Physical Chemistry Experiments

UTAR
FHSC1114 Physical Chemistry

Trimester 1
Topic 1: Introductory to laboratory safety and apparatus

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1. Materials requirement
There are various materials that students must bring along during laboratory session.
Students will be asked to leave the laboratory if they fail to bring the items listed.
Laboratory manual
Appropriate PPE (Personal Protective Equipment)
Protective laboratory coating (Lab Coat) to protect you and your attire.
Covered shoes to protect you from chemical burn or other hazards. Open toes
shoes are strictly not allowed.
Safety glasses or goggles to protect your eyes.
Some other experimental materials which are requested by the lecturer.
Calculator or scientific calculator.
Record book to record observation and experiment results during lab sessions.
2. Practical Exercises
To get the most out of the practical exercises, you are required to obey the
instructions given. These instructions have been designed to provide you with
experience in the following skills:
Following instructions
Handling apparatus
Having due regards for safety
Making accurate observations
Recording results in an appropriate form
Presenting quantitative results
Gives valuable discussion
Drawing conclusions
Following Instructions
Follow the sequence of instructions as they are provided in an appropriate order.
Experimental procedures must be read through before carrying out the experiment. Draw
out the procedure in a flow chart for better understanding of the steps for the experiment.
Apparatus Handling
Before carrying out an experiment, it is important for scientists to plan and gather for
their experiment apparatus. As such, you are advised to list down the apparatus to be used
for the entire experiment before the start of the experiment. You will be able to master
the basic technique of using different types of apparatus. These include measuring
cylinder, bulb pipette, graduated glass pipette, volumetric flasks and burette. For different
type of tasks, different set of the apparatus are to be used.
Lab manual version 4.0

Foundation in Science
UTAR
Trimester 1
Laboratory Safety
Always move slowly and carefully in the lab.
During and after practical session, never touch your mouth or eyes with fingers before
thorough wash of hands with soap and water.
Make sure glass objects (e.g: thermometer or glass rod) are not placed unattended on
the bench to prevent it from being rolled off from the working bench to the floor.
Always put on your PPE such as lab coat, safety glasses and wear covered shoes in
the lab.
Remarks:
Proper heating using Bunsen burner (even with heating of water).
Proper handling of any liquids, particularly those identified as corrosive, irritant, toxic
or harmful.
Careful handling of corrosive work.
Allow hot plate, Bunsen burner, tripods, gauzes and beakers to cool down before
handling them.
Keep long hair tied and do not wear dangly earrings.
Do not allow electrical equipment to come into contact with water.
If you are not sure about how to carry out a scientific procedure, ask the lecturer or
lab officer.
Make sure you understand the rationale and consequences of your actions before you
act.
Follow all safety instructions given in the manual or provided by the lecturer/tutor for
particular experiments (e.g. use of gloves or mask).
Making Accurate Observation
The experiment will make it clear about the needed observation, e.g. the color changes
when two solutions are added together or time taken for a chemical reaction. Ensure that
you know the proper handling of relevant equipment before the start of experiment.
Think carefully about the precision of your observations. You may need to find out
reference for color description from external sources (e.g. reference books or online
references) before the practical session.
Recording Results in an Appropriate Form
Results can be recorded in various ways. Often it is helpful to record raw data in a table.
Most data will be in the form of numbers, e.g. quantitative data (also known as numerical
data). However, some data, e.g. color of solution, are qualitative. Bear in mind that the
best way for data collection is to avoid missing out any observation you have made, and
keep your raw data in safe hand.
Presenting Quantitative Results
Presentation of data can be made using table, graph or other visual means to ease result
analysis. You will have to choose the best way to present the experimental results.
Drawing Conclusion
Conclusions should be drawn from and supported by experimental results.
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Trimester 1
3. Writing a Scientific Report

Title
Refers to the subject investigated.
Introduction
State the hypotheses
Give well-defined reason(s) for making hypotheses.
Explain the chemical basis of the experiment.
Cite sources to substantiate background information.
Explain how the method used will produce information relevant to the
hypotheses.
State a prediction based on the hypotheses.
Material and Methods
Use appropriate format.
Give enough details (so that the experiment can be duplicated).
State the control treatment, replication, and standardized variables that were used.
Results
Summarize the data (do not include raw data).
Present the data in an appropriate format (table or graph).
Present tables and figures neatly so they are easily read.
Label the axes of each graph correctly.
Give units of measurement where appropriate.
Write a descriptive caption for each table and figure.
Include a short paragraph pointing out the important results (do not interpret
the data).
Do not create your own data which is not true.
Discussion
State whether the hypotheses was supported or proven false by the results, or else
state that the results were inconclusive.
Cite specific results that support your conclusions.
Compare the results, with your predictions and explain any unexpected results.
Compare the results with other research or information available.
Discuss any weaknesses the experimental design or problems with the
execution of the experiment.
Discuss how you might extend or improve the experiment.
Conclusion
State conclusion which is supported by results
Restate important results.

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Literature Cited
Use proper citation form in the text.
Use proper citation form in the Literature Cited section.
Refer in the text to any source listed this section.
Acknowledgment
State any appropriate and necessary acknowledgment.
4. Apparatus and Equipments

Apparatus and Equipments
Description and Function
Beaker
Conical flask/
Erlenmeyer flask
Beaker is a simple container for liquids, very commonly

used in laboratories.
Beakers are generally cylindrical in shape, with a flat
bottom.
Beakers are available in a wide range of sizes, from 1 ml
up to several liters.
An Erlenmeyer flask (conical flask) is a type of widely

used laboratory flask which features a conical base with a
cylindrical neck.
They are usually marked (graduated) on the side to
indicate the approximate volume of their contents.
The conical flask's counterpart is the beaker. However the
main difference is its narrow neck.
The neck allows the flask to be stoppered using rubber
bungs or cotton wool.
The conical shape allows the contents to be swirled or
stirred during an experiment (as is required in titration);
the narrow neck keeps the contents from spilling
A filtering funnel is a pipe with a wide, often conical

mouth and a narrow stem.
It is used to channel liquid or fine-grained substances into
containers with a small opening. Without a funnel, much
spillage will occur
Filtering funnel

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A graduated cylinder also referred to as a measuring

cylinder, type of laboratory glassware comprised of a tall
cylinder with a range of calibrated markings that is used
for visually measuring the volumes of liquids in a
quantitative manner.
A graduated cylinder can be made of translucent plastic
or borosilicate glass.
Measuring cylinder
A volumetric flask refers to graduated glassware used

for the measurement of volume of liquids when the
bottom of the meniscus is perfectly aligned with mark on
the neck of the flask.
Volumetric flask
Measuring
pipette
Volumetric
pipette
Pipettes are used to transfer a specific volume of liquid.

2 most common used pipette in a science laboratory are:
a) Volumetric pipette (Bulb pipette)
b) Measuring pipette (Serological pipette)
Pipette
Burette is a vertical cylindrical piece of laboratory

glassware with a volumetric graduation on its full length
and a precision tap, or stopcock, on the bottom.
It is used to dispense known amount of a liquid reagent in
experiments for which such precision is necessary, such as
a titration experiment.
Burettes are extremely precise: class A burettes are
accurate to 0.05 ml.
Burette
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Reagent bottles are used to hold small stocks of reagents

and samples for use.
Reagent bottles must be clean but not necessarily dry.
Reagent bottles
Desiccators are sealable enclosures containing desiccants

used for preserving moisture-sensitive items.
A typical desiccator contains two compartments
separated by a perforated plate; the desiccant is placed at
the lower compartment while the reagent is placed in the
upper compartment.
It should not be used to dry an object, but to maintain an
already dried object indefinitely in a dry condition.
Desiccators
Separating funnel also known as separatory funnel or

separation funnel. It is used to partition the components
of a mixture of immiscible liquids with different
densities.
Typically, one of the liquids will be water, and the other
an organic solvent such as ether or chloroform.
The funnel, which is in the shape of a cone surmounted
by a hemisphere, has a stopper at the top
Separating funnel
An electronic balance uses electromagnet to balance the

weight on the pan.
This unit widely used in science laboratory as weighing
equipment.
Electronic balance

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Topic 2: Precipitation of barium (II) sulphate

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Introduction:
Barium (II) nitrate reacts with sulphuric acid to produce barium (II) sulphate as white
precipitate which is difficult to dissolve in water. If sulphuric acid is in excess compared
to barium (II) nitrate, the entire ion Ba2+ will precipitate as barium (II) sulphate.
Therefore, barium (II) nitrate is a limiting reagent and the quantity of precipitate formed
is determined by this limiting reagent. The excess acid will then be separated using
distilled water.
Apparatus and Equipments:
Pipette (10mL)
Hot water bath
Beaker (100mL)
Filter funnel
Glass rod
Filter paper
Watch glass
Electronic balance
Materials:
0.1 M Barium (II) nitrate solution, Ba(NO3)2
0.5 M Sulphuric acid, H2SO4
Procedures:
1. Pipette 10mL of Ba(NO3)2 into a 100mL beaker.
2. Add 10mL of diluted H2SO4 and stir with a glass rod. Allow the precipitate to settle.
3. Weigh a clean and dry watch glass with a filter paper. Then, put the filter paper into
the filter funnel.
4. Carefully filter all the liquid in the beaker.
5. Add 20mL of distilled water into the same beaker, stir for 1 minute, and rinse the
glass rod and the side of the beaker. Wait for a while and filter like the previous step.
6. Decant the filtrate and remove the filter paper with precipitate to the watch glass.
7. Dry the precipitate in the oven until there is no liquid left on the watch glass.
When the precipitate dries, cool and measure the weight. Repeat this step until the
mass is same or less than 0.02g different.
Treatment of Data:
Mass of dry watch glass with filter paper
Mass of watch glass with filter paper + precipitate
Mass of BaSO4 precipitate
g
g
g
Calculation:
1. Calculate the molecular weights of Ba(NO3)2 and BaSO4.
2. Calculate the moles of BaSO4 are produced in this experiment.
3. Calculate the moles of Ba(NO3)2 are required to react with H2SO4.
4. Determine which is limiting reactant in this experiment.
5. Determine the percentage yield of BaSO4.
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Trimester 1
Topic 3: Determination of the amount of dissolved oxygen in a water sample by

iodometry the Winklers method
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Introduction:
Myriad forms of life exist in lakes, streams and oceans. These creatures depend on
dissolved oxygen (D.O.) in water for their life support. Occasionally something will
happen which depletes the oxygen content of a natural water system.
The dissolved oxygen content is an important index when considering the suitability of
water for town supply. Good potable water will give a D.O. value close to the theoretical
value for a saturated solution for oxygen in water. When there is pollution from organic
matter and other trade effluents, the D.O. is used up in various biochemical oxidation
processes and it is only slowly replaced through surface adsorption. Such water will give
a low D.O. content until oxidation is completed. Adequate D.O. is necessary for the life
of fish and other aquatic organisms.
Gases which are dissolved in water obey Henrys law to a first approximation:
Xi = k . Pi
Where Xi is the mole fraction of the gas in solution, k is the Henrys law constant and P i
is the partial pressure of the gas. For oxygen, at 20 oC, k = 2.5 x 10-5 atm-1 and P (O2) =
0.21 atm for air.
Also, it is approximately true that X (O2) = n (O2) / n (H2O) since n (O2) << n (H2O) and
n (H2O) = 5.5 mol/1. Thus, n (O2) = 2.9 x 10-4 mol/1. The solubility of oxygen is then
S(O2) = 9.3 mg/1 at 20 oC. Experiment indicates that solubility of oxygen is actually 9.2
mg/1 of D.O. in pure water at 20 C (Table 1).
The solubility decreases with increasing temperature and increasing electrolyte
concentration.
Table 1: Solubility of oxygen in natural water
T (oC)
D.O. in pure water (mg/L)
0
14.6
10
11.3
20
9.2
30
7.6
The method described below for the determination of oxygen in water is based on that
devised by Winkler. Since the D.O. content of a sample is so transitory, the sample must
be fixed very soon after collection. The sample is first treated with excess of
manganese (II), potassium iodide and sodium hydroxide. The white manganese (II)
hydroxide that is formed reacts rapidly with oxygen to form brown manganese (III)
hydroxide.
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4Mn(OH)2 (s) + O2 + 2H2O
4Mn(OH)3 (s)
When acidified, the manganese (III) oxidizes iodide which is already present to iodine:
2Mn(OH)3 (s) + 2I- + 6H+
I2 + 6H2O
+ 2Mn2+
The liberated iodine, which is equivalent to the D.O. content, may then be titrated with
standard sodium thiosulphate:
I2 + 2S2O32-
Apparatus:
Volumetric pipette (100 mL)
Conical flask (500 mL)
Burette
Burette clamp
Pasteur pipette
S4O62- + 2I-
Reagent bottle (1 L)
Conical flask stopper
Retort stand
Measuring cylinder (5 mL)
Materials:
Manganese sulfate solution
Alkaline-iodide solution
0.025 M Sodium thiosulphate solution
Concentrated sulphuric acid
Starch solution
Procedures:
1. When sampling water, care must be taken to ensure that a good representative sample
of the water to be analyzed is obtained. For most purposes, this includes attention to
dissolved gases. Therefore, the water sample should be taken in a clean bottle which
must be filled to overflowing and tightly sealed with stopper without introduction of
air. If the water is sampled from a tap, it must be allowed to run for at least 5 minutes
prior to sampling. For this purpose, you may collect the water into a 1 L reagent
bottle fitted with a stopper.
2. Carefully remove the stopper from the conical flask and add 4 mL of the manganese
sulfate solution, discharging the reagent from the tip of a pipette put well below the
water surface. Replace the stopper.
3. Similarly, introduce 4 mL of the alkaline-iodide solution.
4. Place the stopper in the bottle; be sure that no air becomes entrapped. Some overflow
may occur. Thoroughly mix the content by inversion and rotation. Manganese
hydroxide is precipitated and will settle on standing.
5. When the precipitate has settled, introduce 4 mL of concentrated sulfuric acid with
the tip of the pipette well below the surface of the solution.
6. Replace the stopper and mix until the precipitate dissolves completely. The dissolved
oxygen now liberates free iodine from the potassium iodide present.

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7. Pipette 200 mL of the acidified sample into a 500 mL conical flask and titrate with
0.025 M sodium thiosulphate until the solution becomes pale yellow.
8. Add a few drops of starch indicator and continue the titration to the disappearance of
blue color.
(If the blue color doesnt appear after adding starch, repeat the titration and adding
starch before start of titration)
9. Repeat the titration twice.
Treatment of data:
Titration number
Final reading
Initial reading
Volume used (cm3)
Average volume of titrant required for titration = ____________ cm3

Calculation:
1. Determine the concentration (ppm) of dissolved oxygen (DO) in the water sample.
2. Chemical equation below shows the reaction between iodine and thiosulphate.
I2 + 2S2O3-2 S4O6-2 + 2ICalculate the oxidation states for the underlined elements and determine the oxidizing
and reducing agents.

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Topic 4: Gases Boyles Law and Charless Law

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Introduction:
Boyle's Law states that the volume of a given mass of gas sample is inversely
proportional to the pressure applied to the gas if the temperature is kept constant.
P x V = constant
P1 V1 = P2 V2
Charless Law states that the volume of a given mass of gas sample is directly
proportional to its absolute temperature, if the pressure is kept constant.
V
= constant
T
V1
V2
T1
T2
The data collected from the experiment can be plotted on graphs in order to see the
relationship between volume and pressure and the relationship between volume and
temperature.

Syringe (25 mL)
Pressure Gauge
Beaker (500 mL)
Thermometer
Plastic tubing
Lubricating oil
Hot water bath
Retort stand
Burette Clamp
Hotplate
Procedures:
Part 1 Boyles law
1. Pull the syringe plunger to 20 mL mark.
2. Connect the end of the syringe to the plastic tubing.
3. Connect the other end of the plastic tubing to the pressure gauge. (Make sure all of
the tubing are sealed securely)
4. Record the pressure when the syringe plunger is at 20 mL.
5. Reduce the volume in the steps of 2.5 mL until the 5 mL mark and record the pressure
for each.
6. Plot a graph of pressure (P) versus volume (V) and pressure (P) versus inverse of
volume (1/V).

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Part 2 Charless law

1.
2.
3.
4.
5.
6.
7.
8.
Prepare about 400 mL of warm water in a beaker that is placed on top of a hotplate.
Lubricate the syringe plunger with oil to ensure smooth sliding in the syringe tube.
Pull the plunger to 5 mL mark and seal the end of the syringe.
At 50 C, immerse the syringe tube in the warm water by adjusting the height of the
burette clamp holding it. Wait about 1 minute for the air in the syringe to come to the
same temperature as the water.
Record the water temperature and the volume on the syringe.
Increase the water temperature to 55 C (wait about 1 minute for equilibrium to
occur) and record the water temperature and volume on the syringe.
Repeat step 6, by increasing the temperature in the steps of 5 C until 80 C.
Plot a graph of volume (V) versus temperature (C).
Treatment of data:
Part 1 Boyles law
Volume (mL)
20.0
17.5
15.0
12.5
10.0
7.5
5.0
Pressure (kPa)
Calculation:
1. Determine the relationship of volume and pressure and find the proportionality
constant, k.
2. Based on your data, what would be the pressure to be if the volume of the syringe was
increased to 45 mL? Show the calculation steps.
Part 2 Charless law
Temperature(C)
50
55
60
65
70
75
80

Volume (mL)
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Calculation:
1. Determine the relationship of volume and temperature and find the proportionality
constant, k.
2. Based on your data, postulate the x-intercept and y-intercept.

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Topic 5: Thermochemistry Determination of heat of neutralization of hydrochloric

acid by sodium hydroxide
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Introduction:
In adiabatic calorimetry, we try to keep as much as possible of the heat change that is
caused by a reaction of interest confined to the reaction vessel and its content, i.e., we
attempt to keep heat from leaking into and out of the calorimeter, usually by insulating
the reaction vessel. When there is no heat leakage to the surroundings, all the heat
evolved or absorbed by the reaction of interest must remain in the reaction vessel and its
contents, so it raises or lowers the temperature. It is this temperature change that we
measure and relate to the heat evolution or absorption that has occurred.
The relationship between the amount of heat, qs that enters or leaves a system and the
attendant temperature change, T; may be expressed as
qs
C =
T
C = total heat capacity of the system
If the system is composed of several parts, e.g., of a reaction vessel plus the solution it
contains, then the total heat capacity of the system is the sum of the heat capacities of the
individual parts, C = Ci . Since, in the ideal case, no heat is allowed to enter or escape,
the sum of the heat from the reaction (qr) and the heat from the system (qs) must be equal
to zero,
qr + qs = 0
so that,
qr + C T = 0
Heat capacity is a positive quantity. Therefore, if the temperature of the system rises, i.e.,
T is positive, then qr will be a negative quantity.
In practice, it is impossible to make a perfect calorimeter, one which has no heat leakage,
so measuring the temperature change due to the heat from the reaction is complicated by
temperature changes from heat leaking into or out of the calorimeter. By taking these
factors into account and correcting them, a graphical procedure is usually used to obtain
the temperature change T, as shown in the following figure of temperature versus time
for an exothermic reaction.

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Decreasing slope due
to loss of heat to the
calorimeter walls
Room
temperature
Starting time
The initial temperature of the reaction vessel and contents was a little below room
temperature, so heat was leaking into the system. This explains the slow rise in
temperature before the reaction was initiated. After the initial sharp rise in temperature
when the reaction has begun, the temperature began to decrease due to heat loss from the
calorimeter. At first, these readings were a bit erratic, as temperature equilibration was
not yet attained throughout the system.
After some time, the equilibration (and the reaction has completed, the heat loss became
steady and the temperature decreased linearly. Extrapolation of this linear portion of the
curve back to the time when the reaction began, gives a fairly accurate value for the
temperature which would have been attained if the reaction and temperature equilibration
had taken place instantaneously as if that no heat loss has occurred.
Generally, a chemical change is usually accompanied by an evolution or absorption of
energy (e.g. heat); certain physical changes also produce an energy change. The heat of
neutralization of an acid by a base is the energy evolved when 1 mol of the acid is
neutralized by 1 mol of a base, the reaction being carried out in dilute aqueous solution.
For a strong acid and a strong base, the heat of neutralization is effectively constant.
This is because strong acids and strong bases, and the salts they form are all completely
ionized in dilute solution. Thus the reaction between any strong acid and strong base is
simply the formation of unionized water from H+ and OH- ions.
e.g.:
HCl + KOH
KCl + H2O
H+ + Cl- + K+ + OHH+ + OH-

K+ + Cl- + H2O
H2O
H = Heat of neutralization.
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The constancy of the heat of neutralization of any strong acid and any strong base
provides simple, but convincing evidence that strong acids and bases are, in fact,
completely ionized.
The temperature rises accompanying the mixing of a solution of a base with a solution of
acid at the same initial temperature in a calorimeter is caused by the heat released during
the neutralization process.
Joule calorimeter
Digital stop-watch
Thermometer (reading to 0.1 oC)
Hot water bath
Beaker (100 mL)
Materials:
0.5 M Sodium hydroxide, NaOH
0.5 M Hydrochloric acid, HCl
Distilled water
Procedures:
Part 1 Calibration of calorimeter
1. Measure 50 cm3 of distilled water into a calorimeter.
2. Record the temperature of the water (1 minute interval) for 5 minutes.
3. Add another 50 cm3 of water which has initial temperature of 50 oC into the
calorimeter and record the temperature (1 minute interval) for another 10 minutes.
Part 2 Determination of heat of neutralization
Measure 50 cm3 of 0.5 M NaOH solution into the calibrated calorimeter.
Record the temperature of the base every 2 minutes.
Measure 50 cm3 of 0.5 M HCl into another container.
Insert a thermometer and cool or warm slightly until the temperature of the acid is the
same as that of the base.
5. Now add the acid to the base quickly and note the time of mixing.
6. Record the temperature (30 seconds interval) for first 5 minutes and (1 minute
interval) for the next 10 minutes.
1.
2.
3.
4.

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Treatment of data:
Part 1 With 50 cm3 distilled water
Time (minute)
1.00
2.00
3.00
4.00
5.00
Addition of 50 cm3 distilled water
Time (minute)
1.00
2.00
3.00
4.00
5.00
6.00
7.00
8.00
9.00
10.00
Temperature (oC)
Temperature (oC)
(Specific heat capacity of water = 4.184 J g-1 K-1 ; density of water = 1.00 g cm-3)
We can imagine the process that occurs on mixing the hot water with the water already in
the calorimeter as being broken into two parts: the release of enough heat by the high
temperature water reduces its temperature from 50 o C to Tfinal.. Hence,
qr = Mass of hot water (50 oC) x Specific heat of water x Fall in temperature (Tfinal 50oC)
and
qs = [Mass of distilled water x Specific heat of water x Rise in temperature
(Tfinal Tinitial room temp)] + [Heat capacity of calorimeter x Rise in temperature
(Tfinal Tinitial room temp)]
qr + qs = 0
Plot a graph of temperature against time.

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Part 2 With 50 cm3 of 0.5 M NaOH

Time (minutes)
2.00
4.00
6.00
8.00
10.00
12.00
Addition of 50 cm3 of 0.5 M HCl
Time (seconds)
30
60
90
120
150
180
210
240
270
300
360
420
480
540
600
660
720
780
840
900
Temperature (oC)
Temperature (oC)
(Specific heat capacity of water = 4.184 J g-1 K-1 ; density of solution = 1.00 g cm-3)
Assuming the specific heat of the solutions to be the same as that of water, the heat
evolved by the neutralization process is given by
Hneutralization = MNaOH CNaOH T + CCalorimeter T + MHCl CHCl T
Plot a graph of temperature against time.
Calculation:
1. Calculate the heat of reaction (qr) for Part 1.
2. Determine the heat capacity of the calorimeter.
3. Determine the enthalpy of neutralization (Hneutralization) for Part 2.
4. Determine the molar enthalpy of neutralization.
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Topic 6: Reaction kinetics Determination of the activation energy of the reaction

between oxalic acid and potassium permanganate
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Introduction:
Reaction between oppositely charged icons are often very fast but the reaction between
similarly charged ions, e.g. permanganate and oxalate, may proceed at a rate which is
measurable:
2KMnO4 + 5H2C2O4 + 3H2SO4
K2SO4 + 2MnSO4 + 8H2O + 10CO2
or
2MnO4- + 16H + + 5C2O4 2-
K2SO4 + 2MnSO4 + 8H2O + 10CO2
The rate of this reaction is measured by the time taken for the disappearance of the purple
color of the potassium permanganate.
Measuring cylinder, test tube, water bath, stopwatch
Materials:
0.02M Potassium Permanganate
1 M Sulphuric Acid
0.5 M Oxalic Acid
Test tube
Water bath
Measuring cylinder (5mL)
Stopwatch
Procedure:
1. In a test tube, measure 2 cm3 of 0.02 M potassium permanganate and 4 cm3 of 1 M
sulphuric acid.
2. In another test tube, place 2 cm3 of oxalic acid.
3. Place the test tubes in water bath at 35 oC.
4. When the solutions have attained this temperature, pour the oxalic acid into the
acidified permanganate solution and immediately start the time.
5. Record the time taken for the permanganate to decolorize.
6. Repeat the experiment at higher temperatures of 40, 45, 50, 55 and 60 oC.
Treatment of data:
Temperature, T (C)
Temperature, T (K)
1 / T (K-1)
Reaction time, t (sec)
35
40
45
50
55
60
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ln 1/t
Plot a graph of ln 1/t against 1/T.
Calculation:
1. Calculate the activation energy, Ea in J mol -1 according to the Arhenius equation
k = A e -Ea / RT

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Topic 7: Rate law of an iodine clock reaction

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Introduction:
In this experiment you will study the reaction of hydrogen peroxide with iodide ion in the
presence of acid.
H2O2 (aq) + 2 I- (aq) + 2 H3O+ (aq) I2 (aq) + 4 H2O (l)
The rate of the reaction is very much depending on the concentrations. The easiest way to
measure the rate of reaction is by determining the rate of formation of iodine by reaction
between iodine (I2) and thiosulfate ion (S2O32-) to form the tetrathionate ion (S4O62-)
according to:
I2 (aq) + 2 S2O32- (aq) S4O62- (aq) + 2 I- (aq)
The rate of a chemical reaction also depends on temperature, pressure and other physical
characteristics of the reaction surroundings. However, the first consideration a chemist
gives to a chemical reaction is the concentration of the reactants. Thus, chemists often
change the concentration of reactants so that they can study the effect of such changes on
the rate of the reaction.
Graduated pipette(1 mL and 25 mL)
Digital stop watch
Measuring cylinder
250 mL conical flask

Hot water bath
Thermometer
Materials:
0.36 M Sulphuric acid, H2SO4
0.025 M Potassium iodide, KI
0.8 M Hydrogen peroxide, H2O2
0.0025 M Thiosulfate, S2O32Starch solution
Distilled water
Procedures:
Part 1 Measurement of Rate For One Set Conditions
1. To a clean conical flask, add the following in order.
43 cm3 distilled water
35 cm3 0.36 M H2SO4
10 cm3 0.025 M KI
10 cm3 0.0025 M thiosulfate
1 cm3 starch solution
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2. Pipette 1 cm3 of 0.8 M hydrogen peroxide in the fume cupboard. With one eye on a
watch, add the peroxide and noting the time to the nearest second.
3. Note the time at which the thiosulfate is all used up and blue colour appears. Record
the time elapsed.
4. Measure the temperature of the reaction mixture.
5. Repeat the experiment.
Part 2 The Effect of Peroxide
1. Proceed as in Part 1 but
(i) use 2 cm3 peroxide and 42 cm3 distilled water.
(ii) use 0.5 cm3 of peroxide and 43.5 cm3 distilled water.
2. Plot a graph of rate against concentration of peroxide in the 3 mixtures and describe
it. Use axes starting from zero for rate and for [H2O2].
Part 3 The Effect of Iodide
(i) use 20 cm3 KI and 33 cm3 distilled water
(ii) use 5 cm3 KI and 48 cm3 distilled water.
2. Plot a graph of rate against concentration of iodide in the 3 mixtures and describe it.
Use axes starting from zero for rate and for [I-].
Part 4 The Effect of Acid
(i) use 8 cm3 distilled water and 70 cm3 sulphuric acid.
(ii) use 60.5 cm3 distilled water and 17.5 cm3 sulphuric acid.
2. Plot a graph of rate against [H3O+] in the 3 mixtures and describe it. Use axes starting
from zero for rate and for [H3O+].
Treatment of data:
Part 1 Measurement of rate for one set conditions:
Number of trial
Concentration of peroxide (M)
Concentration of iodide (M)
Concentration of sulphuric acid (M)
Concentration of thiosulphate (M)
Time elapsed (s)
Temperature of reaction mixture (oC)
Average time elapsed = _________________________ s

Average rate of reaction of peroxide = _______________________ M s-1
Average rate of reaction of iodide = _________________________ M s-1
Average rate of reaction of sulphuric acid = ___________________ M s-1

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Trimester 1
Part 2 The effect of peroxide:

(i) 2 cm3 peroxide and 42 cm3 distilled water
Number of trial
Time elapsed (s)
Average time elapsed = ______________________ s

Average rate of reaction = ____________________ M s-1
(ii) 0.5 cm3 of peroxide and 43.5 cm3 distilled water
Number of trial
1
Time elapsed (s)
Average time elapsed = _____________________ s

Average rate of reaction = ___________________ M s-1
Part 3 The effect of iodide:
(i) 20 cm3 KI and 33 cm3 distilled water
Number of trial
Concentration of KI (M)
Time elapsed (s)
Average time elapsed = _______________________ s

Average rate of reaction = _____________________ M s-1
(ii) 5 cm3 KI and 48 cm3 distilled water
Number of trial
Concentration of KI (M)
Time elapsed (s)


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Trimester 1
Part 4 The effect of acid:

(i) 8 cm3 distilled water and 70 cm3 sulphuric acid
Number of trial
1
Concentration of sulphuric acid(M)
Time elapsed (s)

(ii) 60.5 cm3 distilled water and 17.5 cm3 sulphuric acid.
Number of trial
1
Concentration of sulphuric acid(M)
Time elapsed (s)
Average time elapsed = ______________________ s

Average rate of reaction = ____________________ M s-1
Calculation:
1. Using Part 2 (i) as an example, show the steps in calculating
(a) concentration of peroxide
(b) average rate of reaction
2. For Part 1,
(a) calculate the number of moles of thiosulfate added to the reaction mixture for use
in reaction
(b) calculate the number of moles of iodine produced by reaction
(c) calculate the rate of reaction (concentration of iodine produced by reaction
divided by the time taken for the blue colour to appear)
3. Based on the results obtained, determine the rate law for this experiment.

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Trimester 1
Topic 8: Determination of pKa of Bromocresol Green
Introduction:
Bromocresol green is a weak acid which dissociates in water according to the equation:
HB- (aq) + H2O B2- (aq) + H3O+ (aq)
yellow
blue
The yellow, acidic form of the indicator is a singly charged anion which can be
represented by the structure:
Br
Br
CH3
Br
C
CH3
OH
Br
SO3Na+
The hydrogen of the phenol group is weakly acidic and dissociates to give the basic form,
a blue coloured, doubly charged anion.
At equilibrium, the pKa of the indicator is related to the pH of the solution by the
equation:
C
pK a pH log 10 HB
C B2
Ka= the equilibrium constant for the dissociation of the acid HBCHB-= concentration of the undissociated form of indicator
CB2-= concentration of the dissociated form of indicator.
The bromocresol green in the acidic solution is completely in its protonated form, HB-. In
the basic solution, it is completely in the unprotonated form, B2-.
Erlenmeyer flask (100 mL)
Graduated pipette (2 mL)
Volumetric flask (100 mL)

Stopper
Pipette (10 mL)
pH meter
UV-Visible Spectrophotometer
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Trimester 1
Materials:
Bromocresol green indicator solution
2 M Hydrochloric acid, HCl
2 M Sodium hydroxide, NaOH
Buffer solution (pH 5)
Distilled water
Procedures:
1. Bromocresol green in basic solution: Put 10 cm3 of 2 M NaOH in a 100 cm3
volumetric flask. Then, pipette 2 cm3 of bromocresol green indicator solution into the
flask. Fill to the mark with distilled water, stopper the flask and mix the contents
thoroughly.
2. Bromocresol green in acidic solution: Put 10 cm3 of 2 M HCl in a 100 cm3
volumetric flask. Then, pipette 2 cm3 of bromocresol green indicator solution into the
flask. Fill to the mark with distilled water, stopper the flask and mix the contents
thoroughly.
3. Bromocresol green in buffer solution: Put 10 cm3 of pH 5 buffer solution in a 100
cm3 volumetric flask. Then, pipette 2 cm3 of bromocresol green indicator solution
into the flask. Fill to the mark with distilled water, stopper the flask and mix the
contents thoroughly. Measure the pH of this solution by using pH meter.
4. Use distilled water as the blank. Measure the spectrum of these solutions from
wavelength 400 630 nm.
Treatment of data:
Bromocresol green in
acidic solution
basic solution
buffer solution
pH
max
Absorbance
Cuvette length = ______________ cm

Wavelength (nm)
Absorbance of bromocresol green in

acidic solution
buffer solution
basic solution
400
410
420
430
440
450
460
470
480
490
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Trimester 1
500
510
520
530
540
550
560
570
580
590
600
610
620
630
Plot a graph of absorbance against wavelength for each of solution with different pH.
Calculation:
1. Determine the isosbestic point for bromocresol green.
2. Calculate the pKa value for indicator using the pH of the indicator/buffer solution.
3. Determine the maximum buffer capacity for the bromocresol green.

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Topic 9: Determination of the percentages of sodium carbonate and sodium

hydroxide in a mixture
________________________________________________________________________
Introduction:
The total alkali (sodium carbonate and sodium hydroxide) present in a mixture is
determined by titration with hydrochloric acid using methyl orange as indicator.
Na2CO3 + 2HCl
2NaCl
H2O
NaOH +
NaCl
H2O
HCl
CO2
To a second portion of the mixture, excess barium chloride solution is added.

Na2CO3 + BaCl2
2NaCl
BaCO3
Thus sodium carbonate is removed from the mixture as insoluble barium carbonate. The
hydroxide ion remaining in solution reacts with the acid during titration. The
concentration of these is determined using phenolphthalein as indicator.
Apparatus:
Burette (50mL)
Pipette filler
Retort stand
Asbestos board
Volumetric pipette (25mL)

Erlenmeyer flasks
Burette clamp
Materials:
Hydrochloric acid, HCl
Mixture of sodium carbonate, Na2CO3 and sodium hydroxide, NaOH in a solution
Barium chloride, BaCl2
Methyl orange indicator
Phenolphthalein indicator
Procedures:
1. Pipette 25 cm3 of the mixture solution into a conical flask.
2. Add a few drops of methyl orange indicator, and titrate with diluted hydrochloric acid
until the yellow color just changes to orange.
4. To another 25 cm3 of the mixture solution, add about an equal volume of barium
chloride solution and one or two drops of phenolphthalein.
5. Titrate the mixture with diluted hydrochloric acid, noting the burette reading when
the solution is decolorized (Take care to run in the acid slowly otherwise some of the
barium carbonate may be acted upon before the end-point is reached).

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Trimester 1
Treatment of data:
(a) Methyl orange as indicator
Titration number
Final reading
Initial reading
Volume Used (cm3)
Average volume of hydrochloric acid required for titration = __________ cm3
(b) Phenolphthalein as indicator
Titration number
Final reading
Initial reading
Volume Used (cm3)
Average volume of hydrochloric acid required for titration = __________ cm3
Calculation:
1. Calculate the respective concentrations of sodium carbonate and sodium hydroxide in
the mixture in the units of g L-1.
2. Determine the percentage of each alkali in the mixture.
(The molecular weights of sodium hydroxide and sodium carbonate are 40 and 106
respectively.)

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Topic 10: Ionic Measurement of the conductivities of strong and weak electrolytes
________________________________________________________________________
Introduction:
Solutions of electrolytes conduct electric current by migration of ions under the influence
of electric field. According to Ohms law,
V=IR
Where V, is the potential difference; I, is the current and R, is the resistance. The term
conductance (L) is generally used for dealing with electrolytes and this is defined as the
reciprocal of the resistance of the solutions, i.e.,
L (ohm -1 or ) = 1 / R
The conductivity (x) may be obtained from
x (-1 cm -1) = d / AR
Where A, and d are the area and separation between the electrodes of the conductivity
cell. The cell constant k of the conductivity cell is defines as
k=d/A
And therefore
x = k. L
Thus, conductivity is the reciprocal of the resistance in ohm of a 1 cm of liquid at a
specified temperature. The molar conductivity of an electrolyte solution is defined as
(-1 mol -1 cm 2) = x / C
Where C = molar concentration
For week electrolytes, the increase of molar conductivity with increasing dilution is
ascribed to increased dissociation of the electrolyte molecules to free ions. For strong
electrolytes, the molar conductivities are higher than those of weak electrolytes at high
concentrations. As the solutions become dilute, the molar conductivities also increase as
in the case of weak electrolytes but the variation is, in general, less steep than for weak
electrolytes.

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Conductivity meter
Volumetric flask (100 mL)
Volumetric pipette (50 mL)
Pipette filler
Beaker (100 mL)

Pasteur pipette
Wash bottle
Materials:
0.1 M Sodium chloride, NaCl
0.1 M Acetic acid, CH3COOH
Distilled Water
Procedures:
1. Calibrate the conductivity meter with known cell constant.
2. Measure the conductivity of 50 cm 3 of 0.1 M acetic acid.
3. Repeat the measurement with 0.0500, 0.0250, 0.0125, and 0.00625M acetic acid
prepared by successive dilution.
4. Repeat with sodium chloride.
5. Measure the conductivity of the distilled water used.
Treatment of data:
Conductivity of distilled water = _________________
Conductivity of electrolytes = Conductivity of solution - Conductivity of distilled water
Tabulate the conductivities as follows:
C (Mol dm-3 )
Conductivity (-1 cm-1 )

CH3COOH
NaCl
0.1000
0.0500
0.0250
0.0125
0.00625
Calculate the molar conductivities and tabulate the results as follows:
Molar Conductivity (-1 mol -1 cm 2)
1/2
-3
C (Mol dm )
CH3COOH
NaCl
Plot a graph of versus C1/2 for each electrolyte.

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Calculation:
1. Show the steps (one example of calculation) in obtaining molar conductivity for each
electrolyte.
2. Determine the conductivity and molar conductivity at infinite dilution (o) for each
electrolyte.
(a) CH3COOH
(b) NaCl
3. The molar conductivity of benzoic acid at infinite dilution is 385 -1 cm2 mol-1 and at
a concentration of 0.0050 mol dm-3 is 40.8 -1 cm2 mol-1. Calculate the pKa of
benzoic acid.

32

Physical Chemistry Experiments

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Physical Chemistry Experiments

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UTAR

FHSC1114 Physical Chemistry

Topic 1: Introductory to laboratory safety and apparatus

Lab manual version 4.0

3. Writing a Scientific Report

Lab manual version 4.0

4. Apparatus and Equipments

Description and Function

Beaker is a simple container for liquids, very commonly

An Erlenmeyer flask (conical flask) is a type of widely

A filtering funnel is a pipe with a wide, often conical

Lab manual version 4.0

A graduated cylinder also referred to as a measuring

A volumetric flask refers to graduated glassware used

Pipettes are used to transfer a specific volume of liquid.

Burette is a vertical cylindrical piece of laboratory

Reagent bottles are used to hold small stocks of reagents

Desiccators are sealable enclosures containing desiccants

Separating funnel also known as separatory funnel or

An electronic balance uses electromagnet to balance the

Lab manual version 4.0

Topic 2: Precipitation of barium (II) sulphate

Topic 3: Determination of the amount of dissolved oxygen in a water sample by

4Mn(OH)2 (s) + O2 + 2H2O

Lab manual version 4.0

Average volume of titrant required for titration = ____________ cm3

Lab manual version 4.0

Topic 4: Gases Boyles Law and Charless Law

Apparatus and Equipments:

Lab manual version 4.0

Part 2 Charless law

Lab manual version 4.0

Lab manual version 4.0

Topic 5: Thermochemistry Determination of heat of neutralization of hydrochloric

C = total heat capacity of the system

Lab manual version 4.0

H+ + Cl- + K+ + OHH+ + OH-

Lab manual version 4.0

Lab manual version 4.0

Lab manual version 4.0

Part 2 With 50 cm3 of 0.5 M NaOH

Topic 6: Reaction kinetics Determination of the activation energy of the reaction

K2SO4 + 2MnSO4 + 8H2O + 10CO2

K2SO4 + 2MnSO4 + 8H2O + 10CO2

Lab manual version 4.0

Topic 7: Rate law of an iodine clock reaction

250 mL conical flask

Average time elapsed = _________________________ s

Lab manual version 4.0

Part 2 The effect of peroxide:

Average time elapsed = ______________________ s

Average time elapsed = _____________________ s

Average time elapsed = _______________________ s

Average time elapsed = _______________________ s

Lab manual version 4.0

Part 4 The effect of acid:

Average time elapsed = _______________________ s

Average time elapsed = ______________________ s

Lab manual version 4.0

Topic 8: Determination of pKa of Bromocresol Green

Lab manual version 4.0

Cuvette length = ______________ cm