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LABORATORY MANUAL
SKF3013
PHYSICAL CHEMISTRY I
Department of Chemistry
Faculty of Science and Mathematics
UNIVERSITI PENDIDIKAN SULTAN IDRIS
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SKF3013: Physical Chemistry I
No Experiments Pages
2 Heat of Combustion 11
5 Adsorption 21
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SKF3013: Physical Chemistry I
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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SKF3013: Physical Chemistry I
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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SKF3013: Physical Chemistry I
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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SKF3013: Physical Chemistry I
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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SKF3013: Physical Chemistry I
EXPERIMENT 1
DETERMINATION OF THE HYDRATION ENTHALPY OF AN ELECTROLYTE
(SOLUTION ENTHALPY)
1.1 OBJECTIVES
1. To measure the integral enthalpy of solution of copper (II) sulphate and anhydrous
copper (II) sulphate
2. To calculate the hydration enthalpy of anhydrous copper (II) sulphate.
1.2 INTRODUCTION
The dissolution of a solid electrolyte in water is primary determined by two simultaneously
occur in processes: the destruction of the crystal lattice and the hydration of the ions.
When a salt exists in both hydrated and dehydrated forms, and one assumes that during
the dissolution of the hydrated salt only the degradation of the crystal lattice occurs, the
enthalpy of hydration can be calculated with Hess’s theorem (Figure 1)
H CuSO4
[CuSO4](s) [CuSO45H2O](s)
+H2O +H2O
L H CuSO4 5 H 2O
LH
LH (1.1)
n
H H Enthalpy of hydration
L H Integral enthalpy of solution
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SKF3013: Physical Chemistry I
q exp
LH (1.3)
n
Texp
q exp q cal . (1.4)
Tcal
Apparatus
Equipment’s set-up
Stop watch
Beaker
Mortar with pestle
Chemicals
1.3 PROCEDURES
1. Weigh 24.97 g (0.1 mol) of copper (II) sulphate and 15.96 g (0.1 mol) of anhydrous
copper (II) sulphate and pulverized using pestle and mortar.
2. Fill in the calorimeter with 900 mL of distilled water. Put the magnetic stirring bar
into the calorimeter and place on hot plate.
3. After attaching the heating coil and the temperature probe, switch on the knob
stirrer (CAUTION : Do not mistakenly switch on the heating knob)
4. When the equilibrium temperature has been reached (approximately 5 min), add
copper (II) sulphate into the calorimeter. Make sure that the entire quantity of salt is
added to the calorimeter.
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SKF3013: Physical Chemistry I
5. Record the temperature with time. Ten minutes after the salt has completely
dissolved, conduct the electrical calibration* in order to determine the total heat
capacity of the calorimeter.
Electrical calibration*: Supply 10 V AC to the work and power meter for the
electrical heating. Performed a reset and then plug the free ends of the heating
coil’s connection cables into the output jacks of the work and power meter.
Continuously heat the system, and measure the supplied quantity of energy. After
electrical energy amounting to approximately 4000 Ws has been supplied, switch
off the heating and read exact quantity of electrical energy from the meter.
7. Determine the corrected temperature differences, T, for the calibration and
solution experiment as shown in Figure 2. (This correction is necessary because of
the heat exchange with the surroundings).
8. Draw the vertical straight line Texp, which intersects the lines T1T2 and T3T4 in
such a manner that the shaded areas are of equal size.
9. For the calibration, analogously determine Tcal from the intersection points of T3T4
and T5T6.
10. Repeat the same experiment to determine the enthalpy of solution for anhydrous
Copper (II) sulphates. At least two measurements should be performed for each
salt to avoid errors and to be able to calculate mean value.
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SKF3013: Physical Chemistry I
4.0
3.8
T5
T (K) 3.6
3.4
3.2
Tcal
3.0
T1 T2
2.8
TExp
T3 T4
Figure 2: Graphical determination of the correct T values from the temperature time curve.
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SKF3013: Physical Chemistry I
EXPERIMENT 2
HEAT OF COMBUSTION
2.1 OBJECTIVES
1. To determine the calorimeter constant using benzoic acid
2. To determine the heat of combustion of an easily combustible material.
2.2 INTRODUCTIONS
Apparatus
Bomb calorimeter
Pallet maker
Thermometer (Scaled divisions accurate to at least 0.200C
Pipette 1.0 cm3
Volumetric Flask 2 litter
Fuse wire
Chemicals
Benzoic acid
100 cm3standardized Na2CO3 (0.00725 M)
Sample: cooking oil, sucrose,activated carbon, petrol, albumin, etc.
2.3 PROCEDURES
1. Weigh approximately 0.8 – 1.0 g of benzoic acid and not more than 1.1 g.
2. Transfer the benzoic acid into the pallet maker and press to form pallet. Weigh the
pallet accurately and carefully place it in the combustion tray. Place the tray in its
holder.
3. Weigh accurately a piece of fuse wire approximately 10 cm in length. Wrap the
fuse wire around the fuse leads on the cover of the bomb as demonstrated
(Demostrate by instructor)
4. Clean and dry the inside of the base of the “bomb” chamber. Pipette 1.00 cm3
distilled water into the base of the bomb.
5. Place the bomb cover on the base and gently screw the base until the bomb is
tightly closed.
6. Connect the gas valve on the bomb cover to the oxygen gas cylinder. Fill the bomb
with oxygen gas to a pressure of 30 atm as directed by your instructor. (CAUTION!
Do not use a pressure in excess of 40 atm. If the oxygen has been allowed to
reach a pressure greater than 40 atm, do not continue with the experiment.
Release the gas through the release valve and refill the bomb with oxygen to the
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SKF3013: Physical Chemistry I
desired pressure.)
7. Place the bomb in the calorimeter base. Connect the wires to the external fuse
leads.
8. Pour 2000 0.5 ml of water into thecalorimeter base covering the base. (Closed
thecalorimeterand begin stirring). Let the water temperature reached equilibrium.
9. Press the ignition switch for about 5 seconds. (CAUTION! Do not stand too near
the calorimeter for about 20 seconds after the ignition). Record the temperature
readings at 30 seconds intervals for about 15 minutes after ignition.
10. Construct a graph (temperature vs. times) using the data collected. Determine the
change in temperature of the system that was caused by the combustion of the
benzoic acid.
11. Open the calorimeter and remove the bomb. Slowly release the gas through the
release valve. Remove the cover of the bomb. If the sample has completely
burned, continue with the following steps, otherwise, record the problem on your
data sheet and prepare to repeat the experiment.
12. Wash the interior of the bomb with distilled water. Pour the washings water into
200 cm3volumetric flask and fill accurately (to the mark).
13. Titrate the aliquot of this solution with the standard solution of sodium carbonate
(Na2CO3 0.0725M) provided using phenolphthalein as the end-point indicator. (The
purpose of this step is to determine the amount of nitric acid produced during the
combustion, if any)
14. Remove the remaining pieces of fuse wire from the leads and weigh them
accurately.
15. Repeat the procedure using benzoic acid to determine an average value for the
calorimeter constant.
16. Repeat the procedure using and accurately weighed amount of combustible
material.
Data processing
1. Find the number of mole of nitric acid produced during the combustion.Determined
the heat released in the formation of this amount of nitric acid. (the heat formation
of nitric acid is given as 13,800 cal mol-1).
2. Calculate the heat released in the combustion of the fuse wire. (The heat of
combustion of the fuse wire used is 1400 cal g-1)
3. Calculate the calorimeter constant using the following equation.
qm e1 e2
W (2.1)
T
Where :
W = Calorimeter Constant cal C-1
q = Heat of combustion and for benzoic acid, 6318 cal.g-1
m = Mass of combustible material
e1 = Heat of formation of HNO3, cal
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SKF3013: Physical Chemistry I
26.454
m (2.2)
q
Where:
m = Mass of sample, g
q = Estimated value of heat of combustion of sample,
cal g-1
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SKF3013: Physical Chemistry I
EXPERIMENT 3
3.1 OBJECTIVES
3.2 INTRODUCTION
Due to intermolecular interactions the measured total volume resulting from the mixture
of two real liquids (e.g. ethanol and water) deviates from the total volume calculated from
the individual volumes of the components (volume contraction). To describe this non-
ideal behaviourin the mixing phase, one defines partial molar quantities (including partial
molar volumes), which are dependent on the system composition, for the components;
these values can be experimentally determined.
In the ideal mixing phase the volume vid and the mean molar volume Vidof a mixture of
components A and B, which is independent of the system size, can be calculated if the
quantitative composition is known
nA nB
xA xB …….(3.1)
n A nB n A nB
vid
Vid V A x A VB x B …………….(3.2)
n A nB
However, the assumed additivity in equation (3.2) loses its validity in cases involving real
mixture, as the thus measured real volume vr and Vr deviate more or less strongly from
the volumes obtained using equation (3.2) due to the volume contraction occurring on
mixing.
The volumes vr and Vr of the real mixture can, however still be calculated if the molar
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SKF3013: Physical Chemistry I
volumes Vi of the pure components A and B in equation (3.1) are replaced with the
partial molar volumes VA and VB which are independent of the composition.
v v
V A r VB r …………(3.3)
n A T , P ,nB n B T , P ,n A
vr
Vr V A x A VB x B …………………….(3.4)
n A nB
The difference between the mean molar volumes defined according to the equations
(3.2) and (3.4) is designated as the mean molar mixing volume MV and is an intensive
measure for the mixture’s deviation from ideal behaviour.
d ( M V ) dVr dVid
(V A VB ) (V A VB ) ………………(3.6)
dx A dx A dx A
d ( M V )
VB M V x A VB
dx A
And …………………………(3.7)
d ( M V )
VA M V xB VA
dx A
Are obtained. According to them the desired partial molar volumes of the components A
and B for the specific compositions (xA and xB) and the measured MV can be determined
if the molar volumes of the pure substances (VA, VB) and their differential quotients
d ( M V )
are known. These can be obtained as the tangent to the graphical plot of MV
dx A
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SKF3013: Physical Chemistry I
MV/ mL mol-1
-0.4
-0.6
-0.8
-1.0
-1.2
-1.4
-1.6
Apparatus
Aluminium foil
Water Bath
Chemicals
Ethyl alcohol
Distilled water
3.3 PROCEDURES
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SKF3013: Physical Chemistry I
3. Fill in dry pycnometers of known empty mass completely with the mixtures of
ethanol and water.
4. Cover the pynometers with aluminium foil and place in temperature-controlled
bath at 20 0C for about 30 minutes.
5. Remove the pycnometers individually, seal it with the corresponding stopper and
weight after meticulous drying.
Data processing:
vr
Vr
nA nB
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SKF3013: Physical Chemistry I
EXPERIMENT 4
4.1 OBJECTIVES
4.2 INTRODUCTION
The relationship between the solubility of a substance and temperature is given by the
equation,
d ln S H
(4.1)
dt RT 2
Where , S = Solubility
H = Heat of solution of substances.
This equation is called the Van’t Hoff isocore. IfH assumed to be constant between
T1and T2equation (4.1) becomes,
S 1 H 1 1
ln . (4.2)
S2 R T2 T1
or
S1 H T1 T2
log10 (4.3)
S 2 2.303R T1T2
If the solubility of the substances is determined at two different temperatures, the heat of
solution can be calculated from the above equation. More accurate results can be
1
obtained by plotting log S vs. using data at several temperatures.
T
The “freezing point reduction curve” and the “solubility curve” are two different names for
the same curve, that is, the curve of temperature vs. composition for a solid and liquid in
equilibrium at a constant pressure. This type of curve is shown in following Figure 3 for
two component system containing compounds benzene and naphthalene.
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SKF3013: Physical Chemistry I
Benzene Naphthalene
80
T
Solution D
60
40
C
Solid Naphthalene
20 +
Solution
Solid
benzene
+ Solution
E
Solid Benzene + Solid Naphthalene
These statements are two ways of understanding the same thing: in the first case,
temperature is taken as a function of concentration while in the second case;
concentration is taken as a function of temperature.
The lowest point in the temperature vs. composition diagram, E, is called the “EUTECTIC
POINT” (from the Greek word meaning “easily melted”)
Apparatus
Beaker
Test tube
Water bath
Thermometer
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SKF3013: Physical Chemistry I
Chemicals
Naphthalene
Diphenylamine
4.3 PROCEDURE
Data processing:
1. By using cooling curve (temperature vs. composition), plot the phase diagram of
naphthalene-diphenylamine system (freezing point vs. composition). Label all
parts of the diagram – lines and area.
2. Determine the heat of fusion of naphthalene and diphenylamine by plotting log
1
composition vs.
T
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SKF3013: Physical Chemistry I
EXPERIMENT 5
ADSORPTION
5.1 OBJECTIVES
5.2 INTRODUCTION
There are two types of adsorption that can occur namely physisorption and
chemisorption. Chemisorption is also called active adsorption due to the formation of
chemical bond. Physisorption however, involves van der Waals forces between the
molecule of adsorbates and adsorbent. When chemisorption occurs, only a monolayer of
adsorbate is formed on the surface of the adsorbent. However, physisorption involves
the formation of multilayer of the adsorbed molecules.
Freundlich stated that the equation for adsorption isotherm can be written as :
N KC a (5.1)
Where;
N = total number of mol adsorbate adsorbed by 1 g of activated carbon
C = Concentration at equilibrium
K = Constant
a = Constant (range between 0-1)
KC
(5.2)
1 KC
Where,
= Surface fraction that is covered by the adsorbate molecules
N
Nm
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SKF3013: Physical Chemistry I
C C 1
(5.4)
N N m KN m
C 1
A plot of versus C will give a straight line with a slope of . If the cross section area
N Nm
() of the adsorbed molecule is known (which is the area occupied by each adsorbate
molecule on the surface of adsorbent), The specific surface area, A (m2 g-1) can be
calculated using the following equation :
Apparatus
Chemicals
Activated Carbon
Acetic acid (2M)
PelleteNaOH
Standard solution of HCl (0.10 M)
Phenolphthalein
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SKF3013: Physical Chemistry I
5.3 PROCEDURE
Data processing:
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SKF3013: Physical Chemistry I
EXPERIMENT 6
6.1 OBJECTIVES
1. To prepare manganum dioxide (MnO2) sol
2. To test the Schulze-Hardy Rule
6.2 INTRODUCTION
The term”colloid” was first introduced by Thomas Graham (1861) to explain the
dispersion of small particles of a material in a medium and they are inseparable when left
for a long time. A colloid system consists of a dispersion phase and a dispersion
medium. If the diameter of the dispersed particles is in range between 20 Å to 2000 Å,
then the colloid is formed.
There are eight classes of common colloidal system. These colloids are made-up of
solids, liquids and gases. A colloid formed by the dispersion of a solid in a liquid is called
a sol. Sols exhibit several physical properties such as tyndall effect, electrical effect and
molecular-collision effect.
In general, sol can be classified into two types; lyophilic (solvent-attracting) and
lyophobic (solvent-repelling). Lyophilic sol can be prepared by dispersion (normally by
vigorous stirring of a solid in the form of gel or resin in a liquid), and condensation.
During dispersion, solids are disintegrated into particles of suitable sizes to form a colloid
in a dispersion medium. During condensation however, molecules or atoms are
condensed into clusters/particles of suitable sizes to form a colloid.
Lyophobic colloids are very sensitive to the presence of electrolytes, in which a small
amount of added electrolytes resulted in precipitation. The precipitation of sol by
electrolytes can be predicted using Schulze-Hardy rule, which stated that “The effect of
precipitation by a given ion on a (lyophobic) dispersed phase of opposite charge
increases by the increase of the valence of the ion”.
Apparatus
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SKF3013: Physical Chemistry I
Stop Watch
Chemicals
6.3 PROCEDURE
1. Take 4 (or more) clean test tubes and label them with numbers; 1, 2, 3, 4….
2. Add 10 mL of 0.10 M NaCl solution in test tube no. 1.
3. Add in 1 mL of same solution in test tube no. 2 then 9 ml of distilled water and
homogenized the solution by swirling.
4. Transfer 1 mL of the NaCl solution from test tube no. 2 into test tube no. 3, and
then add 9 mL of distilled water.
5. Perform further dilution on the NaCl solution in the test tube no 4, 5….
6. Add 1 mL of the MnO2 sol into each test tube. Mildly swirl the test tube and
observe the one which form a precipitate in 2 minutes. Record the concentration
of the NaCl solution.
7. After obtaining the result, perform further tests using NaCl solutions with
concentration lower than the lowest concentration that yield a precipitate. The
purpose of this test is to obtain a more accurate minimum concentration. For
instance, supposed the result of step (6) shows that the 0.1 M NaCl solution
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SKF3013: Physical Chemistry I
yielded a precipitate of MnO2 but not the 0.01 M solution, then a series of NaCl
solutions with concentration between 0.1 and 0.01 M (e.g. 0.08 M, 0.06 M, 0.04 M
and 0.02 M) should be prepared, for the formation of the precipitate within 2
minutes as in step (6)
8. Repeat steps (1) to (7) using CaCl2 and AlCl3 solutions.
Data Processing:
1. Calculate the minimum concentration of the salt solutions (NaCl, CaCl2 and AlCl3)
required for the precipitation of the MnO2 sol in 2 minutes.
2. From the result of this experiment, determine whether the MnO2 sol is positive or
negative charged
3. By what method the MnO2 sol was prepared?
4. Supposed a soluble lyophilic sol was added into an MnO2 sol prior to the addition
of an electrolyte, what would be the effect? Explain your answer.
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