduction to Physical Chemistry
1. DO NOT ENTER the laboratory without the permission of the laboratory instructor.
2. All bags should be placed on the rack provided. All gadgets (handphone, tablet, etc) are
NOT ALLOWED during experiments.
3. Please wear a proper attire to work in the lab (Short pants, short skirt, “purdah”,
sleeveless shirt are not permitted).
4. Wearing jewellery is not permitted in the laboratory.
5. Long hair and scarf must be properly manageable.
6. DO NOT wear contact lenses.
7. Wearing personal protection equipment (PPE) is compulsory in laboratory such as lab
coat, cover shoes and safety glasses, gloves and etc.
8. Student are NOT ALLOWED to smoke, drink, eat, play around and run in laboratory
9. Know the location of all safety equipment.
10. No experiment can be performed without the permission of the laboratory instructor.
11. Read the label on the container of a chemical twice to make sure you are using the right
chemicals. Follow the instructions properly. DO NOT waste chemicals. Use required
amount only.
12. DO NOT contaminate chemicals. Once chemical has been removed from their
containers, DO NOT put it back into the stock container.
13. DO NOT use cracked or chipped glassware.
14. NEVER use mouth suction when using a pipette. Use a pipette filler/bulb.
15. DO NOT leave any heating, vigorous or rapid reaction unattended.
16. Always use fume hood when working with flammable organic compounds, strong acid
and base, volatile solvent, corrosive and toxic materials.
17. DO NOT heat flammable materials directly.
18. Make sure your surrounding is safe before using Bunsen burner.
19. While heating chemicals in test tubes, NEVER point the tubes to yourself or others.
20. Waste chemicals must be disposed properly by placing them in waste container
provided. Ask your instructor how to discard used reagents.
21. Broken apparatus, water and gas leakage must be reported to laboratory assistant on
duty immediately.
22. In case on fire or hearing emergency siren, evacuate the laboratory quickly in orderly
manner. In case of small accident or small fire occurs, try to overcome them wisely.
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SKF1013: Introduction to Physical Chemistry
23. Report any accidents (minor or major) to your laboratory instructor. This accident must
be recorded in log book “CATATAN KEMALANGAN”.
24. Clean all glassware and place them appropriately before leaving laboratory. Make sure
to switch off instruments, water and gas supplies.
25. Final year project students should require permission from supervisor and head of
department if they want to work after normal working hours.
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SKF1013: Introduction to Physical Chemistry
OBJECTIVE
State the objective clearly in a complete sentence. A few explanatory sentences may be
included, if needed.
The objective should answer the question: What is the lab objective designed to determine?
EXPERIMENTAL PROCEDURE
The experimental methods should give a detailed description in your own words of how YOU
accomplished the experimentation (Passive voice sentences).
*Tips: This should include equipment used in the experiment as well as how it was used. The
description should have sufficient detail so that another experimenter could duplicate your
efforts.
Use sketches and diagrams to describe the experimental set-up. Label the main components.
Tips: Any information copied directly from Lab manuals or other references should be stated
within quotes and referred, otherwise, it is considered plagiarism.
CONCLUSIONS
State your discoveries, judgments and opinions from the results of this experiment and relate it
with your experiment objectives. Suggest ways to improve the results of this experiment.
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SKF1013: Introduction to Physical Chemistry
REFERENCES
List the book, publication or website that you referenced in writing your report. Provide authors,
publisher, date of publication, page number, etc.
*Tips: Follow the standard format for typing a reference:
[1] Little, P., and Cardenas, M., “Use of Studio Methods in the Introductory Engineering
Design Curriculum,” Journal of Engineering Education, Vol. 90, No. 3, 2001, pp. 309-318.
[2] Nunally, J., Psychometric Theory, 2nd ed., New York, N.Y.: McGraw-Hill, 1978.
[3] Lister, B., “Next Generation Studio: A New Model for Interactive Learning,”
www.ciue.rpi.edu/pdfs/nextGenStudio.pdf.
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SKF1013: Introduction to Physical Chemistry
EXPERIMENT 1
FACTORS AFFECTING THE RATE OF A REACTION
1.1 OBJECTIVE
Upon completion of this experiment, students should be able to:
1. determine factors that affecting the rate of reaction
1.2 INTRODUCTION
There are several factors that affect the rate of a reaction. Some of these factors are:
• Mixing
• Concentration of a reactant
• Temperature
• The presence of a catalyst
• Surface area in a heterogeneous reaction
In this experiment we will examine these factors. This experiment is an introduction to the more
commonly encountered factors that affect the rate of reactions. There are other factors that
influence the rate of a reaction such as light, molecular geometry and the type of solvent used;
however, we do not have the time to explore all factors that affect reaction rate.
Chemicals
Potassium permanganate
Starch (as an indicator)
Acetic acid
Potassium iodide
Sodium thiosulfate
3wt% Hydrogen peroxide solution (H2O2)
3 M Copper (II) nitrate and 1M Copper (II) nitrate
3 M Iron (III) nitrate
Deionized water
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SKF1013: Introduction to Physical Chemistry
Apparatus
Test tubes
Beaker
Stop watch
Water bath
Glass rod
Gas collection set up (Conical flask, stopper and tube)
Iron nail
Ball of steel wool
1.3 PROCEDURE
Part A: The effect of mixing
1. Fill two (2) test tubes ¼ full with water.
2. Add a small crystal of solid potassium permanganate into each test tube.
3. Swirl one of the test tube to dissolve the potassium permanganate. Let the other test
tube undisturbed.
Record the time needed to dissolve the sample (form a solution).
4. Observe the undisturbed tube every 5 minutes while continuing with the next experiment
(Part B - E). Record the time needed for the potassium permanganate to dissolve
and diffuse throughout this tube.
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SKF1013: Introduction to Physical Chemistry
4. Repeat steps 2 and 3 using 5.0 mL of solution A and a mixture of solution (4.0 mL of
deionized water + 1.0 mL of the hydrogen peroxide).
Part C: The effect of temperature.
1. Prepare a test tube containing 5.0 mL of solution A and another test tube containing 4.0
mL of deionized water combined with 1.0 mL of the 3 wt% hydrogen peroxide solution.
Place both test tubes into a warm water bath for about 5 minutes.
2. Measure the temperature of the water bath.
3. Mix the two solutions into a small beaker and start your timer.
4. Record the time needed (in sec) for the solution to turn blue/black.
5. Compare the time needed in this experiment with the experiment in part B.
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SKF1013: Introduction to Physical Chemistry
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SKF1013: Introduction to Physical Chemistry
1.5 QUESTIONS
1. Looking at part A of this experiment, how would you expect the rate of the reaction to
change if you were to stir a reaction mixture instead of just letting it sit?
2. Recall that the rate of the reaction is inversely proportional to the time measured.
a. Based on this, in part B, which tube had a higher rate of reaction?
b. Which tube had the higher concentrations of either or both reactants?
c. How does concentration affect the rate of the reaction?
3. In part C of this experiment the temperature was raised above that used in part B.
Comparing the rate of the reaction in the second part of part B and the rate of the
reaction in part C, how does temperature affect the rate of the reaction?
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SKF1013: Introduction to Physical Chemistry
4. a. In part D of this experiment how did the presence of the copper (II) nitrate affect the
rate of the reaction?
b. How did the presence of iron (III) nitrate affect the rate of the reaction?
c. Which compound is a better catalyst?
d. Does having both catalysts present increase the rate of the reaction more than
either one alone?
5. If you have a choice of either to grind up a reactant or leave it in a large lump, which
would you choose so that the reaction rate is increased? Refer to your results from part
E.
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SKF1013: Introduction to Physical Chemistry
EXPERIMENT 2
RATE OF REACTION AND INITIAL RATES
2.1 OBJECTIVE
2.2 INTRODUCTION
Sodium thiosulfate solution is reacted with acid and a sulphur precipitate forms in a cloudy
suspension. The time required for a certain amount of sulphur to form can be used to indicate
the rate of the reaction.
Na2S2O3 (aq) + 2HCl (aq) 2NaCl (aq) + S (s) + H2O (l) + SO2 (g)
The initial rates is inversely proportional to the time taken. In symbols:
1
initial rates ∝
t
The order of reaction could be investigated by plotting 1/t as a measure of rate against the
varying concentration of sodium thiosulfate you are investigating. If the reaction is the first order
with the respect to the sodium thiosulfate, then you will get a straight line. In this experiment, the
effect of the concentration of sodium thiosulfate on the rate of reaction will be investigated.
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SKF1013: Introduction to Physical Chemistry
Chemicals
Apparatus
2.3 PROCEDURE
3. Add the acid to the flask and immediately start the clock. Swirl the flask to mix the solutions.
4. Look down at the cross from above. When the cross disappears stop the clock and record
the time. Record the data in the table.
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SKF1013: Introduction to Physical Chemistry
Volume of Volume of [Na2S2O3] (M) Time taken for cross 1/ time (s-1)
Na2S2O3 (mL) H2O (mL) to disappear (s)
50 0 0.15
40 10
30 20
20 30
10 40
2.5 QUESTIONS
1. Calculate the concentration of sodium thiosulfate in the flask at the start of each experiment.
Record the results in the table.
2. Plot a graph of concentration of sodium thiosulfate on the vertical (y) axis and time on the
horizontal (x) axis. Calculate the initial rates of the experiment
3. For each set of results, calculate the value of 1/time. (This value can be taken as a measure
of the rate of reaction).
4. Plot a graph of 1/time taken on the vertical (y) axis and concentration on the horizontal (x)
axis.
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SKF1013: Introduction to Physical Chemistry
EXPERIMENT 3
RATE OF REACTION AND RATE LAW
3.1 OBJECTIVES
3.2 INTRODUCTION
Decomposition of pure hydrogen peroxide, H 2O2 is a first-order reaction. The rate of this
decomposition at t time (t t) depends on the concentration of H 2O2.
2H2O2 H2O + O 2
d[H 2 O 2 ]
k[H 2 O 2 ] (Equation 1)
dt
d[ H 2 O2 ]t
kdt
[ H 2 O2 ]0
[ H 2 O2 ]t
ln k1t (Equation 2)
[ H 2 O2 ]0
= rate of reaction
[H2O2] = concentration of H2O2 at (t) time
k = rate constant
Equation 2 shows the relationship between initial concentrations of H2O2 with the final
concentration of H2O2 at (t) time. Usually the rate of decomposition is slow at room
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SKF1013: Introduction to Physical Chemistry
temperature but heterogeneous catalyst such as tiny platinum metal or manganese dioxide
will enhance the decomposition process. Homogenous catalyst such as dissolve ferric ion
(Fe3+), manganese ion (Mn 2+), bromide ion (Br -) and enzyme "blood catalyst" or "amylase"
are also suitable for this reaction (able to increase the rate of reaction).
Without catalyst, the decomposition reaction of H2O2 will need higher energy. Thus, a
concentrated H2O2 solution was stored in a refrigerator to prevent it from being decompose.
Otherwise, the present of catalyst such as manganese will speed up the decomposition
process.
For example:
We can reduce the decomposition process of H2O2 by using a negative catalyst (inhibitor)
like dilute mineral acid, ether or glycerol. This is because the catalyst active centre is being
neutralized or becomes inactive, and the hydrogen peroxide itself has the inhibition due to
the present of dust, which one of the factor effect the catalyst activity. In this experiment, the
dissolve ferric ion with concentration of 0.025 M is used as a catalyst. The catalyst helps to
increase the rates of H2O2 decomposition.
Chemicals
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SKF1013: Introduction to Physical Chemistry
Apparatus
Burette
Pipette 2.5 and 10 mL
Conical flask 250 mL
Measuring cylinder
Stop watch
3.3 PROCEDURES
1. Dilute 2.5 mL of concentrated H2O2 (30 % v/v) with 200 mL of distilled water in a
conical flask. Wait for 10 minutes for homogenous solution to form.
2. Meanwhile, prepare 7 conical flasks containing 10 mL of 1 M H 2SO4 each.
3. After 10 minutes, add 20 mL of FeCl 3 into H2O2 solution (name as solution A) and
directly pipette 10 mL of solution A into one of the conical flask containing 10 mL of 1
M H2SO4 (name as solution B). This time is called as (t = 0 minutes).
The decomposition reaction of H 2O2 already started when FeCl 3 was added.
4. Quickly titrate the solution B with standard potassium permanganate solution (KMnO 4)
0.05 M until colour change to light pink and record the volume, V (mL) at time, t=0 (V o)
5. After each 10 minutes within an hour, take one sample (solution A) and mix with 10 mL
of 1 M H2SO4 prepared in step 2. Directly titrate with standard solution of 0.05 M
KMnO4 as in step 4 (because Vt at time = t is needed to calculate the rate constant).
6. Plot a graph of ln Vt/Vo versus t (seconds) and estimate the k value from the slope by
using equation 2 (tangent).
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SKF1013: Introduction to Physical Chemistry
Vo = _______________
ii. What is the k value? (Calculate it from the graph by using Equation 2 )
iii. Determine the reaction rate law (from the graph). Show your calculation if required.
iv. What is the meaning of "ferric catalyst is activated by copper ions”?
v. What other methods that have been used to determine the order of reactions by
decomposition?
vi. Discuss the uncertainty that you get in this experiment.
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SKF1013: Introduction to Physical Chemistry
EXPERIMENT 4
THE EFFECT OF TEMPERATURE IN BROMINATION OF ACETONE
4.1 OBJECTIVE
4.2 INTRODUCTION
The rate of a reaction depends upon several factors i.e. the type of reaction, the concentration
of the reactants and the catalyst used, if any. For a given reaction, the rate of reaction usually
increases when the concentration of the reactants is increased. The relationship between rate
and concentration for the generalized reaction:
aA + bB cC + dD
1 d [ A] 1 d [ B] 1 d [C ] 1 d [ D]
Rate k[ A] m [ B] n (4.1)
a dt b dt c dt d dt
The superscript is called the “order” of the reaction with respect to the individual reactants. In
this case m, then, is the order of the reaction with respect to the reactant A while n is the
reaction order with respect to the reactant B.
The reaction rate is also a function of temperature. An increase in temperature will result in a
faster reaction rate. A general “rule of thumb” is that an increase of 10 °C doubles the rate of a
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SKF1013: Introduction to Physical Chemistry
reaction. Just as for concentration, there is a relationship between reaction rate and
temperature. This relation based upon the theory that for a reaction to occur, the reactants must
possess a minimum energy (specific to particular reaction). Usually this reaction is assumed to
be in the form of kinetic energy (energy of motion) of the reactants. This minimum energy
required for reaction is called the activation energy of the reaction. It appears as a maximum in
the progress-of-reaction vs energy profile for the reaction. The equation that relates the rate
constant with the absolute temperature, T, and the activation energy, Ea is
Ea
ln k ln A (4.2)
RT
Where; R = gas constant k = rate constant
A = constant, normally known as Arrhenius parameter.
If the rate of the reaction is determined at several temperatures, the activation energy can be
found from the graph.
Chemicals
Apparatus
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SKF1013: Introduction to Physical Chemistry
4.3 PROCEDURES
1. Fill in 10.0 mL of 4 M of acetone into boiling tube, then followed with 10.0 mL 1.0 M HCl and
20.0 mL distilled water (boiling tube A).
2. Measure 10.0 mL 0.02 M bromine solution (CAUTION: Dangerous) using graduated
measuring cylinder and pour into another boiling tube (boiling tube B).
3. Immerse both boiling tubes in water bath at room temperature for about 5 minutes until the
solution have reached the temperature 20°C of the water bath. Mix together two solution
and at the same time start the stop watch to record the exact time of mixing.
Fill the water bath with ice cubes to obtain temperature lower than room temperature
(≈ 20 °C)
4. Record the time, t, when the reaction is complete, that is, when the solution becomes
colourless (all the bromine has reacted). You should use a test tube filled with distilled water
for colour comparison.
5. Repeat the step 1 - 5 at temperature: 35 °C, 40 °C, 45 °C and 50 °C. Repeat step 1 to 5 (for
each temperature) two or three times to ensure that reproducible results are obtained. Use
the average time, to calculate the rate of reaction at that temperature.
Calculate the rate of reaction at each temperature studied and determine the activation energy
1
of the reaction from the graph of ln rate vs
T
4.5 QUESTION
1
Explain why the graph used to determine the activation energy is ln rate vs
T
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SKF1013: Introduction to Physical Chemistry
EXPERIMENT 5
ENTHALPY
5.1 OBJECTIVES
5.2 INTRODUCTION
A chemical or physical change involves in the transfer of heat (energy). Reactions that release
energy in the form of heat are called exothermic reactions. While, a process that absorbs
energy from its surroundings is called endothermic reaction. Calorimeter is used to measure the
quantity and heat transfer, in which undergoes chemical or physical change. Heat transfer in a
chemical reaction is defined quantitatively as enthalpy (heat) reaction, ∆H at constant pressure.
∆H is negative for exothermic reaction and positive for endothermic reaction. The heat capacity
of a substance is the amount of heat required to raise the temperature, 1 °C of one gram of the
substance.
The enthalpy of neutralization involves acid base reaction and for strong acid and base, the
reaction is exothermic. AHn is determined by
a) assuming the density and specific heat for acid and base solution are the same as water
b) measure the temperature change, ∆T
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SKF1013: Introduction to Physical Chemistry
The unit of ∆Hn is kJ/mol of acid and base reacted. Mass (g) of solution is the total mass of acid
and base in solution.
The enthalpy of solution is produced when a salt dissolve in water. Energy is absorbs and
releases. Pottasium nitrate (KNO3) dissolves in water:
H2O
KNO3 (s) K + (aq) + NO 3- (aq)
The lattice energy (enthalpy) of salt, ∆HLE and hydration energy (enthalpy), ∆Hhyd will
determined whether heat is absorbed or released when 1 mole of salt dissolve in water. The
enthalpy of solution and dilution; ∆Hs is total of ∆HLE and ∆Hhyd Salt dispersion enthalpy, ∆Hs is
determined experimentally with the combination of heat loss from the salt and water whenever
both of them are mixed.
Apparatus
Styrofoam cup with lid with a tiny hole for thermometer
Thermometer
Measuring cylinder
100 mL beaker
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SKF1013: Introduction to Physical Chemistry
5.3 PROCEDURES
1. Weigh 5.0 g (± 0.001 g) potassium nitrate KNO3 salt, which is already prepared for you.
2. Measure the mass of a dry cup and put in 20 mL of distilled water and record the
temperature.
3. Add salt in the Styrofoam cup and place the lid on top of the cup. Swirl the cup while
recording the temperature for every 10 - 20 seconds until the temperature is constant.
4. Plot a temperature (°C) vs time (seconds) graph and determine the maximum temperature
for the neutralization of the reaction.
5. Repeat experiment to get an accurate data.
6. Repeat step 1-5 by using potassium sulphate K2SO4 and both of the ∆Hn will be
compared.
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SKF1013: Introduction to Physical Chemistry
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SKF1013: Introduction to Physical Chemistry
Salt: _____________________________
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