Laboratory

Manual
Practical Chemistry
CHL0315 & CHL0325

Prepared by:

Siti Munira Yahaya

Ahmad Afandi Muda

Mohd Azmi bin Sulong

M. Haswaneezal Rizan Azri Department of Chemistry

Centre for Foundation Studies
Nur Diyana Syamim Hasnol International Islamic University Malaysia
 Table of Content

Before Doing the Experiment ii

CHL0315

Experiment 1 The Use of Volumetric Ware and Chemical Balances 2

Experiment 2 Standardization of Solutions 10

Experiment 3 Acid-Base Titration 13

Experiment 4 Rates of Chemical Reaction, A Clock Reaction 17

CHL0325

Experiment 1 Identification of Unknown Organic Compounds 21

Experiment 2 Hess’s Law-Additivity of Heat of Reaction 24

Experiment 3 Le Chatelier’s Principle ‒ Disturbing the Position of Equilibrium 28

Experiment 4 Acid-Base Titration Curve 31

Laboratory Report Sheets

 Practical Chemistry

Before Doing the Experiment

THINGS TO BRING arises about the theory or the method, consult

your instructor. The laboratory supervision and
Every student should have
preparation of the experiments are the
o a marker for labeling responsibilities of the laboratory staff.
o stationeries such as note-book for writing
down data & observations or reference
LABORATORY SAFETY GUIDE
about the experiment; a ruler and a
calculator The laboratory can be but is not necessary a
dangerous place. When intelligent precautions
and a proper understanding of techniques are
EQUIPMENT employed, the laboratory is no more dangerous
All the equipment prepared are in good than any other classroom. Most of the
condition. Every student must keep the table precautions are just common-sense practices.
tidy and clean including all the apparatus. The These include the following:
instructor or the laboratory staff must be 1. Wear approved eye protection (including
informed about any damage done. After splash guards) at all times while in the
completing your experiment, make sure laboratory. (No one will be without it.)
everything is clean, including your table and the Your safety eye protection may be slightly
sink. Your table should be wiped dry. different from that shown, but it must
include shatterproof lenses and side shields
to provide protection from splashes.
CHEMICALS
The chemicals to be used are usually placed
specifically in the laboratory. Use it carefully and
avoid contamination. Some of the hazardous
chemicals are kept in the fume hood. Different
droppers must be used for different chemicals.
After using the dropper, place it back in the
bottle that contained the chemical. Do not mix
the droppers to avoid contamination of
The laboratory has an eyewash
chemicals.
fountain available for your use. In the event
that a chemical splashes near your eyes,
DO NOT TAKE OR USE ANY CHEMICAL you should use the fountain before the
MORE THAN IS NEEDED! material runs behind your glasses and into
your eyes. The eyewash has a ‘panic bar’,
which enables its easy activation in an
INSPECTION emergency.

The instructor will brief about the experiment at 2. Wear shoes at all times. (No one will be
the beginning of each laboratory class. Even admitted without them.)
though this is done, the student himself must 3. Know to find and how to use all safety and
read, understand and be ready with a flow chart first-aid equipment.
of the method or a summarized method before
coming to the laboratory class. If any problem

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Practical Chemistry Before Doing the Experiment

4. Consider all chemicals to be hazardous

unless you are instructed otherwise.
Dispose of chemicals as instructed by your
instructor. Follow the explicit instructions
given in the experiments.
5. If chemicals come into contact with your
skin or eyes, wash immediately with
copious amounts of water and then consult
your laboratory instructor.
6. Never taste anything. Never directly smell 10. Do not perform any unauthorized
the source of any vapor or gas. Instead, by experiments.
means of your cupped hand, bring a small 11. Clean up all broken glassware immediately
sample to your nose. Chemicals are not to and report to the lab assistants.
be used to obtain a ‘high’ or clear your
sinuses. 12. Always pour acids into water, not water
into acid, because the heat of solution will
7. No drinking, eating or chewing in the cause the water to boil and the acid to
laboratory. spatter.
13. Avoid rubbing your eyes unless you know
that your hands are clean.
14. Dispose of insoluble waste such as filter
paper, litmus paper, matches and broken
glasses in the wastebasket, not in the sink.
15. Never return unused chemicals to the
reagent bottles to avoid possible
contamination.
16. When inserting glass tubing or
8. Perform in the fume exhaust hood any thermometers into stoppers, lubricate the
reactions involving skin-irritating or tubing and the hole in the stopper with
dangerous chemicals, or unpleasant odors. glycerol or water. Wrap the rod in a towel
This is a typical fume exhaust hood. and grasp it as close to the end being
Exhaust hoods have fans to exhaust fumes inserted as possible. Slide the glass into the
out of the hood and away from the user. rubber stopper with a twisting motion. Do
The hood should be used when you are not push. Finally, remove the excess
studying noxious, hazardous and lubricant by wiping with a towel. Keep
flammable materials. It also has a your hands as close together as possible in
shatterproof glass window, which may be order to reduce leverage.
used as a shield to protect you from minor
explosions. Reagents that evolve toxic
fumes are stored in the hood. Return these
reagents to the hood after their use.
9. Never point a test tube that you are heating
at yourself or your neighbor. It may erupt
like a geyser.

17. Notify the instructor/lab assistant

immediately in case of an accident no

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Practical Chemistry Before Doing the Experiment

matter how insignificant it may seem. Accuracy and precision

Quick treatment can often prevent
The limitations of both accuracy and precision
infection or other complications from
will contribute to uncertainty in the
occurring.
measurement. The error in a measurement, or
18. Many common reagents, for examples better, the average of several measurements, is
alcohols, acetone and ether are highly the difference between the measured value and
flammable. Do not use them anywhere the true value of the quantity measured.
near open flames.
The smaller the error, the closer the measured value
19. Keep the balance and the area around it is to the true value and the more accurate is the
clean. Do not place chemicals directly on result.
the balance pans. Place a piece of weighing
The true value is sometimes difficult to
paper or a small container/weighing bottle
establish. Generally, it involves applying the
on the pan first, and then weigh your
same measurement technique to an unknown
material. Never weigh an object while it is
sample and to a carefully prepared or analyzed
hot.
standard sample that resembles the unknown
20. Observe all special precautions mentioned as much as possible. Typically, when we make
in experiments. Be neat in your work. If a series of several measurements on the same
you spill something, clean it up sample or replicate samples, we do not get
immediately. exactly the same value for each measurement.
There will be a dispersion (or spread) of the
21. Whenever possible, use hot plates in place
measured values.
of Bunsen burners.
The smaller the spread of values, the more precise
22. Learn the location and operation of fire
will be the average (or mean) value of the
protection devices.
measurements.
23. In case someone’s clothing or hair is on fire,
So accuracy and precision are different
immediately lead the person to the shower
concepts.
and pull the metal ring. Safety showers
generally dump 40 to 50 gallons of water, Accuracy is a measure of how close the measured
which should extinguish the flames. value is to the true value.
Precision is a measure of the reproducibility (or
dispersion) of the measurements.
THE ASSESSMENT OF EXPERIMENTAL
ERRORS The average of several measurements might be
accurate without being very precise, or a set of
Every measurement involves some
measurements might have good
measurement uncertainty (often referred to as
reproducibility, and therefore good precision,
“error,” but not in the normal sense of this term
but the average (or mean) value might not be
as a synonym for “mistake”). Because many
very accurate. Good-quality measurements
generalizations or laws of science are based on
will be both precise and accurate. Figure 1-2
experimental observations involving
shows graphically what is meant by accuracy
quantitative measurements, it is important for
and precision. We’ve said that we determine
a scientist (or a student of a quantitative
accuracy by comparison with standards. How
science) to take into account any limitations in
do we measure precision? By making several
the reliability of the data from which
measurements and determining the spread of
conclusions are drawn. In the following section,
the measurements. How many measurements?
we will discuss different kinds of errors —
Somewhere between 3 and 30. Three is a
systematic, random, and personal errors — and
minimum for making a rough estimate of the
assess the quality of a measurement by
precision. Thirty measurements would give
considering its accuracy and precision.
you a decent estimate. A single individual
seldom has time in a general chemistry lab to
make 30 replicate measurements of the same

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Practical Chemistry Before Doing the Experiment

quantity, but we might aggregate the results of miscalibrated scale on a ruler, for example,
all the students in a lab section or in the whole would cause a systematic error in the
class in order to get a better estimate of the measurement of length.
precision.
Similarly, in Figure 1, the B group of
measurements shows evidence of a systematic
error, Perhaps due to a misunderstanding of
how to read the position of the meniscus in a
graduated cylinder or pipet. If the volume is
read at the top rather than the bottom of the
curved meniscus, the measured volume is
systematically too small.

Random Errors
If a measurement is made a large number of
times, you will obtain a range of values caused
by the random errors inherent in any
measurement process (or deviations in a
manufacturing process). For random errors,
small errors are more probable than large
errors and negative deviations are as likely as
positive ones.

Personal Errors
To the types of errors already described —
FIGURE 1 The results of an acid–base titration systematic and random — we might add a third
exercise are shown for four individuals. Each person category, the personal error, or blunder. Such
titrated six nominal 10-mL samples of the same errors are all too common in student work.
0.0400 M acid solution with 0.250 M NaOH Thus, if the numbers on a scale are misread,
(sodium hydroxide) dispensed from a 2-mL recorded incorrectly, or if part of a solution is
microburet. The horizontal position of the black dots spilled in a titration, the result will contain an
shows the measured titration volumes. The vertical error. Careful work will not contain any
columns of two or three black dots mean that those blunders, and any work suspected of
measured volumes were the same. The results of containing one should be repeated
individual A were both accurate and precise, while
those of B were precise but not accurate. The results
of C were accurate but not precise. The results of D
were neither accurate nor precise. (There is a
systematic error combined with substantial random
errors.)
TYPES OF ERRORS
Systematic Errors
Errors are of two general types, systematic
(determinate) and random (indeterminate). A
systematic error causes an error in the same
direction in each measurement and diminishes
accuracy, although the precision of the
measurement may remain good. A

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Practical Chemistry Before Doing the Experiment

FIGURE 2: Some common laboratory equipment

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Practical Chemistry Before Doing the Experiment

FIGURE 2: Continued

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Practical Chemistry Laboratory Techniques

Laboratory Techniques

1 TRANSFERRING OF CHEMICALS
SOLIDS
A number of steps are involved when transferring solids from reagent bottle to reaction
flask or weighing paper. If you are using weighing paper, the paper should sharply crease
down the middle, so that chemical can pour off more easily.
▪ Read the label and make sure that you have the proper reagent bottle.
▪ Tilt the sealed bottle until some chemical gets near the bottle’s mouth.
▪ Remove the bottle’s cap. It is generally a bad idea to lay the cap on a bench top, due to
the possibility of contamination. (If the bottle’s cap is flat, it can be safely set upside
down). Hold the cap in the same hand as the bottle.
▪ Center the bottle over the reaction flask or weighing paper. Gently roll the bottle, until
the desired amount of solid has been transferred (Figure 1.1 a). Alternatively, the
chemical can be scooped from the bottle using a spatula (Figure 1.1 b). The spatula is
then tapped until the desired amount of solid has been transferred (Figure 1.1 c).

Never use the same spatula to obtain different chemicals unless the spatula has been
carefully cleaned and dried in between.

LIQUIDS
Decanting, or pouring of liquids, has two major functions in the laboratory. The first is to
simply measure out a quantity of liquid, usually from a reagent bottle. The second is pouring
off a supernatant liquid, to separate it from a precipitated solid.
▪ Read the label and make sure that you have the proper reagent bottle.
▪ Remove the bottle’s stopper. It is generally a bad idea to lay the stopper on a bench top,
due to the possibility of contamination. Hold the stopper in the same hand as the bottle.
▪ Pour the liquid into the desired reaction flask, preferably down a glass rod (Figure 1.2).

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Figure 1.1: Proper method of transferring solids:

(a) Rolling the bottle to transfer a solid.
(b) Use of a spatula to remove a solid from a bottle.
(c) Tapping the spatula to deliver the solid.

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Practical Chemistry Laboratory Techniques

Figure 1.2: Proper method for pouring liquids

▪ Do not pour from a wide-mouthed bottle into a narrow- mouthed container. This is
a major cause of spills.
▪ When decanting (pouring off) a liquid from a solid, it is best to let the solid settle to
one side of the container. This is most easily accomplished by placing the container at
a sharp angle (in a secure location) while the solid is settling.

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Practical Chemistry Laboratory Techniques

2 WEIGHING
▪ Never move a balance without the laboratory instructor’s approval. Some types of
balances are easily thrown out of adjustment if they are improperly moved,
necessitating an expensive repair.
▪ Chemicals should never be placed directly on the balance pan. If any chemical is spilled
on or near a balance, clean it up right away. Most chemicals are corrosive and can cause
a balance to malfunction.
▪ Objects to be weighed should be dry and at room temperature. If the sample is not dry,
its mass will decrease with time due to evaporation of water. If it is not at room
temperature, it will generate air currents as it heats or cools the air around it, and this
will cause inaccurate or unsteady readings.
▪ If a digital balance drifts away from a zero reading, merely push the tare bar (on the
front of the balance). Place the object to be weighed on the balance pan. When the
reading come to a constant value, the weight of the object can be read directly.
(Figure 2.1)

Figure 2.1: Electronic balance

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Practical Chemistry Laboratory Techniques

3 LIQUID VOLUMES

PIPETTE
When reagent, solvent, or solution needs to be accurately measured, it is convenient to use a
pipette.
▪ NEVER use mouth suction to draw any liquid in the pipette! Serious injury may
result if this advice is not followed. The technique of using a pipette with a pipette
pump / rubber bulb is shown in Figure 3.1 a.
▪ When making a reading (Figure 3.1 b), be sure to have your eye at the same level as
the meniscus (the curved surface of a liquid) to avoid problems due to parallax. The
meniscus is always read at the curve center.
▪ Take care when reading the volume. Graduated pipettes and burettes read from 0 at
the top to a maximum at the bottom, whereas graduated cylinders go from 0 at the
bottom to the maximum at the top.

Figure 3.1 a: A typical volumetric pipette, rubber bulbs, and the pipette-filling technique

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Practical Chemistry Laboratory Techniques

Figure 3.1 b: Reading the meniscus

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Practical Chemistry Laboratory Techniques

VOLUMETRIC FLASK
Volumetric flasks (Figure 3.2) should be used as the container when the concentration of the
solution being prepared must be very accurate. There is only one graduation which is etched
on the neck of the flasks (frequently referred to as “the mark”). When the meniscus is exactly
on the line, the flask contains exactly the calibrated volume.
▪ The flask should be rinsed with solvent before use.
▪ To prepare a solution, partially fill the volumetric flask with solvent, add the
appropriate amount of solute. Swirl to dissolve and mix, and then fill to a little below
the mark with additional solvent. The last few drops of solvent should be added with
a dropper. If the solvent is added too quickly, the meniscus may wind up above the
mark. The entire solution must then be discarded.
▪ When mixing the contents of the volumetric flask, be certain to hold both the flask and
the stopper.
▪ Filled flask should not be held by the neck, as there are too heavy for the glass in the
flask neck to support. Broken flasks and severe cuts can be the result of improper
shaking.

Graduation mark

Figure 3.2: Volumetric flask

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4 HEATING METHOD
▪ When heating glass containers over a burner flame, use wire gauze square with a

nonflammable ceramic center as a support.

▪ Never heat thick-walled vessels, such as filter flasks or volumetric flasks.

▪ When heating liquids in small test tubes, always heat from the top to bottom to avoid

explosive boiling of the liquid. (Figure 4.1). Better still is to use a hot water bath.

▪ Never heat the flammable object over an open flame.

▪ Be aware that most solvent vapours are denser than air and will sink and flow along

countertops and into sinks. They may even be ignited by a burner some distance away.

▪ When heating solution containing solids, especially finely divided solids, be sure to stir

continuously to avoid bumping. Never use a thermometer as a stirring rod.

▪ When boiling a liquid, it is often wise to use boiling chips / bumping granules. These

sit at the bottom of the container, promote local boiling, and prevent bumping. Always

use fresh boiling chips.

▪ Never heat a closed container.

▪ Heat side of test tube gently to avoid bumping.

Figure 4.1: Proper way of heating a test tube

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Laboratory Report

THE LABORATORY REPORT

A lab report must be submitted after each (c) Data Analysis
experiment. Depending on the experiment, the
▪ The analysis of data, the
report can be individual report or group report.
manipulation of data,
You should do your own report. Discussions
calculation, graph and others.
are allowed but your report must be different.
Calculation
Copying other report or cheating of data is
forbidden and strict action will be taken. ▪ Formula used must be shown.

The laboratory report among other things ▪ Use the correct significant
should have: figures and the correct unit.

(a) The objective(s) of the experiment. Graph

(b) Data & Results ▪ Graphs showing the pattern or

the relationship or predicting
▪ Observations (measurements,
information.
physical changes).
(d) Discussion
▪ Use the correct significant figures
and the correct unit. ▪ Statement about scientific facts
and theories learnt related to the
Examples:
experiment.
(i) Physical Chemistry
▪ Explanation about observation.
Table 1: For organic chemistry, write the
equation for each reaction that
Volume of acid used to neutralize a base.
occurs.
1 2 ▪ Percentage of error/difference.
▪ Sources of error.
Final volume (mL) 24.10 48.30
▪ Precautionary steps.
Initial volume (mL) 0.00 24.10
(e) Conclusion
Volume of acid ▪ Must be brief, accurate and
24.10 24.20
used (mL) reflect on the objectives of the
experiment.
(f) Reflection
(ii) Organic Chemistry
▪ Islamic values and teaching
from Al-Quran and Hadith or
Observation
quotations from books or
Test journals of Islamic scholars
Unknown Unknown Unknown
X Y Z related to the experiment or
scientific theories under study.
No
Yellow Yellow (g) Bibliography (APA style)
yellow
Brady’s orange orange
orange ▪ Author’s name, title of the
Test is is
is book/journals, edition/volume
formed formed
formed number, publisher and year of
publication, relevant pages.

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Organic Compound Experiment 1

1
EXPERIMENT

Identification of Unknown Organic

Compound
IN THIS EXPERIMENT, YOU WILL

▪ Determine the classes of alcohol by using the Lucas Test

▪ Identify the carbonyl compound by using Brady’s, Tollen’s and Fehling’s Test.
▪ Identify the methyl carbonyl and methyl carbinol compounds by using the Iodoform Test

INTRODUCTION
Alcohols are organic compounds in which, as their functional group, one or more
hydrogen atoms in an alkane have been replaced by a group of – OH (hydroxyl).
Alcohols fall into various classes depending on how the -OH group is positioned
on the carbon atom chain. Alcohol can be oxidized to aldehyde, ketone, and
carboxylic acid. The product formed from the oxidation depends on the classes of
alcohol used as reactant.

Aldehydes and ketones are carbonyl compounds. They contained a carbonyl

group; a double bond of carbon-oxygen, (C=O). Oxygen is far more
electronegative than carbon, and thus has a strong tendency to pull electrons
towards itself in a carbon - oxygen bond. That makes the bond between carbon
and oxygen extremely polar. Nucleophiles can attack the partially positive carbon-
atom in the carbonyl group. Aldehydes have the RCHO structure, in which R is
an alkyl or aryl group. The hydrogen atom attached to the carbonyl group leads
to different oxidation behavior in aldehydes compared to that seen with ketones.
Ketones meanwhile have the RR'CO structure where R and R' are an alkyl group
attached to both ends of carbon in a carbonyl group.

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Organic Compound Experiment 1

In this experiment, several tests will be conducted to identify the class of alcohol
and to determine the carbonyl compound.

a) Classification of alcohols can be determined by using Lucas reagent through

different reactivity with a different rates.

b) An organic compound is a carbonyl compound if its forms an orange or yellow

precipitate when sample is tested with Brady’s reagent; 2,4-
dinitrophenylhydrazine (2,4-DNP),

c) Tollen’s test is used to identify whether the carbonyl compound is an aldehyde

or ketone.

d) Fehling’s test is commonly used to differentiate between aldehyde and ketones.

Aldehydes can be oxidized by Cu2+ in the presence of strong base to form
carbonic acids.

e) The Iodoform test is used to determine whether the carbonyl and alcohol
compound has methyl carbonyl group

H3C
C O

or;

methyl carbinol group

OH

H3C C

CHEMICALS Unknown X, Y, Z, Lucas reagent, 2,4-dinitrophenylhydrazine (Brady’s reagent),

dilute H2SO4(aq), K2Cr2O7(aq), Tollen’s reagent, Fehling’s reagent, 0.10 M
iodine(aq), 1.0 M of NaOH(aq), NH3(aq) and AgNO3(aq).

APPARATUS Test tubes, test tube rack, hot water bath, dropper

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Organic Compound Experiment 1

EXPERIMENTAL PROCEDURE

Perform the following tests on unknown X, Y, and Z compounds, consisting of

Alcohol and Carbonyl
alcohol and carbonyl compounds. Identify the functional group of these
Compounds
unknown. Record each test observation and propose the possible structure for
each compound.

Procedure.
You will conduct five tests in this experiment. For each test, you will need three
test tubes. Label it as X, Y and Z

1. Lucas test
Into each of the three labelled test tubes, place 2 mL of Lucas reagent.
Then, add 3 – 4 drops of sample X, Y and Z into the respective test tube.
Close the test tube and shake vigorously with stopper. Keep the solution
transparent and homogeneous at room temperature.

2. Brady’s test
Place 2 – 3 drops of sample X, Y and Z into the respective labelled test
tubes. Then, add 5 drops of Brady’s reagent into the test tube.

3. Tollen’s test
Into each of the three test tubes, add 5 drops of ammonia. Next, add silver
nitrate, drop by drop until a grey solution is formed. Then, add 5 drops
of the sample X, Y and Z into the respective test tube and warm in the hot
water bath if necessary.

4. Fehling’s test
Mix 10 drops each Fehling’s solution A and solution B in a clean test tube
followed by adding 5 drops of sample X. Warm the mixture gently in the
hot water bath for 10 minutes. Replicate the same procedure for sample Y
and Z.

5. Iodoform test
Add 5 drops of sample X to 5 mL of iodine aqueous in the labelled test
tube. Carefully add NaOH aqueous until almost discharged from the
iodine colour. Warm the mixture for 2 - 3 minutes in the hot water bath.
Refrigerate the test tube and record the observation. Replicate the same
procedure for sample Y and Z.

DATA
Record the observations in Table 1.1 of your lab report sheet.
RECORDING

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Hess’s Law Experiment 2

2
EXPERIMENT

Hess's Law‒ Additivity of Heat of

Reaction
IN THIS EXPERIMENT, YOU WILL

▪ Study on how the enthalpy change of the following three reactions are related as stated by the
Hess’s Law.

INTRODUCTION Hess’s Law states that the overall enthalpy change in a chemical reaction is
constant, and not dependent on the route taken. When reactants A and D are
changed into product C by Route 1, or by Route 2 (A change to B and B reacts with
D to produce C), then according to Hess’s Law the enthalpy change of reaction in
route I equal to the enthalpy change of the reaction in route II changed into product
C by Route 1, or by Route 2 (A change to B and B reacts with D to produce C), then
according to Hess’s Law the enthalpy change of reaction in route I equal to the
enthalpy change of the reaction in route II .
Route 1

A + D C
∆H1

∆H2 ∆H3

B + D

Route 2

A+D → C : ∆H1
A+D → B+D : ∆H2
B+D →C : ∆H3
 ∆H1 = ∆H2 + ∆H3
In this experiment, you will study on how the enthalpy change of the following three
reactions are related as stated by the Hess’s Law. The reactions are:
(i) Solid sodium hydroxide dissolves in water producing an aqueous solution of
ions.
NaOH(s) → Na+(aq) + OH-(aq)

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Hess’s Law Experiment 2

(ii) Solid sodium hydroxide reacts with aqueous hydrochloric acid producing water
and an aqueous solution of sodium chloride.

NaOH(s) + H+(aq) + Cl-(aq) → H2O(l) + Na+(aq) + Cl-(aq)

(iii) Solutions of aqueous sodium hydroxide and hydrochloric acid react producing
water and aqueous sodium chloride.

Na+(aq) + OH-(aq) + H+(aq) + Cl-(aq) → H2O(l) + Na+(aq) + Cl-(aq)

CHEMICALS Solid sodium hydroxide (NaOH), 1.00 M NaOH(aq), 0.500 M HCl(aq), distilled

APPARATUS PASPORT Xplorer GLX, base and support rod, stainless steel temperature probe,
utility clamp, stirring rod or magnetic stirrer and stir bar, 400 mL beaker,
Styrofoam cup and lid and graduated cylinder, 100 mL

EXPERIMENTAL PROCEDURE
A. Sensor You do not need to calibrate the sensor.
Calibration and Procedure
Equipment Setup
1. Use a base and support rod. Place the stir plate on the base. Place a
Styrofoam cup in a 400 mL beaker as shown in Figure 2.1. Then use a
clamp and a slit stopper to support a temperature sensor so that it is
close to the bottom of the cup, and it will not interfere with the stir bar
that you would put into the cup.
Note: You will use this equipment set up for experiment in Part B, C
and D.

Figure 2.1
Setup of Calorimeter

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Hess’s Law Experiment 2

B. Data Recording ‒ Procedure

Solid NaOH and 1. Measure out 100.0 mL of water in a graduated cylinder and pour it into a
Water styrofoam cup. Turn on the magnetic stirrer and begin the stirring of
water.
2. Weigh out approximately 2.000 g of solid sodium hydroxide.
NOTE: Since sodium hydroxide absorbs moisture from the air, weigh it
and proceed to the next step without delay. Caution: Handle the NaOH
and resulting solution with care.
3. When everything is ready, press (start button) to begin recording the
temperature.
4. After about 10 seconds, add the solid sodium hydroxide into the cup of
water.
(Observe the change in temperature on the Graph display)
5. Observe the temperature for 200 seconds or until a maximum
temperature has been reached and the temperature starts to drop.
6. As soon as the temperature begins to drop after reaching a maximum,
press again to end data recording.
7. Remove the Temperature Sensor from the cup, rinse and dry the sensor.
8. Dispose the solution as directed. Rinse and dry the cup and stir bar.

C. Data Recording ‒ Procedure

Solid NaOH and 1. Measure 100.0 mL of 0.500 M hydrochloric acid in a graduated cylinder
0.500 M and pour it into the styrofoam cup. Re-clamp the temperature sensor in
Hydrochloric Acid position to measure the temperature of the solution. Turn on the magnetic
stirrer and begin the stirring of HCl(aq) solution.
2. Weigh out approximately 2.000 g of solid sodium hydroxide.
3. When everything is ready, press (start button) to begin recording the
temperature.
4. After about 10 seconds, add the solid sodium hydroxide into the
styrofoam cup of HCl(aq) solution.
(Observe the change in temperature on the Graph display)
5. Observe the temperature for 200 seconds or until a maximum
temperature has been reached and the temperature starts to drop.
6. As soon as the temperature begins to drop after reaching a maximum,
press again to end data recording.
7. Remove the Temperature Sensor from the cup, rinse and dry the sensor.
8. Dispose the solution as directed. Rinse and dry the cup and stir bar.

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Hess’s Law Experiment 2

D. Data Recording ‒ Procedure

Aqueous Sodium 1. Measure 100.0 mL of 0.500 M HCl(aq) in a graduated cylinder and pour it into
Hydroxide and the styrofoam cup. Re-clamp the temperature sensor in position to measure the
Aqueous temperature of the solution. Turn on the magnetic stirrer and begin the stirring
Hydrochloric Acid of HCl(aq) solution.
2. Measure out 50.0 mL of 1.00 M NaOH(aq) into a graduated cylinder.
3. When everything is ready, press (start button) to begin recording the
temperature.
4. After about 10 seconds, add the aqueous sodium hydroxide solution into the
cup of HCl(aq) solution.
(Observe the change in temperature on the Graph display)
5. Observe the temperature for 200 seconds or until a maximum temperature has
been reached and the temperature starts to drop.
6. As soon as the temperature begins to drop after reaching a maximum, press
again to end data recording.
7. Remove the Temperature Sensor from the cup, rinse and dry the sensor.
8. Dispose the solution as directed. Rinse and dry the cup and stir bar.
CAUTION: Make sure that both solutions are at approximately the same
temperature. Handle the HCl(aq) solution and NaOH(aq) solution with care.

DATA RECORDING
Record data and calculations in Table 2.1 as you complete your analysis.
1. Fill in row 2- 6 of your data table.
2. In the Graph display, press to best view the data.
3. From the F3 Tools menu, select the Smart Tool. Use the Smart Tool to
determine the initial temperature for each run of data and record the value in
your data table.
4. From the F3 Tools menu, select Statistics to find and record the maximum
temperature for each data run.

CALCULATIONS

1. Determine the temperature change, ∆T for each reaction.

2. Calculate the heat of reaction, q for reactions (i), (ii) and (iii) by using the
formula:
qrxn = -qsoln = -msoln x csoln x ∆Tsoln
(Assume c of solution = c of water = 4.18 J/g°C)
Convert joules, J to kilojoules, kJ in your final answer.
3. Calculate moles of NaOH(aq) used for reactions (i), (ii) and (iii).
4. Use the heat of reaction and the number of moles to determine the enthalpy
change, ∆H of NaOH in each of the three reactions.

Department of Chemistry 8
Hess’s Law Experiment 2

5. To verify the results of the experiment, combine the enthalpy change, ∆H for
Reaction (i) and Reaction (iii).
This sum should be similar to the enthalpy change ∆H for reaction (ii).
6. Using the value in reaction (ii) as the theoretical value and the sum of reactions
(i) and (iii) as the experimental value, find the percent difference for the
experiment.
Note : Assume density of solution = density of water = 1.0 g/mL

Department of Chemistry 9
Le Chatelier’s Principle Experiment 3

EXPERIMENT
3
Le Chatelier's Principle ‒ Disturbing the
Position of Equilibrium
INTRODUCTION

Many chemical reactions do not go to completion. As soon as some product

molecules are formed, they react with one another to form reactant molecules. In
these reactions, there will be measurable amounts of reactants and products even
after a considerable period of time. Equilibrium is established, and the ratio of
products to reactants will remain constant if the temperature is kept constant. It
is possible to shift the equilibrium in the desired direction by applying a stress to
the system. This process is explained by Le Chatelier's Principle that states,
"When a system at equilibrium is subjected to a stress, the system will react so as
to relieve the stress." Some examples of stresses that can be applied to a system
are changes in concentration (both increasing and decreasing), pressure (for
systems involving gases), and temperature.
Consider the following hypothetical reversible reaction:

A + B ⇌ C + heat

A reversible reaction will reach equilibrium when the rate of the forward
reactions equals to the rate of reverse reaction. At this stage, any changes that
occur cannot be seen. However, this does not mean that the reactions have
stopped. The reaction still occur, but with at the same rate.
According to this expression, the reactants A and B react to produce product C
and liberate a quantity of heat. Reactions that give off heat as a product are called
exothermic reaction. Reactions that absorb heat (heat is a reactant) are called
endothermic reaction. At equilibrium, the rate at which A and B react to form C
and liberate heat is equal to the rate at which C absorb heat, and decomposes to
form A and B. In short at equilibrium, the rates of the forward and reverse
reactions are identical. Under such equilibrium conditions, the concentrations of
A, B and C in the reaction mixture must remain constant with time. A change in
equilibrium can be determined if one or more of the substances change in color
or change phases such as precipitation.
When the concentration of any substances in an equilibrium mixture is changed,
the equilibrium will move either forward or reverse to restore equilibrium. For
example, some A are added to the equilibrium system. The resulting stress can
be relieved by eliminating the excess A. This is accomplished when some B reacts
with a part of the added A to form C. This process will occur until the rates of
the forward and the reverse reactions are once again equal. The new equilibrium
will be characterized by a higher concentration of A and C, and a lower

Department of Chemistry 28
Le Chatelier’s Principle Experiment 3

concentration of B than the original; thus the equilibrium has shifted toward the
right.
If the original equilibrium were heated, some of the excess heat would ease the
resulting stress by utilizing it. That is accomplished when C reacts to form A and
B with heat. Therefore, the balance will shift to the left and the new equilibrium
will be characterized by higher concentrations of A and B, and a lower
concentration of C than the original.

Potassium nitrate, 0.100 M potassium dichromate, 5.25 M sulfuric acid, 6.00 M

CHEMICALS
sodium hydroxide, 0.100 M iron (III) chloride, 0.100 M potassium thiocyanate,
0.100 M sodium hydroxide, 0.100 M silver nitrate, solid potassium chloride,
distilled water, and ice.

Test tubes, test tube rack, beakers, dropper, 10.0 mL measuring cylinder.
APPARATUS

EXPERIMENTAL PROCEDURE

A. Effect of Procedure
Temperature On
A Physical Change The equilibrium is shown by the following equation:
KNO3(s) ⇌ K+(aq) + NO3− (aq) ∆H = +ve

Place 2.0 - 3.0 mL of a saturated potassium nitrate solution in a test tube. Add
one crystal of potassium nitrate to a solution to act as a seed crystal. (It should
not dissolve. If it does, the solution was not saturated). Immerse the test tube in
a beaker of ice water for 10 minutes and record the result. Remove the test tube
from the ice water, wipe it dry, and place it in the test tube rack. Note what
happens as the solution warms to room temperature.

B. Effect of The chromate/dichromate equilibrium is illustrated by the following equation:

Concentration on 2 CrO4 2- (aq) + 2 H+(aq) ⇌ Cr2O72− (aq) + H2O(l)
Chemical System
The chromate, CrO4 2-, is yellow in color, while the dichromate, Cr 2O72- is orange.
The difference in color between the two species allows one to determine whether
the reaction shifts toward products (turns orange) or shifts toward the reactants
(turns yellow).
Procedure
Place into each three test tubes 10 drops of 0.100 M K2Cr2O7. The first test tube is
the control. To the second test tube, add 2 drops of 5.25 M H 2SO4 (aq), mix and
record the results. To the third test tube, add 2 drops of 6.00 M NaOH (aq), mix
and record the results. Next add 4 drops of the 5.25 M H2SO4 (aq) to the third test
tube. Mix and record the results.

Department of Chemistry 29
Le Chatelier’s Principle Experiment 3

C. Effect of Procedure
Common-Ion on The ferric ions, thiocyanate ions and iron (III) thiocyanate ions equilibrium is
Chemical System illustrated by the following equation:
Fe3+(aq) + SCN−aq) ⇌ [Fe(SCN)]2+(aq)

For the three ions, Fe3+ is pale yellow, SCN- is colorless, and [Fe(SCN)]2+ is blood
red.
Add 1.0 mL of 0.100 M iron (III) chloride (FeCl3) solution and 1.0 mL of 0.100 M
potassium thiocyanate (KSCN) solution to 50.0 mL of distilled water. Shake to
mix and note the color. This is the test solution.
Pour about 5.0 mL of the test solution into each of four test tubes. The first test
tube is the control. To the second test tube, add about 20 drops of 0.100 M iron
(III) chloride and mix. To the third test tube, add about 20 drops of 0.100 M
potassium thiocyanate and mix. To the fourth test tube, add about 1.0000 g of
solid potassium chloride and shake to dissolve. Note any changes in color and
compared with your control.

DATA RECORDING Record the observations in Table 3.1, Table 3.2 and Table 3.3 of your lab
report sheet.

Department of Chemistry 29
30
Acid-Base Titration Curve Experiment 4

4
EXPERIMENT

Acid-Base Titration Curve

IN THIS EXPERIMENT, YOU WILL

▪ Plot the titration curve

▪ Calculate the unknown molarity of acetic acid
▪ Determine the pH of solution at equivalence point using the plot

INTRODUCTION Acid-base titration curves are graphs that show the successive pH values that
occur during the titration. Titration curve for the titration of weak acid with the
strong base is shown in Figure 4.1 below.

Figure 4.1 An acid-base titration curve resulting from the titration of a solution of weak
acid with strong base.
A titration is a technique where a solution of known concentration is used to
determine the concentration of an unknown solution. An indicator is an organic
molecule whose color is different when in acid and in base and is used to monitor
the equivalence point of a titration or the pH of solution.
From the titration curve we can determine the equivalence point by using the
following graphical procedure. Firstly, two straight lines (line 1 and line 2) should
be drawn as shown in Figure 4.2, below. Then, obtained two intersection points,
labeled as A and B.

Department of Chemistry 31
Acid-Base Titration Curve Experiment 4

Figure 4.2 A method for locating the equivalence point.

The equivalence point will be located at the midpoint of the vertical line between
A and B.
For this experiment, ethanoic acid (CH3COOH), a weak acid will be titrated with
sodium hydroxide (NaOH), a strong base. The pH change can be observed using
a pH meter or predicted using basic chemical calculations.
The reaction involved in this experiment can be represent as follow:
CH3COOH(aq) + NaOH(aq) → CH3COONa(aq) + H2O(l)
The Ka for acetic acid is 1.8 x 10-5.

CHEMICALS 25.0 mL of acetic acid, 0.1000 M NaOH and phenolphtalein

APPARATUS PASPORT Xplorer GLX, pH sensor, magnetic stirrer and stir bar, retort stand,
clamp, burette and 150 mL beaker.

EXPERIMENTAL PROCEDURE

APPARATUS Procedure
SETUP 1. Place a clean 150 mL beaker on the magnetic stirrer and add in the stirring bar.
Use a clamp to attach the pH electrode.
2. Use a burette clamp to attach a clean burette to the retort stand above the
beaker. Ensure the burette stopcock is closed.
3. Pipette 25.0 mL of an unknown molarity of acetic acid, CH3COOH into the 150
mL beaker.
4. Add 1-2 drops of phenolphthalein indicator into the acetic acid solution.
5. Fill in 0.1000 M NaOH solution into the burette.

Department of Chemistry 32
Acid-Base Titration Curve Experiment 4

GLX Setup Procedure

1. Connect the Chemistry Sensor to Port #1 on the GLX.
2. Connect the pH electrode to the Chemistry Sensor.
3. From the Home screen, press to open the Digits Display.
4. Press to turn on the active fields. Press again and select pH from the
list of measurements.

DATA Procedure
RECORDING 1. Titrate the CH3COOH (aq) solution using NaOH (aq) according to Table 4.1
and Table 4.2 in your lab report sheet. Be careful to stop exactly at each volume
stated.
2. Turn on the magnetic stirrer and adjust the stirring rate to a moderate speed
(without splashing).
(You must make sure that the solution is completely mixed before
determining the pH).
3. Record the pH of the solutions in Table 4.1 and Table 4.2 of your lab report
sheet.
4. Use a graph paper to plot the titration curve.

Department of Chemistry 33
32
 CENTRE FOR FOUNDATION STUDIES DEPARTMENT OF CHEMISTRY
INTERNATIONAL ISLAMIC UNIVERSITY MALAYSIA CHL0325

___________________________________ _______________ _________ ________

name matric no. section experiment date

IDENTIFICATION OF UNKNOWN ORGANIC

EXPERIMENT 1 COMPOUND 1
OBJECTIVE

Table 1.1 (data): Unknown Compounds

Observation
Test
Unknown X Unknown Y Unknown Z

1 Lucas Test

2 Brady’s reagent

3 Tollen’s reagent

4 Fehling’s reagent

5 Iodoform test

Department of Chemistry 31
Table 1.2 (data and report): Unknown Compound

Draw the complete possible structure of the

Compound
unknown compound

1 X

2 Y

3 Z

Department of Chemistry 32
 CENTRE FOR FOUNDATION STUDIES DEPARTMENT OF CHEMISTRY
INTERNATIONAL ISLAMIC UNIVERSITY MALAYSIA CHL0325

___________________________________ _______________ _________ ________

name matric no. section experiment date

HESS’S LAW –
EXPERIMENT 2 ADDITIVITY OF HEAT OF REACTION 2
OBJECTIVE

RESULTS
Table 2.1 (data and report)

Reaction (i) Reaction (ii) Reaction (iii)

Mass of solid NaOH(s)

Volume of NaOH(aq) (mL)

Volume of water (mL)

Volume of HCl(aq) (mL)

Mass of solution (g)

Final temperature, T2 (°C)

Initial temperature, T1 (°C)

Change in temperature, ∆T (°C)

Heat of reaction, q rxn (kJ)

Moles of NaOH (mol)

∆Hrxn (kJ/mol)

Department of Chemistry 1
CALCULATIONS
1. (a) Draw an energy cycle to represent the relationship of the three reactions you have
conducted.

(b) Use your energy cycle drawn above to calculate the heat (∆H/mol) for reaction (ii).

2. Calculate the percentage difference for the experiment by using the value in reaction (ii) as the
accepted value and the sum of reaction (i) and reaction (iii) as the experimental value.

Department of Chemistry 2
 CENTRE FOR FOUNDATION STUDIES DEPARTMENT OF CHEMISTRY
INTERNATIONAL ISLAMIC UNIVERSITY MALAYSIA CHL0325

___________________________________ _______________ _________ ________

name matric no. section experiment date

LE CHATELIER’S PRINCIPLE –
EXPERIMENT 3 DISTURBING THE POSITION OF EQUILIBRIUM 3
OBJECTIVE

RESULTS
A. Effect of Temperature Change on a Physical System
Table 3.1 (data)

Conditions Observations

Cooling to 0C

Warming to room temperature

B. Effect of Concentration on a Chemical System

Table 3.2 (data)

Test
Conditions Observations
tube

1 Equilibrium without stress

2 Addition of H2SO4(aq)

3 Addition of NaOH(aq)

Addition of H2SO4(aq) to the solution

3
that was added NaOH(aq)

Department of Chemistry 1
C. Effect of Concentration on a Chemical System
Table 3.3 (data)

Test tube Conditions Observations

1 Control

2 Addition of FeCl3 (aq)

3 Addition of KSCN (aq)

4 Addition of KCl (s)

Department of Chemistry 2
 CENTRE FOR FOUNDATION STUDIES DEPARTMENT OF CHEMISTRY
INTERNATIONAL ISLAMIC UNIVERSITY MALAYSIA CHL0325

___________________________________ _______________ _________ ________

name matric no. section experiment date

EXPERIMENT 4 ACID-BASE TITRATION CURVE 4

OBJECTIVE

RESULTS
Table 4.1 (data): Before and at End-Point

Volume of NaOH(aq) added

0.00 2.00 4.00 6.00 8.00 10.00 12.00
(mL)

pH of solution

2 drops 2 drops 2 drops 2 drops

14.00 16.00 18.00 20.00 22.00 23.00
( ) ( ) ( ) ( )

2 drops 2 drops 2 drops Solution turns permanent pale pink

( ) ( ) ( ) (end-point) = …… mL

Department of Chemistry 1
Table 4.2 (data): After end-point

Volume of NaOH(aq) added 2.00 4.00 6.00 8.00 10.00 12.00 14.00
(mL)

pH of solution

16.00 18.00 20.00

Table 4.3 (data)

Molarity of NaOH (aq) used (mol/L)

Volume of NaOH (aq) used at end-point

(mL)

Volume of CH3COOH (aq) used (mL)

Department of Chemistry 2
CALCULATIONS
1. From your graph, determine the pH of the solution at equivalence point. Label it on your graph.

2. Calculate the number of moles of NaOH (aq) used to completely react with CH3COOH (aq).

3. Calculate the molarity of CH3COOH (aq) used in this experiment.

4. Determine whether the pH of the salt solution is acidic, basic, or neutral. Explain your answer
briefly.

Department of Chemistry 3
Department of Chemistry 3