Labwork Manual Fundamental Chemistry MKK 1113

LABORATORY WORK MANUAL
FUNDAMENTAL
CHEMISTRY
Odd Semester 2022/2023
FUNDAMENTAL CHEMISTRY
LABORATORY
Department of Chemistry, Faculty of Mathematics
and Natural Sciences, Universitas Gadjah Mada
2022
GENERAL CHEMISTRY I /INORGANIC CHEMISTRY
Authors
Nuryono
Iqmal Tahir
Deni Pranowo
Winarto Haryadi
Indriana Kartini
Sri Sudiono
Laboratory of General Chemistry

Faculty of Mathematics and Natural Sciences UGM
Sekip Utara Yogyakarta 55281, telp 0274-545188; 6492370, Fax. 0274-545188
email: chemistry-kd@ugm.ac.id
PREFACE
Thank God we pray to the presence of Allah SWT, Who has

bestowed His Mercy and Grace, so that the preparation of this General
Chemistry I Laboratory Work Manual Book can be completed in due
time. Do not forget to thank to all those who have helped the preparation
of this book. This Laboratory Manual Book provides guidance for
undergraduate students to work at General Chemistry Laboratory of
Faculty of Mathematics and Natural Sciences of UGM at the odd
semester.
Improvement and refinement to the previous Laboratory Manual
of General Chemistry Lab Work that has long been used by General
Chemistry Laboratory for adapting the needs and the development of
sciences have also been included in this edition. General Chemistry
Laboratory of Faculty of Mathematics and Natural Sciences UGM is one
of service laboratories, which is not only serving Lab Work for Chemistry
Department Students, but also serving for other students from other
departments who require basic knowledge and skill of chemistry. This
book is completed with warnings about occupational safety and health of
works at the laboratory, so it is expected that workplace accident in the
laboratory can be avoided.
Hopefully all users of this book can use this book and can get the
benefits from it. Finally, supported critics and suggestions are our hope to
improve this book.
Yogyakarta, July 2021
Authors
General Chemistry I Lab. Work 2

LABORATORY WORK RULES
AT GENERAL CHEMISTRY LABORATORY
1. All participants must be on site at the appointed time (according to the

respective schedule). If the participant is late of more than 5 (five)
minutes from the appointed time, the participant is not allowed to join
the Lab Work on schedule and is required to follow the Lab Work on
another schedule.
2. During the lab work, participant must wear clean white long-sleeved
laboratory coat, Striped neatly and wearing shoes (Forbidden to use
sandals)
3. Every participant should write lab work report in the specified format
and signed by the assistant after the Lab Work. The reports are
collected before the next lab work. Lab work report is a requirement to
follow the next lab work.
4. Participant is not allowed to carry their stuffs except ones needed for
Lab Work. Stuffs that are not allowed to carry must be put into the
available locker. 1 locker is for 1 group.
5. Every participant must check all the equipment before Lab Work and
return the equipment after being used in dry and clean condition.
Before leaving the laboratory, participant must return all chemical
bottle that have been closed tightly to the original place, and return the
desk and locker keys. Losing keys is the responsibility of the
participants.
6. Every participant must keep the laboratory clean, work with calm,
and organized. During the lab work, participant must be polite, both in
speaking and behaving.
7. Assessment of the Lab Work is formative, carried out continuously
during the process of Lab Work. Assessment includes the
understanding of laboratory techniques and occupational health and
safety culture, material understanding (pre-test, laboratory skills, report
writing and final test).
8. Participant, who has not joined the Lab Work on schedule, is allowed to
join the following Lab Work (inhal) if the requirements are fulfilled, by
filling in an inquiry letter to the Head of General Chemistry Laboratory.
3 General Chemistry I Lab. Work

9. Taking the Lab Work not in the scheduled time cannot be more than
twice. Absence twice without replacement, results in failing to do the
Lab Work (E score).
10. Point number 9 does not apply to those who are sick and hospitalized at
the hospital.
11. If the participant violates the things set out above then participants may
be excluded from the laboratory and unable to attend the Lab Work that
day. The lab work is then declared to be failed and not allowed to join
the following Lab Work.
12. Things that have not been mentioned above and required for successful
implementation of the Lab Work will be arranged accordingly.

Head
of General Chemistry Laboratory
Dr. Deni Pranowo, M.Si.

CONTENTS
PAGES
Cover Page 1
Preface 3
Laboratory Work Rules at General Chemistry Laboratory 5
Contents 5
Schedule of General Chemistry I Laboratory Work 9
Experiment : Laboratory Techniques and Work Safety on 11
Laboratory
Experiment P : Introduction of Lab Equipment and Basic 23
Techniques at Laboratory
Experiment A-1 : Kinetics reaction of Permanganate Ion with 25
Oxalic Acid
Experiment A-2 : The Decrease in Freezing Point of Solution 29
Experiment B-1 : Determination of Commercial Vinegar 36
Content
Experiment B-2 : Analysis of Water Hardness 41
Experiment C-1 : Analysis of Electrical Conductivity 47
Experiment C-2 : Acidity Control of Buffer Solution 51

SCHEDULE OF
BASIC CHEMISTRY I LABORATORY WORK
Laboratory Test and Work in week(s)

Group
Number
1 2 3 4 5 6 7 8 9
I Assistance I A-1 A-2 B-1 B-2 C-1 C-2 Final Test
II Assistance I A-2 A-1 B-2 B-1 C-2 C-1 Final Test
III Assistance I B-1 B-2 C-1 C-2 A-1 A-2 Final Test
IV Assistance I B-2 B-1 C-2 C-1 A-2 A-1 Final Test
V Assistance I C-1 C-2 A-1 A-2 B-1 B-2 Final Test
VI Assistance I C-2 C-1 A-2 A-1 B-2 B-1 Final Test

EXPERIMENT
LABORATORY TECHNIQUES AND SAFETY CULTURE
Experimental Objectives : 1. To recognize some simple laboratory

glassware
2. To recognize some variant preparation
techniques and material treatments.
These following will be discussed about simple equipment that used

in the lab work at Basic Chemistry Laboratory. Some equipment is shown in
Figure P.1.
Figure P.1 Simple glassware for chemistry laboratory work
Here are the description of equipment and function of each

glassware on Figure P.1.

1. Volumetric Flask
Volumetric flask (measuring flask or graduated flask) is a piece of
laboratory glassware, a type of laboratory flask, calibrated to contain a
precise volume at a particular temperature. Volumetric flasks are used
for precise dilutions and preparation of standard solutions. They are
available in several size of volume.
2. Graduated Cylinder
Used for measuring the volume of chemical substance in liquid phase.
This equipment has scale, available in several size of volume. It is not
allowed to be used for measuring solution/solvent in hot condition.
Give attention to the meniscus at the time of scale reading.
3. Beaker
Beakers are generally cylindrical in shape, with a flat bottom. Most
also have a small spout (or "beak") to aid pouring the contained
solution. Beakers are available in a wide range of sizes, from one
millilitre up to several litres. This glassware is not for measuring even
there is a scale. The error is quite large. It is used for a place of solution.
It can also be used for heating chemical substance and evaporating
solvent or concentrating the solution.
4. Glass rod/ Stirring rod

Used for stirring a mixture or chemical solution at the time of chemical
reaction. It is also used for helping to pour/decant the solution on the
filtering process.
5. Bottle Washer
This bottle is made of plastic. This bottle filled with distilled water that
is used for washing or helping in dilution.
6. Funnel
A 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, spillage may occur. Funnels are
usually made of stainless steel, aluminium, glass, or plastic.
7. Erlenmeyer
The Erlenmeyer flask was created by EmilErlenmeyer, a German
chemist, in the 1860s. He developed a flask that has a flat bottom with a
tapered neck. The mouth, or opening, is used for pouring solutions and
may be closed with a stopper in order to store samples. Although there
is a scale, this glassware is not for measuring. Erlenmeyer is also
commonly used as a container for solution to be titrated.
8. Test Tube
Test tubes are made of glass and widely used by chemists to handle
chemicals, especially for qualitative experiments and assays. It can be
heated. It is used for reacting chemical substance in small portion. Their
spherical bottom and vertical sides reduce mass loss when pouring,
make them easier to wash out, and allow convenient monitoring of the
contents.
9. Cuvette
A cuvette (French: cuvette = "little vessel") is a small, straight-sided
tube-shaped container with a circular or square cross section. It is sealed
at one end, and made of an optically-clear material such as plastic of
polystyrene or polymetacrillate, glass, or fused quartz (for UV light).
The shape is similar to the test tube, but the size is smaller. It is used as
the sample place for analysing using spectrophotometer. Cuvette is not
allowed to be heated.
10. Test Tube Rack

It is made from wood or metal. It is used as a container to place the
glass equipment with heater/electrical stove.

11. Preparate glass
A microscope slide or preparate glass is a thin flat piece of glass,
typically 75 by 26 mm (3 by 1 inches) and about 1 mm thick, used to
hold objects for examination under a microscope.
12. Wire Netting

It is made of metal and it is used as a pad when heating the glass
equipment with heater/electrical stove.
13. Clamp
It is made of metal and it is used for clamping the test tube at the time
of heating or helping to take the filter paper or other things in hot
condition.
14. Spatula
It is made of metal and it is used as helping tool to take solid material or
crystal.
15. Litmus Paper

This is a red and blue paper-shaped indicator. Other indicators are
liquids such as Phenolphthalein (PP), methyl orange (MO) and so on. It
is the material to measure or show acidity of the solution (pH).
16. Watch Glass

It is made of glass and is used to place the substance to be weighed
17. Porcelain Cup

This equipment is used to place substances to be evaporated by heating.
18. Dropping Pipettes/ Pasteur Pipettes

It is used to take liquid substance in small portion.
19. Brush
Brush is used to clean the tubes.

20. Graduated Pipettes
It is made of glass and has a scale. The shape of the pipette is shown in
the figure below. This is used to take solution for a given volume. Use a
pro pipette or pipette pump to take the solution, do not take it by mouth.
21. Volumetric Pipette

The volumetric pipette allows very accurate measurements (up to four
significant numbers) of a number of solutions. The pipette as shown in
the figure below has a large bulb with a long narrow section above with
a mark for one volume (such as a volumetric flask). Use a pro pipette or
pipette pump to take the solution, do not take it by mouth.
22. Burette
Burette is made of glass and has a scale. This is used for titration. The
substance used for titration (titrant) is placed inside the burette and is
dropwise released through the tap. The volume of the substances used
can be seen on a scale.
Several Basic Techniques at Chemistry Laboratory
Having understood the use of the equipment introduced above, here are
some experiments to use the equipment. Things to note here is how to use
the equipment properly and correctly.
I. Production of Gas and Introduction of Litmus Paper

Ammonia (NH3) gas is a gas with a very bad smell. This gas can be
produced by reacting ammonium chloride with NaOH solution while
heating the solution in the test tube. The presence of this gas can be
identified from its smell. Avoid to directly smell harmful or toxic gases. A

relatively safe way to smell the gas is to fan our hands over the tube and
nose at a relatively long distance. This is shown in Figure P.2.
Figure P.2 Technique of gas smelling and pH measurement
Litmus paper (there are two colours, blue and red) is used as
indicator to confirm whether the compound is acidic or alkaline by looking
at the colour change. If the solution tested with blue litmus paper is still
blue, and with the red litmus paper is still red so that the solution is neutral.
If the blue litmus paper changes into red, and the red litmus paper will
remain red colour, so that the solution is acidic. The solution is said to be
alkaline when the solution tested with blue litmus paper remains blue while
the red litmus paper changes into blue. The way to use the litmus paper is
shown in Figure P.2.
Experimental Method
Take some NH4Cl solution and insert the solution into the test tube
and add some NaOH solution. Hold the test tube with a clamp, then heated
while wagging. The mouth of the tube should be slightly leaned but should
not be directed to yourself or others. Find an empty place to perform this
experiment. The heated way is shown in Figure P.3.
When boiling, keep the substance inside the tube, lest the substance
out of the mouth of the tube (particularly for flammable substances). The
way we can do is lifting the tube away from the fire when the substance has
started to out of the tube. Try to practice how to smell like as explained
above. Note how the smell of gas and observe the substance before and after
reaction. Hold the red litmus paper close to the mouth of the tube. Observe
the colour change from litmus paper and give conclusions. What is the
benefit of wagging during the heating time?
Figure P.3 Technique of heating material properly
Information of material properties, Health and Safety

Works/Environments (HSWE)
- Keep away the flammable substance out of the fire.
- Work quietly and attentively to avoid accidents.
II. Dilution using Volumetric Flask

Preparation of standard solution is sometime carried out by diluting
solution that already prepared (stock solution). For example to prepare
standard solution of HCl 0.1 M from HCl 0.2 M. First, determine the desired
volume of the standard solution to make and calculate the volume of the
stock solution required with the following equation:
V2 M2
V1 M1 = V2 M2 or V1 =
M1
where
V1 = Initial volume of solution required
M1 = Initial molarity
V2 = volume of standard solution to make
M2 = molarity of standard solution to make

Experimental Method
Take several amount of HCl solution 0.1 N with volumetric pipette.
Put attention to the meniscus, concave surface of liquid must be precisely
reached with the boundary line on the volumetric pipette. Insert the HCl
solution into the volumetric flask and dilute to the limit of the flask. Do not
add water more than necessary then throw the excess amount to the limit,
since it will cause a big mistake.
Therefore, dilution must be carefully done. As the solution is closely
to the limit of the volumetric flask, use Pasteur pipette/volumetric pipette to
add dropwise the solvent. How to use volumetric pipette for these drops by
drops is to cover the top of the pipette with index finger while the thumb
and middle finger are used for holding the pipette with a slowly spin.
III. Titration
Titration is one of the most commonly used analytical techniques in
quantitative analysis. Solutions with known concentrations are referred to as
standard solutions, usually placed into burets as titrant. The solution to be
determined concentration is introduced into Erlenmeyer and it is referred to
as a titrated substance. Titration is done by opening the buret tap gradually.
Titrant will be gently added into Erlenmeyer with slowly shaking. How to
hold and wiggle Erlenmeyer is shown in Figure P.4. The end point of the
titration occurs at the color change, which can be observed using indicators.
At that time, the number of moles of titrant is equal to the number of moles
of the titrated substance. In the monobasic acid base tritration such as
titration of HCl with NaOH, the previously written equation can be used for
calculating the molarity of the substance to be titrated.

Figure P.4 Titration equipment and technique of titration
Experimental Method
Wash the burette with washing solution. Rinse with the standard
solution that will be used, eg. NaOH 0.1 M. Fill the burette with standard
solution until 0 scale. Use the volumetric pipette to take 20 mL of HCl 0.1
M from the previous dilution product. Pour the HCl into the Erlenmeyer
then add 3-4 drops of phenolphthalein (PP) indicator. Open the burette, add
the titrant gradually to the Erlenmeyer. The Erlenmeyer should be gently
wiggling. Titration is stopped when the addition of a drop of NaOH gives
very light red colour that will not disappear in wiggling. Repeat the titration
for three times (3x). Note how many mL of standard solution that is used by
looking at the scale shown by the solution in the burette. Calculate the
molarity of titrated solution.
IV. Dilution of Solution

Dilution is done by adding solvent to the substance that will be
diluted. This is a usual way of dilution. For substances exhibiting
exothermic reaction in the dilution process, such as concentred H2SO4, the
dilution is carried out slightly differently, i.e. by gradually pouring the
concentrateded solution of H2SO4into the solvent (water).

Works/Environments (HSWE)

Reversed process that is adding water to the concentred H2SO4 will cause
an explosion and hot sparks and it is dangerous if contacting with skin.
Experimental Method
Take 10 mL of distilled water with graduated cylinder. Put attention to
the bottom of the water meniscus that must be precisely reached 10 mL of
scale. The eye vision must be precisely aligned with the high of meniscus of
water. Pour the solution into the test tube. Take 3 mL of concentrated H2SO4
with graduated cylinder. Use the same way of measurement from the
previous step. Pour the concentrated solution of H2SO4 into the test tube that
is already filled with distilled water. Remember, the pouring must be done
gradually and carefully. Notice the heat change before and after concentred
H2SO4 poured into the test tube.
V. Filtering
Filtering is a way to separate a precipitate/sediment from a solution.
The basic principle of filtering is material separation technique based on
particle size through the filter. In this following step, we will filter the
PbSO4 that is produced by reacting H2SO4 with Pb-acetate.
Experimental Method
Take 5 mL of Pb-acetate solution into the test tube then add H2SO4
from previous dilution product. Observe the precipitated occurred. Note the
colour of precipitate. Take the filter paper in round shape and fold into ¼
round shape, then fold again into 2-3 folded. Put the folded filter paper in
the funnel and wet with distilled water until stick to its glass. Set the funnel
with filter paper at the mouth of Erlenmeyer to accommodate filtrate/
washing solution. Pour the solution that will be filtered into the funnel. The
pouring is done by using stir rod that hold exact at the mouth of used
beaker. This must be done carefully and gently. Etiquette bottle must be
hold with the etiquette is facing the palm of hand. If pouring the solution do
not touch the etiquette/label. Bottle cap must be placed in reversed state on
the table and put back in the similar bottle.

How to fold the filter paper and how to pour the solution will be
filtered are clearly shown in Figure P.5
Fold filter paper in half fold into quarters with top open cone
smaller than button like this
Figure P.5 Technique of folding filter paper and filtering solid
compound from a solution
VI. How to read meniscus

Volume measurement of a solution other than using graduated or
volumetric pipette, often used with graduated cylinder and burette. The
transparent solution or liquid is more appropriate when looking at scale of
measurement equipment on precisely horizontal with the meniscus point, as
shown in this Figure P.6 below. If the solution is too clear and the scale of
the measurement cannot be seen, then it can be helped with dark coloured
paper.
Figure P.6 How to read meniscus

EXPERIMENT P
INTRODUCTION OF LABORATORY EQUIPMENT
AND BASIC WORK TECHNIQUES AT LABORATORY
Experimental Objectives: To understand the use of some equipments at

laboratory and some of basic work techniques at
laboratory
Experimental Method:
I. Introduction of Laboratory Equipments
1. Draw all available laboratory equipments in the basket on your
desk!
2. Write down the name and function of each equipment you draw!
II. Introduction of Basic Work Techniques at Laboratory

1. Make 100 mL of NaCl 0.1 M solution by using available material
and equipment!
2. Dilution of NaCl solution.
Make 100 mL of NaCl 0.01 solution from 0.1 M of NaCl solution
by using available material and equipment!
III. Introduction of Titration Technique

Conduct the titration of 10 mL HCl solution with standard solution of
NaOH 0.1 M using phenolphthalein (PP) as indicator. Record how
many volume of NaOH and calculate the concentration of HCl solution.

EXPERIMENTAL A-1:
KINETICS OF REACTION OF PERMANGANATE ION
AND OXALIC ACID
Experimental Objectives : To determine reaction order of MnO4 with

H2C2O4.
Basic Theory:
The reaction rate of chemical reaction is expressed as a
concentration function of the reactants that play roles on its reaction. For
bimolecular reaction, the reaction rate r is proportional to the product
concentration of H2 and I2, and can be written in equation as follow:
H2(g) + I2(g) → 2HI(g)
r=k [H2 ]1 [I2 ]1
This equation shows that the reaction above is second order reaction
or can be expressed that the reaction is first order to the H2 and first order to
the I2. It should be emphasized that there is no direct relation between
reaction orders with stoichiometry coefficient reaction as above. The
similarity between reaction order and stoichiometry of reaction, is just only
a coincidence. Reaction order is related to the reaction mechanism that
occurred.
The mechanism of reaction cannot be determined simply by
reviewing the reaction, but must be determined experimentally, as well as
reaction order that should be determined by experiment. In this experiment,
reaction order of MnO4 with H2C2O4 will be determined. Reaction rate of
MnO4 with H2C2O4 is expressed in equation as follows:
r=k [H2 C2 O4 ]x [MnO4 - ]y

If a reaction has n reaction order to the reactant, so that the reaction
rate will be proportional to the concentration to the power of n and inversely
proportional to the time, t.
r=kCn r = Cn
where
C = concentration
n = reaction order
t = time
dC 1
r=k r=
dt t
1
Therefore, 𝐶 𝑛 ≈ 𝑡 . Therefore, graph of Cn versus 1/t will always form
straight line and reaction order of chemical reaction can be determined by
making a graph as shown on the following table:
Reaction order Linear graph

1 C versus 1/t
2 C2 versus 1/t
3 C3 versus 1/t
1. Prepare 4 Erlenmeyer flasks (50 mL) and 3 burettes (50 mL) in clean
condition.
2. Fill the 1st burette with solution of KMnO4 0.1 M, fill the 2nd burette
with distilled water, and fill the 3rd burette with solution of H2C2O4 0.7
M.
3. In the available Erlenmeyer, mix and react H2C2O4 and KMnO4
according to the following table.

Group 1 Group 2
H2C2O4 Distilled KMnO4 H2C2O4 Distilled KMnO

4
(mL) water (mL) (mL) water (mL)
(mL) (mL)
Erlenmeyer 1 8.0 11.0 1 6.0 11.0 3.0
Erlenmeyer 2 8.0 10.0 2 8.0 9.0 3.0
Erlenmeyer 3 8.0 9.0 3 10.0 7.0 3.0
Erlenmeyer 4 8.0 8.0 4 12.0 5.0 3.0
Note:
a. Firstly mix H2C2O4 and distilled water and shake the Erlenmeyer
until homogeneous.
b. Then add KMnO4 by gradually opening the burette tap.
4. Repeat the procedure of 1 to 3 for three times (3x) and note the time
required from the addition of KMnO4 until the purple colour is
disappeared within the Erlenmeyer.
5. Reaction order is determined by making the graph Cn versus 1/t for each
reactants, (with n = 1, 2 and 3)
Observation Data
Group 1
Time
H2C2O4 KMnO4
Exp (seconds)
mL M mL M
1.
2.
3.
4.

Group 2
Time
H2C2O4 KMnO4
Exp (seconds)
mL M mL M
1.
2.
3.
4.

Works/Environments (HSE)
KMnO4 solution is a thick purple solution. It will give brown color if
exposed to the skin. Oxalic acid will cause itching on the skin

EXPERIMENT A-2:
THE DECREASE IN FREEZING POINT OF SOLUTION
Experimental Objectives: A. To determine the constant of molality

decreasing freezing point of solvent.
B. To determine molecular mass (Mr) of non-
volatile substance.
Basic Theory
If the substance that is not volatile (non-volatile) is inserted to the
solvent, the free solvent energy will be then decreased. This decreasing in
free energy follows the Nernst equation.
G1° − Gx° = RT ln X (1)
where
G1° − Gx° = decreasing free energy of solvent
R = common gas constant (R= 1.987 cal K-1 mol-1)
T = absolute temperature (K)
X = mole fraction of solvent in solution
The decrease in free energy will decrease the tendency of the solvent
to turn into its vapour phase. Therefore, the vapour pressure of solvent in the
solution will be lower than that of the same solvent vapour pressure at the
pure state. The effect of decreasing vapour pressure to the freezing point in a
solution will be easier to learn with phase diagram at the following figure.

Figure of phase diagram of a solution and pure solvent
The figure shows that the freezing point of a solution Tf, is lower
than the freezing point of pure solvent 𝑇𝑓𝑜 . From the explanation above, it is
clear that the decreasing of freezing point in a solution depends on mole
fraction of its solute substance.
∆Tf (Tfo − Tf ) ≈ X
Since the mole fraction of x solvent is a linear function to the mole
fraction of solute X1; according to the equation of 𝑥 = 1 − 𝑋1, then the Tf
can be expressed as a function of X1 as follows:
R (Tfo )2 X1
∆Tf = (2)
∆Hf
Where ∆𝐻𝑓 heat dissolving solvent.
If m amount of solute substance is added into 1000g of solvent, then

the solution with m molality is obtained. This solution has mole fraction of
solute substance equal to:
m
X1 = (3)
1000⁄Mr1 + m

Where Mr1 = molecular mass of solute substance.
For diluted solution (m=0), the X1 = m Mr1 ⁄1000, hence the
decreasing of freezing point in a solution can be written as:
R (Tfo )2 Mr1
∆Tf = m (4)
1000 ∆Hf
R (To )2 Mr1
f
If K f = is substituted to the equation (4), so that the simple
1000 ∆Hf
equation is obtained:
∆Tf = K f m (5)
Considering that X1 = m Mr1 ⁄1000, so:
1000 X1
m= (6)
Mr1
While:
W1
n1 Mr1
X1 = = (7)
n1 + n W1 W
Mr1 + Mr
Where:
W1 = mass of solute substance

Mr1 = molecular mass of solute substance
W = mass ofsolvent
Mr = molecular mass of solvent
W1 W
For very dilute solution, therefore = so that:
Mr1 M1

W1
Mr1
X1 = (8)
W
Mr
If the equation (5), (6), (8) are combined, it will give the equation:
1000 K f W1
Mr1 = x (9)
∆Tf W
From the equation (9), molecular mass of solute substance Mr1, can be
calculated. The value of K can be also calculated with the following
equation:
∆Tf W Mr1
Kf = (10)
1000 W1
Experimental Method
Tool can be constructed like the following figure:
Caption: Other tools:

A. Thermometer 1. Beaker glass of 100 mL
B. Glass tube 2. Erlenmeyer
C. Metal stirrer 3. Graduated cylinder of 100 mL
D. Glass tube II 4. Stopwatch
E. Glass tube III

I. Preparation
1. Fill the glass tube E with the mixture of water, ice and enough salt.
2. Glass tube D is filled with sufficient amount of water.
3. Take 20 mL of solvent and insert it to the glass tube B (solvent
used is glacial acetic acid).
II. Determination of constant of decreasing molal freezing point

1. After 20 mL of glacial acetic acid is inserted to the glass tube B
while cooling down, note the temperature every minute.
2. If the temperature appears to remain constant, then observe
whether the solvent has been frozen or not.
3. Repeat the steps 1 and 2 for once, then determine the freezing
point of pure solvent, Tfo .
4. Let the solvent thaw back, then insert the naphthalene (Mr = 128)
as helper solvent. Conduct the same step 1,2, and 3 and note the Tf
(freezing point)
So that ∆Tfo − Tf = ∆Tf

∆Tf = decreasing freezing point of solution.
From the ∆Tf , calculate Kf of glacial acetic acid by using formula
(11).
ATTENTION: The solution should not be disposed!
III. Determination of Mr of X substance

1. Let the solution from previous experiment thaw back, then add 2 g
of X substance.
2. Do the same way as part II, observe its 𝑇𝑓 then calculate Mr of X
substance by using modified equation as follows:
1000 K f Wx W1
∆Tf = ( + ) (12)
W Mrx Mr1

where
∆Tf = decreasing of freezing point of final solution
Kf = decreasing of solvent molality
W = mass of solvent in grams
𝑊𝑥 = mass of X substance
W1 = mass of naphthalene in grams
Mrx = molecular mass of X substance
Mr1 = molecular mass of naphthalene
Observation
A. Determination of Molality Freezing Point Constant of Glacial
Acetic Acid
1. Determination of acetic acid freezing point (𝑇𝑓𝑜 )

Volume of acetic acid =……………………… mL
Density of acetic acid =……………………… g/mL
Mass of acetic acid (W) =……………………… g
Time (minutes) 2.5 5.0 7.5 10.0 15.0 20.0 25.0

Temperature (C) ….. ….. ….. ….. ….. ….. …..
Glacial acetic acid freezing point Tf = ……………………………

2. Determination of naphthalene freezing point (Mr = 128)
Mass of naphthalene = ………………. G
Time (minutes) 2.5 5.0 7.5 10.0 15.0 20.0 25.0
Temperature (C) ….. ….. ….. ….. ….. ….. …..
Naphthalene freezing point (W1) = …………………………….

Decreasing of freezing point in naphthalene solution:
∆Tf = …………………… C -…………….. C = ……………. C
B. Determination of molecular mass (Mr) X substance
Volume of acetic acid =……………………… mL
Mass of acetic acid =……………………… g
Mass of X substance (Wx) =……………………… g
Time (minutes) 2.5 5.0 7.5 10.0 15.0 20.0 25.0

Temperature (C) ….. ….. ….. ….. ….. ….. …..
Freezing point of X solution = ……………C

Decreasing of freezing point of X solution = ……………C
Molecular mass (Mr) of X substance = ……………
Based on the value of Mr and physical properties of X substance that
visually observed, estimate what is the X substance?

Glacial acetic acid (CH3COOH) is corrosive acid solution and very
strong smelling substance can cause headache. Close the bottle container
of glacial acetic acid after being used.

EXPERIMENT B-1:
DETERMINATION OF COMMERCIAL VINEGAR CONTENT
Experimental Objectives : 1. To determine the molarity of NaOH solution

with oxalic acid standard solution.
2. To determine the commercial acetic acid
content.
Basic Theory
Acidimetry and alkalimetry are volumetric quantitative analysis
based on neutralization reaction. Both are distinguished by their standard
solution. While acid is used as standard solution in acidimetry, alkaline
solution is used for standard solution in alkalimetry. These analyses are
done by titration.
In alkaline titration of the acetic acid, the following reaction occurs:
In titration of acetic acid with NaOH (as standard solution) will

produce salts that derived from weak acid and strong base. This sodium
acetate salt will perfectly dissociated since it is salt, while acetic acid ions
will be hydrolyzed by water, the following reaction occurred:
Acetate ion will be hydrolized by the water molecule and produce

acetic acid molecule and hydroxide ion. Therefore, a salt solution of strong
base and weak acid such as sodium acetate will be alkaline in water (pH>7).
If the salt is composed by weak base and strong acid, the salt
solution will be acidic (pH<7). For a salt that composed by both strong base
and acid, the solution will be neutral (pH=7). Hydrolysis occurs only to
weak acid, weak bases, and weak base and acidic ions. Equivalent point in
the titration process of acetic acid with sodium hydroxide will be reached at
the pH>7. Knowing the equivalent point is used by certain indicator as a

guide for completion of the process. The indicator colour change at low pH
is not the same as the colour change at high pH.
Titration of acetic acid with NaOH uses those kinds of indicators. In
the analysis of acetic acid on the commercial vinegar, we will get the
information whether the content written on label is correct or not. Analysis
is conducted by titrating commercial acetic acid with NaOH standard.
Molarity of acetic acid can be calculated as:

Macetic acid = (VNaOH x MNaOH )/Vacetic acid
QUESTIONS:
1. What is the meaning of standard solution?
2. What is the meaning of primary and secondary standard solutions?
3. If strong acid solution is titrated with strong base by using PP indicator,
is it appropriate if the inverse titration is used PP indicator? Explain!
Experimental Method
I. Standardization of NaOH solution with oxalic acid solution
1. Weigh 0.63 g of oxalic acid, dissolve it in the volumetric flask of 100
mL by using distilled water up to the mark limit of the flask.
2. Insert the solution to the 50 mL of burette.
3. Pour 10 mL of NaOH solution into the Erlenmeyer, and add 10 mL of
distilled water and 1-2 drops of phenolphtalein indicator, then titrate
with the oxalic acid solution until the pink colour disappeared into
colourless solution.
4. Repeat the procedure for 3 times.
Observation and Calculation

Mass of cup + (C2H2O4.2H2O) crystal ………………………… g
Mass of empty cup ………………………… g
Mass of (C2H2O4.2H2O) ………………………… g
Molarity of oxalic acid ………………………… M

Volume of NaOH solution used: (C2H2O4.2H2O) solution used:
1. ……………………….mL …………………………….mL
2. ……………………….mL …………………………….mL
3. ……………………….mL …………………………….mL
Molarity of NaOH:
M1 =………………… molar
M2 =………………… molar
M3 =………………… molar
Results of Analysis
M1 + M2 + M3
Molarity of NaOH = = ………………………… M
3
Maverage
Factor of NaOH = = …………………………
0.1
II. Determination of Commercial Vinegar Concentration

1. Take 5 mL of commercial vinegar with volumetric pipette or
graduated pipette then insert the solution to the 100 mL
volumetric flask and dilute it until its volume becomes 100 mL
(until mark).
2. Take 10 mL of diluted vinegar and insert to the Erlenmeyer then
add 2 drops of phenolphtalein indicator.
3. Conduct the titration using NaOH standard solution until the
colour change occurred.
4. Repeat the titration for 3 times.

5.Having finished, wash the burette with washing acid (rest of
diluted commercial acetic acid)
6. Then wash the burette with tap water until clean and put in the
stative in upside down position.
Observation
Brand of the used vinegar …………………………………………….
Burette scale
I II III
reading
Final titration
Initial titration
Vol. of solution
Average volume of the used NaOH ……………………………….. mL
Calculation:
Molarity of the used NaOH is 0.1 M
Volume of the used NaOH = a mL for 10 mL of diluted acetic acid
The content of acetic acid in commercial vinegar (in g/100 mL) =
100/5 x 100/10x 0.1 x a x 60 mg.

Oxalic acid crystal (C2H2O4.2H2O) is white crystal and can cause
itching on the skin. Commercial vinegar contains around 5% of acetic acid
that has strong enough smell and can cause headache. Close the bottle
container of the vinegar after being used. NaOH solution is an alkaline,
feels slimy like a soap when in the skin.

EXPERIMENT B-2
ANALYSIS OF WATER HARDNESS
Experimental Objectives : A. To study the cause and the effect of hard

water
B. To determine the hardness in water sample.
Basic Theory
Hard water is water that contains soluble salt from calsium,
magnesium or iron ions. At low concentration, these ions are not harmful
for household needed, but at high concentration, the ions will interfere to the
washing process with soap and accelerate the corrosion of steel pipes,
especially those that carry hot water. The source of hard ion within the
natural water is produced from slightly acidic rainwater that flows through
mineral deposits with varying compositions. Acidic rainwater is reacted
with calcium salt and magnesium carbonate that slightly soluble and with
various rocks that contain iron. Partial dissolution of salt releases ion into
the water surface or groundwater.
Hard ions such as Ca2+, Mg2+, and Fe3+ may form compound that is
insoluble with soap. Soap, which is sodium salt from fatty acid like sodium
stearate, C17H35CO2-Na+, is very effective as cleaning agent as long as it
remains in the solution. However, the existence of hard ion causes the
formation of grey scum in the form of insoluble salt such as
(C17H35CO2)2Ca.
This grey precipitate appeared as a ring on the bath/washer and the

impurities also stick to the cloth that cause white cloth look dull. Hard water
is also responsible to the formation of unwanted crust in the container to
boil/heat water. The crust has poor heat conductivity, which can reduce heat
transfer efficiency. The crust is also found on the hot water pipe and
decrease the water flow; in an extreme condition, crust can cause clogged
pipe. The crust is primarily made up of carbonate salt from hard ion and
formed a reaction.

Groundwater becomes hardness since it flows through the
underground limestone deposits; generally, water from deep wells has
higher water hardness than shallow well water due to the longer contact to
the rock. It also happens on surface water (river, lake, and others). This
water collects the hard ion while flowing through the limestone, the
dissolved carbon dioxide in rain water dissolves deposit of limestones.
The reaction is a reversed reaction from the formation of crust. Two

similar reactions are the key in the formation of stalactites and stalagmites in
cave that located at the limestone area.
Considering the abundance of limestone and calcium minerals, such
as gypsum, CaSO4.2H2O, is relatively large in nature, so it is not surprising
that Ca2+ ions are the major component of hardness rather than Mg2+. The
concentration of hardness ion in a sample usually expressed as the hardness
due to Ca2+. The unit for hardness is mg CaCO3/L, which is equivalent with
ppm CaCO3. General classification for water hardness is shown in the
following table.
The Hardness (ppm CaCO3) Hardness classification

< 15 Very low
15-50 Low
100-200 High
>200 Very high
Theory of Analysis
In this experiment, titration technique is used to measure the
combined concentration of Ca2+ and Mg2+ ions in water sample. Titrant is
disodium salt solution from ethylendiaminetrtraacetic acid (abbreviated as
Na2H2Y or Na2EDTA). In a solution, Na2EDTA is dissociated to Na+ and

H2Y2- ion. The H2Y2- ion reacts with hardness ions, Ca2+ and Mg2+, to
generate a very stable complex ion, especially in buffer solution at pH of
about 10. Buffer ions of ammonium-ammonia are often used for pH control
in analysis.
Figure of Na2EDTA structure:
Na2H2Y (Na2EDTA) structure

If a titrant of H2Y2- is added to the analyte, then the reaction of
complex ion formation with Ca2+ and Mg2+ occurs as follows:
From the equilibrium reaction above, it is clear that if the molar

concentration of Na2H2Y is known, the moles of hardness ion in water
sample can be calculated according to 1:1 stoichiometric reaction.
Volume of H2Y2- x molar concentration of H2Y2- = H2Y2- mole = hardness
ion mole.
Hardness ion is assumed exclusively as Ca2+ from dissolving of
CaCO3. Since 1 mole of Ca2+ is formed from 1 mole of CaCO3 per litre
sample, so
Mole of hardness ion = mole of Ca2+ = mole of CaCO3
CaCO3 ppm (mg CaCO3/L sample) = mole of CaCO3/L sample x
100,1 g CaCO3/mole x mg/10-3 g
Indicator used for detecting equivalent point in titration is
Eriochrome Black T (EBT). This indicator also forms complex with both
Ca2+ and Mg2+ ions, but binds stronger to Mg2+ rather than Ca2+. Since only
a small amount of EBT is added then only a few Mg2+ are complexed and
there is no Ca2+ ion form complex with the EBT. Therefore, most of
hardness ion remains as free ions in solution. The EBT indicator is blue sky
colour in solution but then forms a wine red complex of [Mg-EBT]2+.

Before the H2Y2- titrant is added for analysis, the colour of analyte is
red wine due to the formation of [Mg-EBT]2+ complex ion. If H2Y2- is
complexing all the Ca2+ and Mg2+ is “free” from water sample, so the wine
red complex of [Mg-EBT]2+ is dissociated and the red wine colour changes
into blue sky colour from EBT indicator, and the end point is reached. all of
the hardness ion has already complexed with H2Y2-.
Therefore, Mg2+ must be present in the water sample for EBT

indicator to work. Often, only a few of Mg2+ as MgY2- is added to the
analyte in the beginning of analysis for making sure the formation colour of
red wine occurred.
Experimental Method
I. Standardization of 0.01 M of Disodium Ethylendiaminetetraacetate
solution, Na2H2Y (Na2EDTA)
1. Fill the burette with 0.005 M of Disodium
Ethylendiaminetetraacetate solution (Na2EDTA).
2. Take 25 mL of 0.0005 M Ca2+ standard solution by using
volumetric pipette, then add it to 125 mL Erlenmeyer. Add 1 mL of
buffer solution at pH 10 and 2 drops of EBT indicator to the
Erlenmeyer. Prepare three (3) Ca2+ standard solution.
3. Titrate the Ca2+ standard solution with Na2H2Y titrant gradually.
When approaching the end point, decrease the addition rate of
titrant. At the last drops of addition should be at 3-5 seconds
intervals. End point occurs when the addition of titrant changes the
colour to the blue sky permanently.
4. Repeat the titration for the second and third standard solution. Then
calculate the molar concentration of Na2H2Y solution.

II. Water Sample Analysis
1. Take 25 mL of water sample by using volumetric pipette, then insert
it to the 125 mL of Erlenmeyer.
2. Add 1 mL of buffer solution (pH 10) and 2 drops of EBT indicator
to the Erlenmeyer.
3. Conduct the titration with 0.0005 M Na2H2Y solution gradually.
When approaching the end point, decrease the addition rate of
titrant. At the last drops of addition should be at 3-5 seconds
intervals. End point occurs when the addition of titrant changes the
colour to the blue sky permanently.
4. Repeat the steps above for three (3) times.

EXPERIMENT C-1
ANALYSIS OF ELECTRICAL CONDUCTIVITY
Experimental Objectives: 1. To measure the electrical conductivity of

various types of compound and solution at
various concentrations.
2. To learn the effect of various types of
compound and the concentration of a
solution on electrical conductivity.
Basic Theory
Electrical current can be interpreted as an electron current that
carrying negative charge through the conductor. This charge transfer may
occur when there is a potential difference between one place with another
place and the current will flow from high potential to the lower potential.
At the figure below, the potential at A is higher than the potential at
B. When a conductor with resistance is installed, it will flow an electric
current of I. The same potential difference does not always produce the
same strong current but depends on the size of resistance used. The greater
R resistance, the less electrical charge is delivered.
Conductor
The ability of a conductor to move the electric charge is known as
electrical conductivity that inversely proportional to the resistance (R).
Formula of electrical conductivity:
1
L=
R
Where: L = conductivity (ohm-1)
R = resistance (ohm)
Experimental Method
I. Determination of electrical conductivity of various compound.
1. Prepare 5 beakers 100 mL.
2. Each of it fill with 25 mL of kerosene, H2O, NaCl solution and
NaCl crystal.
3. Measure the electrical conductivity of each solution using a
multimeter arranged as the following figure shown:
4. Determine the properties of substance against the electrical

conductivity (strong conductor, weak conductor and isolator).
II. The Effect of Concentration of electrolyte solution to The Electrical

Conductivity
1. Prepare 25 mL of each solution with the concentration of 0.05, 0.1,
0.5 and 1.0 M.
Group 1 Group 2
CH3COOH NaCl
NH4OH NaBr
HCl NaI
NaOH NH4Cl
2. For each solution, measure the electrical conductivity. Conduct the

measurements from the most diluted solution.
3. Draw the electrical conductivity graph of solution to the
concentration of Group 1. Determine which compounds are strong
electrolytes and which ones are weak. Explain the difference effect
of dilution on strong and weak electrolytes.

4. Draw the electrical conductivity graph of solution to the
concentration of Group 2. Compare the cation and anion electrical
conductivity in a group (between Cl-, Br-, I- and between Na+ and
NH4+)
Observation
I. Determination of The Electrical Conductivities of Various
Compound
Compound I, mA V, volt L = 1/R, ohm-
Kerosene
H2O
NaCl solution
NaCl crystal
II. The Effect of Concentration of Electrolyte solution to The

Electrical Conductivity
Group 1
Concentra CH3COOH NH4OH HCl NaOH
tion
I, mA V, volt L,ohm- I, mA V, volt L,ohm- I, mA V, volt L,ohm- I, mA V, volt L,ohm-
(M)
0.05
0.10
0.50
1.00
Group II
Concentr NaCl NaBr NaI NH4Cl
ation -
(M) I, mA V, volt L,ohm- I, mA V, volt L,ohm- I, mA V, volt L,ohm- I, mA V, volt L,ohm
0.05
0.10
0.50
1.00

Please return materials such as kerosene, H2O, NaCl solution and
NaCl crystal to container (DO NOT THROW TO THE SINK).
Please dispose other chemical material to the available waste bottle.
Although all the solution is in diluted condition, taking the solution must be
used pro pipette.

EXPERIMENT C-2
ACIDITY CONTROL OF BUFFER SOLUTION
Experimental Objectives: 1. To study the technique of pH controlling for

different application.
2. To understand buffer system and the function
of its system.
Basic Theory
Most of physiological processes are very sensitive to the change of
pH. For example: pH on human blood is constantly maintained at 7,2. Only
at that pH, the blood is able to carry oxygen and carbon dioxide well. If the
pH decreases below 7,2 (higher concentration of H+), the haemoglobin in
the blood will not react with oxygen, and if pH increases (higher
concentration of OH- ion), the bicarbonate will not be changed into carbon
dioxide in the lungs. Human body has a mechanism that control and
maintain the pH by using a certain mixture compound called as buffer. In
this experiment, a buffer solution will be made and we will observe how the
solution works to maintain the pH. If a few of acid or base is added to the
either buffer solution or non-buffer solution, there will be a difference on
the pH value.
Weak Acid, Weak Base and Their Salts.

Buffer system is a weak acid solution (or weak base) and their salts.
Weak acid or weak base are acid or base that only partially ionized in water.
Acetic acid, for example, is one of the weak acids. If it is dissolved in water,
the equilibrium will occur:
Most of the acetic acid molecules remain in solution, while only a

small amount of acetic ions are present in the solution. Ammonium
Hydroxide (Ammonia solution) is one example of weak base since this base
is partially ionized in water to give NH4+ and OH- ions.

Acid and base can be classified as strong and weak depend on its
degree of ionization. The acids that dissociated in large quantity (close to
100%) in aqueous solution include H2SO4, HCl, and HNO3. Ionic base such
as NaOH, KOH nad Ca(OH)2 exist as ion in the solid phase and also
perfectly dissociated in water. In contrast, acids such as CH3COOH, HCN
and H3PO4, organic acid (RCOOH, R = hydrocarbon group), and some
bases (amine, R-NH2) are only partially (only a few percent) ionized in
water.
Salt of weak acid is a salt that has anion from weak acid. Salt can be
produced by allowing weak acid to react with a base. For example, salt that
contains acetate ion CH3COO- is an acetate salt. Certain salts, such as
sodium acetate, CH3COONa can be made from suitable acid and base.
Similarly, sodium cyanide, NaCN, and potassium cyanide, Ca(CN)2

are cyanide salts, -CN. Potassium monohydrogen phosphate, K2HPO4 is a
potassium dihydrogen phosphate salt, K2HPO4 as shown by the equation:
The weak base salt has a cation with a base. Ammonium hydroxide
salt, NH4OH (ammonia, NH3 solution) for example, is a ammonium
chloride, NH4Cl and ammonium sulphate, (NH4)2SO4. So, buffer solutions
are produced by making the solution that contains whether weak acid or
weak base and its salt.
How Buffers control pH

How does the buffer system maintain a constant pH, which controls
the concentration of H+ and OH- ions? In this experiment, we will use a
mixture of acetic acid, CH3COOH and sodium acetate, CH3COONa, in a
solution for representing how the buffer system works. If H+ = (HCl, as an
example) is added to the buffer system, most of H+ ions (hydrogen ion, H2O
reacts with CH3COO) forms acid that is only partlially ionized (weak acid)
CH3COOH and H+ ion concentration that only increases slightly.

If OH- ion (NaOH) is added to the buffer mixture, the following
reaction occurs.
Concentration of hydroxide ions will not increase significantly

because most of OH- ions from NaOH react with acetic acid to produce
acetate and water.
In blood, the important buffer pairs are H2PO4- and PO42- as well as
H2CO3 and HCO3-. This following equation shows how the excess of H+ and
OH- ions are removed (controlled) with its buffer.
and
In working with pH and buffer system, it should be noted that a

change of 1 unit of pH means a change of one tenth (1/10) concentration of
H+ and OH- ions. pH 5 solution has only 1% (1/100) concentration of H+
from pH 3 solution, but 1000 times greater than pH 8.
A. The pH change of non-buffer solution

1. Preparation of 0.0001 M (10-4 M) HCl solution:
Experimental Method
Take 5 mL of 0.1 M HCl solution with 5 mL of volumetric pipette
and insert it to the volumetric flask 50 mL, then add distilled water
until the limit mark and shake it until homogenous. (0.01 M HCl
solution). Take 5 mL of 0.01 M HCl solution with 5 mL of

volumetric pipette and insert it to the volumetric flask 50 mL, then
add distilled water until limit mark and shake it until homogenous.
(0.001 M HCl solution). Take 5 mL of 0.001 M HCl solution with
5 mL volumetric pipette and insert it to the volumetric flask 50 mL,
then add distilled water until limit mark and shake it until
homogenous. (0.0001 M HCl solution). The solutions are divided
into 3 test tubes; test tube 1 with no addition of any solution, test
tube 2 is added by 1 drop of 1 M HCl and test tube 3 is added by 1
drop of 1 M NaOH. Then, the pH of the three tubes is determined.
2. Preparation of 0.0001 M (10-4 M) NaOH solution:
Experimental Method
Take 5 mL of 0.1 M NaOH solution with 5 mL volumetric pipette
and insert it to the volumetric flask 50 mL, then add distilled water
until limit mark and shake it until homogenous. (0.01 M NaOH
solution). Take 5 mL of 0.01 M NaOH solution with 5 mL
volumetric pipette and insert it to the volumetric flask 50 mL, then
add distilled water until limit mark and shake it until homogenous.
(0.001 M NaOH solution). Take 5 mL of 0.001 M NaOH solution
with 5 mL volumetric pipette and insert it to the volumetric flask 50
mL, then add distilled water until limit mark and shake it until
homogenous. (0.0001 M NaOH solution). The solutions are
divided into 3 test tubes; test tube 1 with no addition of any
solution, test tube 2 is added by 1 drop of 1 M HCl and test tube 3 is
added by 1 drop of 1 M NaOH. Then, the pH of the three tubes is
determined.
B. The pH Change of Buffer solution
1. Preparation of Buffer Solution of H2PO42- and HPO42-:
Experimental Method
Mix 10 mL of 0.5 M NaH2PO4 with 10 mL of 0.5 M NaHPO4 in 50
mL of beaker. The mixture is stirred until homogenous. Solution is
divided into 2 test tubes; test tube 1 is added by 1 drop of 1 M HCl
and test tube 2 is added by 1 drop of 1 M NaOH. Then, the pH of
the both tubes is determined.
2. Preparation of Buffer Solution of 1 M CH3COOH and 1 M
CH3COONa:

Experimental Method
Mix 10 mL of 1 M CH3COOH with 10 mL of 1 M CH3COONa in
50 mL of beaker. The mixture is stirred until homogenous. Solution
is divided into 2 test tubes; test tube 1 is added by 1 drop of 1 M
HCl and test tube 2 is added by 1 drop of 1 M NaOH. Then, the pH
of the both tubes is determined.
3. Preparation of Buffer Solution 1 M NH4OH and 1 M NH4Cl:
Experimental Method
Mix 10 mL of 1 M NH4OH with 10 mL of 1 M NH4Cl in 50 mL of
beaker. The mixture is stirred until homogenous. Solution is divided
into 2 test tubes; test tube 1 is added by 1 drop of 1 M HCl and test
tube 2 is added by 1 drop of 1 M NaOH. Then, the pH of the both
tubes is determined.
4. Preparation of Buffer Solution 1 M NH4OH and 1 M NH4Cl:
Experimental Method
Mix 5 mL of 1 M NH4OH with 20 mL of 1 M NH4Cl in 50 mL of
beaker. The mixture is stirred until homogenous. Solution is divided
into 2 test tubes; test tube 1 is added by 1 drop of 1 M HCl and test
tube 2 is added by 1 drop of 1 M NaOH. Then, the pH of the both
tubes is determined.

References
Anonim, 2000, Petunjuk Praktikum Kimia Dasar I, Laboratorium Kimia

Dasar FMIPA UGM.
Anonim, 2000, Petunjuk Praktikum Kimia Dasar II, Laboratorium Kimia
Dasar FMIPA UGM.
Beran, J.A., 2010, Chemistry in the Laboratory, 2nd.ed, John Wiley and
Son., New York, USA.
Heasley, L., Christensen, V. J., Heasley, G. E., 1997, Chemistry and Life in
the Laboratory, 4th ed., Prentice Hall. Inc, USA.

GENERAL CHEMISTRY II /ORGANIC CHEMISTRY
Authors
Nuryono
Iqmal Tahir
Deni Pranowo
Winarto Haryadi
Indriana Kartini
Sri Sudiono
Laboratory of General Chemistry

Faculty of Mathematics and Natural Sciences UGM
Sekip Utara Yogyakarta 55281, telp 0274-545188; 6492370, Fax. 0274-545188
email: chemistry-kd@ugm.ac.id
PREFACE
Thank God we pray to the presence of Allah SWT, Who has

bestowed His Mercy and Grace, so that the preparation of this General
Chemistry I Laboratory Work Manual Book can be completed in due time.
Do not forget to thank to all those who have helped the preparation of this
book. This Laboratory Manual Book provides guidance for undergraduate
students to work at General Chemistry Laboratory of Faculty of
Mathematics and Natural Sciences of UGM at the odd semester.
Improvement and refinement to the previous Laboratory Manual of
General Chemistry Lab Work that has long been used by General Chemistry
Laboratory for adapting the needs and the development of sciences have
also been included in this edition. General Chemistry Laboratory of Faculty
of Mathematics and Natural Sciences UGM is one of service laboratories,
which is not only serving Lab Work for Chemistry Department Students,
but also serving for other students from other departments who require basic
knowledge and skill of chemistry. This book is completed with warnings
about occupational safety and health of works at the laboratory, so it is
expected that workplace accident in the laboratory can be avoided.
Hopefully all users of this book can use this book and can get the
benefits from it. Finally, supported critics and suggestions are our hope to
improve this book.
Team
2 General Chemistry II Lab. Work

LIST OF CONTENTS
PAGES
Cover Page 1
Preface 3
Contents 4
Schedule of General Chemistry I Laboratory Work 5
Laboratory Work Rules at General Chemistry Laboratory 6
Introduction of Laboratory Techniques and Safety on Laboratory 8
Experiment P : Introduction of Laboratory Equipment and Basic 14
Work Techniques at Laboratory
Experiment A-1 : Saponification Reaction and Determination of 15
Surfactant Properties of Soap and Detergent
Experiment A-2 : Preparation of Ethyl Acetate via Esterification 19
Reaction
Experiment B-1 : Analysis of Aspirin and Caffeine in Tablets 23
Experiment B-2 : Separation of Compounds using Chromatography 27
Experiment C-1 : Polymer – Macromolecule 30
Experiment C-2 : Identification of The Hydrocarbon Compounds 34
References 40
General Chemistry II Lab. Work 3

SCHEDULE
GENERAL CHEMISTRY II LABORATORY WORK
Group Laboratory Test and Work in week(s)

Number
1 2 3 4 5 6 7 8 9
I Assistance P A-1 A-2 B-1 B-2 C-1 C-2 Final Test
II Assistance P A-2 A-1 B-2 B-1 C-2 C-1 Final Test
III Assistance P B-1 B-2 C-1 C-2 A-1 A-2 Final Test
IV Assistance P B-2 B-1 C-2 C-1 A-2 A-1 Final Test
V Assistance P C-1 C-2 A-1 A-2 B-1 B-2 Final Test
VI Assistance P C-2 C-1 A-2 A-1 B-2 B-1 Final Test

LABORATORY WORK RULES
AT GENERAL CHEMISTRY LABORATORY
1. All participants must be on site at the appointed time (according to the

respective schedule). If the participant is late of more than 5 (five)
minutes from the appointed time, the participant is not allowed to join
the Lab Work on schedule and is required to follow the Lab Work on
another schedule.
2. During the lab work, participant must wear clean white long-sleeved
laboratory coat, Striped neatly and wearing shoes (Forbidden to use
sandals)
3. Every participant should write lab work report in the specified format
and signed by the assistant after the Lab Work. The reports are
collected before the next lab work. Lab work report is a requirement to
follow the next lab work.
4. Participant is not allowed to carry their stuffs except ones needed for
Lab Work. Stuffs that are not allowed to carry must be put into the
available locker. 1 locker is for 1 group.
5. Every participant must check all the equipment before Lab Work and
return the equipment after being used in dry and clean condition.
Before leaving the laboratory, participant must return all chemical
bottle that have been closed tightly to the original place, and return the
desk and locker keys. Losing keys is the responsibility of the
participants.
6. Every participant must keep the laboratory clean, work with calm,
and organized. During the lab work, participant must be polite, both in
speaking and behaving.
7. Assessment of the Lab Work is formative, carried out continuously
during the process of Lab Work. Assessment includes the
understanding of laboratory techniques and occupational health and
safety culture, material understanding (pre-test, laboratory skills, report
writing and final test).
8. Participant, who has not joined the Lab Work on schedule, is allowed to
join the following Lab Work (inhal) if the requirements are fulfilled, by
filling in an inquiry letter to the Head of General Chemistry Laboratory.

9. Taking the Lab Work not in the scheduled time cannot be more than
twice. Absence twice without replacement, results in failing to do the
Lab Work (E score).
10. Point number 9 does not apply to those who are sick and hospitalized at
the hospital.
11. If the participant violates the things set out above then participants may
be excluded from the laboratory and unable to attend the Lab Work that
day. The lab work is then declared to be failed and not allowed to join
the following Lab Work.
12. Things that have not been mentioned above and required for successful
implementation of the Lab Work will be arranged accordingly.
Yogyakarta, December 2017

Head of General Chemistry
Laboratory
Dr. Deni Pranowo, M.Si.

INTRODUCTION OF LABORATORY TECHNIQUES
AND SAFETY CULTURE
A. Introduction of equipment
Laboratory Work Manual of General Chemistry I has discussed various
glasswares that are often used for working at laboratory. The Manual will
discuss some of the equipments that will be used in this laboratory work of
General chemistry II at General Chemistry Laboratory.
1. Equipment for extraction process (extractor)

The separation of a compound from the mixture can
be carried out by various methods. The methods that can
be performed are extraction, distillation, or by
chromatography.
Extraction is one step to get the compound from a
mixture. Based on the phases, extraction is classified into
liquid-liquid extraction and solid-liquid extraction.
Liquid-liquid extraction is performed to obtain a
compound in a mixture within liquid phase with another
liquid solvent. The basic principle of this separation is a
compound that has different solubility in two different
solvents. The equipment that used is separation funnel.
Solid-liquid extraction is performed to separate one component within a

solid compound by using liquid solvent. The equipment that used is Soxhlet
extractor. For example, to extract non-essential oils (compounds contained
in non-volatile natural product). The extracting solution (solvent) is placed
on a round bottom flask (a), the sample has been wrapped with filter paper
placed on the extractor tube (b), the upper part (c) the Alihn condenser and
ball condenser. This Soxhlet extractor is a continuous extractor, the solvent
in the flask is heated and evaporated, condensed at the condenser (c), then
the solvent will re-enter into the extractor. When the solvent has reached the

capillary upper limit, the solvents that have been in contact with the sample
will enter in the flask (a), and so on.
2. Equipment for distillation (distiller)

Distillation is a separation method based on the difference boiling point
of components in a mixture. The usual distillation is carried out for the
separation of the mixture having considerable boiling point difference.
While steam distillation is carried out for the separation of the mixture
having considerable saturated vapour pressure difference between the
components present in the mixture. In addition, distillation may also be
carried out at the pressure under atmospheric pressure. This method is
known as distillation under reduced pressurre. When the boiling point
difference of the components present in the mixture is small, then the
distillation appliance component is added with the Vigreux column.
Distillation apparatus vapour distillation apparatus

3. Equipment for reflux
Chemical reactions sometimes can
perfectly occur above the room
temperature or at the boiling point of the
solvent used in the reaction system. One
of the equipments that can be used at high
temperature is reflux set. Some of reflux
sets are shown at the figure beside. There
are some types of reflux set.
The most simple reflux set: [1] occupied with round bottom flask (a)
and Liebig condenser (b), [2] occupied with round bottom flask (a), Liebig
condenser (b) and separation funnel (c). [3] occupied with round bottom
flask (a), Liebig condenser (b), separation funnel (c) and stirrer or
thermometer (d).
4. Buchner Funnel
Buchner funnel is used for filtering processes that
cannot be done with common filtration. The filtration is
usually carried out by the utilization of gravity, while in
the Buchner funnel, the filtrate is separated from the
mixture by vacuum.
5. Chamber
This equipment is used for Thin Layer Chromatography (TLC)
experiment. It is used as a container for eluent and TLC plate that has been
spiked by sample or standard.
B. Introduction of Healthy and Safe Environment at Laboratory

Working skills in the laboratory can be obtained by students through
practicum activities. The more often and serious students work in the
laboratory, they will be more skilled. The skills are required to support the

research of thesis. Students, laboratory and practicum seem to be
inseparable unity. On the other hand, the lab is a terrible place since it
contains various equipment and chemicals which are potentially dangerous.
Possible hazards include the presence of chemicals that are carcinogenic
either due to their vapour or exposure to certain substances in the skin, fire
hazards, poisoning hazards, and other potential hazards. In addition, the
people who work at great risk since they use:
1. Chemicals which are explosive, flammable, corrosive, carcinogenic and
toxic.
2. Glassware that break easily and can affect our bodies.
3. Electrical appliances such as electric stoves, oven, heating lamps, UV
lamps and so on, which may cause an electric shock.
4. Water heater and oil that can be sprinkled.
The existence of this potential should not be over-feared by avoiding
practicum activities or passive in every practicum. However, we must act
more actively and find out every potential danger in the laboratory so that
we are always vigilant and careful in every action to avoid every danger that
can happen any time.
The things we should do while working in the laboratory include:
1. Preparation Stage
a. Knowing exactly (precisely and accurately) what will be done on the
lab work, by reading the lab guide book, knowing the purpose and
workings and how the experimental data will be obtained, knowing
the things or actions to avoid, such as keeping the combustible
material from the source of fire, throw the trash and waste of lab
work at a predetermined place and so forth.
b. Knowing the properties of the materials that will be used whether
materials are flammable, toxic, carcinogenic or harmful, and so on,
so as to avoid potential hazards that may result from the chemicals
used.
c. Preparing body protective equipment such as, white lab coat with
long sleeves, goggles, rubber gloves, mask, etc. according to the
requirement of lab.

2. Practice Stage
a. Wearing body protective equipment properly.
b. Checking the equipment and materials to use.
c. Assembling the tools used appropriately, and taking enough
chemicals. DO NOT EXCESS OUT when using chemicals as they
may cause environmental pollution.
d. Removing chemicals from the experiments in place according to the
residual properties of the materials used.
e. Working in an orderly, calm and diligent manner, record the
necessary data.
3. Post-Practice Stage
a. Returning the body protective equipment properly.
b. Avoiding any possible dangers by turning off electrical equipment,
tap water, closing containers of chemicals tightly (according to its
bottle lid).
c. Cleaning the place or table where you work.
d. Getting out of the lab in an orderly manner.
The fact that happens to this day is that some students who work in the
laboratory have never noticed the risks that occur in the laboratory. This is
due to the lack of knowledge of the risks or hazards of working in the
laboratory or awareness of occupational health and safety in the laboratory.
Knowledge of material properties becomes a necessity before working in the
laboratory. The properties of the materials in detail and complete can be
read on the Material Safety Data Sheet (MSDS) in books, CDs, or over the
internet. The following explanation simply conveys the nature of the
material based on the existing drawing code on the packaging of the
chemicals.
Hazard Symbol
Legislation on packing and labelling of hazardous substances
determines the level of chemical hazards under the following categories:

Toxic. This product may cause death or serious illness if
the chemical enters the body through respiration,
inhalation of vapours, odours or dust, or skin resorption.
Corrosive. This product can damage the living tissue,

causing irritation to the skin, itching can even cause skin
to peel. Watch out! Do not get blown to the eye.
Explosive. This product may explode in the presence of

heat, sparks, shocks or friction. Some compounds form the
explosive salts of contact (alloys with metal / metal).
Oxidizing. This compound can cause a fire. This

compound produces heat in contact with organic matter
and reducing agents.
Flammable. This compound has a low flash point and a

material acting with water or moistening air (misty) to
produce flammable gas (like hydrogen) from a metal
hydride. Flame source of Bunsen fire, hot metal surface,
electric spark jump and others.
Harmful. Irritant chemicals cause skin burns, mucus,

disrupt the respiratory system. All chemicals have
properties like this (harmful) especially when contact with
skin, inhaled or swallowed.

EXPERIMENT P
INTRODUCTION OF LABORATORY EQUIPMENT AND
BASIC WORK TECHNIQUES AT LABORATORY
Experimental Objectives: To understand the use of some equipments at

laboratory and some of basic work techniques
at laboratory
I. Introduction of Laboratory Equipments

1. Draw all available laboratory equipments in the basket on your
desk!
2. Write down the name and function of each equipment you draw!
II. Introduction of Basic Work Techniques at Laboratory

1. Draw some set of equipments on your desk!
2. Observe the process!
3. Explain the function and the working principle of the sets.
III. Introduction of Dilution Technique

1. Make 100 mL of 0.1 M sucrose solution (C12H22O11)!
2. Make 100 mL of 0.01 M sucrose solution (C12H22O11) from 0.1 M
sucrose solution!

EXPERIMENTAL A-1:
SAPONIFICATION REACTION AND DETERMINATION OF
SURFACTANT PROPERTIES OF SOAP AND DETERGENT
Experimental Objectives : 1. To study the saponification process of fat by

using potassium hydroxide (KOH) and
sodium hydroxide (NaOH).
2. To study the differences of soap and
detergent properties.
3. To determine the degree of saponification
of fat.
Basic Theory:
Triglycerides are relatively high molecular weight fat or ester oils that
can be saponified (hydrolyzed) with an alkaline solution to produce soap
and glycerol.
Based on the reaction, the soap is said to be a mixture of carboxylic

anion salts and univalent cations. Mixed anions can be generated since each
triglyceride molecule contains different type of fatty acid residue. It is also
because the oil or fat is a mixture of fatty acid molecules.
Potassium soap is more soluble in water than sodium soap. Potassium
soap is commonly used as a liquid soap. Soap is hard when made from fat or
oil that has high degree of saturation such as lard or shorten. On the other
hand, saponification from unsaturated oil will produce soft soap.

Treatment of soap solution with diluted hydrochloric acid will produce a
mixture of fatty acids as follows:
Synthetic detergents differ from soaps because detergents are salts of

long-chain alkyl sulfuric acid or an alkyl benzene sulfonic acid, which is
different from the long-chain carboxylic acid.
The soap and detergent molecules can dissolve non-polar particles such
as fat, oil and lard. The molecules are composed of both non-polar ends of
hydrocarbons and polar or ionic ends. The non-polar part will surround the
oil droplets and dissolve them in accordance with the principle of “like
dissolve like” (compounds that have similar polarity will dissolve each
other). The polar / ionic end of the soap molecule will be dissolved in water.
The soap cannot work well in hard water due to the presence of divalent
cations, such as Ca2+, Mg2+ and Fe2+, which may interact with soap
carboxylate anion to generate the precipitate. It is often encountered as a
crust on the walls and the bathroom faucet. On the other hand, anions of the
detergent (alkyl sulphates or alkyl sulphonates) cannot form precipitate with
the cations. Thus, the detergent can be used effectively in hard water.

Experimental Method
A. Preparation of Potassium and Sodium Soaps
- Insert 6 mL of oil to the 50 mL of beaker. Add 40 mL of
KOH/ethanol 10%. Heat the mixture while stirring. Monitor the
completion of saponification reaction by dropping the reaction
mixture to water (no droplet of fat). Potassium soap is formed until
viscous liquids formed.
- Add 50 mL of distilled water to the soap. The mixture is divided
into 2 part with the volume of 25 mL for each. The first is
potassium soap and the second is used to prepare the sodium soap.
- Insert 25 mL of potassium soap to the 100 mL of beaker. Add 25
mL of saturated NaCl, stir until blended and filter. The solid formed
is sodium soap.
- Collect potassium and sodium soap at the available container.
- Use the available soap for experimental materials.
B. Analysis of fatty acid of soap

- Insert 10 mL of potassium soap solution to the test tube.
- Add dropwise HCl to the tube and strongly shake the tube for
several times until the solution becomes acidic.
- Test the solution with litmus paper.
- Filter and take the solid formed using stir rod.
- Place the solid in the test tube and add 20 drops of acetone into the
tube. Observe the solubility of solid.
- Repeat the procedure for palm oil sample and sodium soap.
C. Soap and detergent properties
- Take 3 watch glasses. Each of them is dropped by 1 drop of oil.
- The first, second and third watch glasses are cleaned by 3 drops of
sodium soap, potassium soap and detergent, respectively.
D. The ability as surfactant (hard ions effect)
Take 12 test tubes
a. Add 1 mL of sodium soap solution to 4 of the first test tubes
b. Add 1 mL of potassium soap solution to 4 of the second test tubes
c. Add 1 mL of detergent solution to 4 of the third test tubes

Add 1 mL of 0.1% CaCl2, 0.1% MgCl2, 0.1% FeCl2 and tap water to
each test tube.
Discussion
1. Explain why the addition of 1 drop of soap solution to the water in
the preparation potassium soap can be used as to determine whether
the saponification reaction is complete!. Based on molecular
structure, why the saponification product can dissolve in water, and
not the fat!
2. Explain the structure of sodium soap whether sodium soap includes
salt type!.
3. Can potassium soap and sodium soap clean fat stains?
4. Explain whether metal ions can form precipitates with soap
molecules or detergent molecules? Which materials can cause the
formation of precipitate?

Ethanol is a volatile solvent, flammable in the open air and can cause
dizziness if inhaled. Acetone is a flammable solvent and should be kept away
from a flame.

EXPERIMENT A-2:
PREPARATION OF ETHYL ACETATE VIA ESTERIFICATION
REACTION
Experimental Purpose: To study the concentration effect of sulfuric acid

catalyst in the preparation of ethyl acetate via
esterification reaction.
Basic Theory
Interaction between organic acid and alcohol can produce ester. The
reaction occurred is a reversible reaction and very slow. The preparation of
the ester is known as esterification reaction. The opposite reaction, the
decomposition reaction of the ester into alcohol and the acid, is called the
hydrolysis reaction.
The esterification process can be accelerated in the presence of

concentrated sulfuric acid or hydrochloride acid. This reaction is carried out
by refluxing the mixture of organic acids and alcohols with few mineral
acids. Equilibrium will be achieved after the reaction lasts for several hours.
The use of mineral acids as catalysts in esterification reactions was
introduced by F. Fischer and Speier in 1895.
Ethanol and acetic acid in stoichiometric amount react in the presence
of slightly concentrated sulfuric acid. When 2/3 parts of ethanol and acetic
acid reacts, there will be a mixture comprising 2/3 parts of the ester and
water, while the remaining 1/3 is in the form of ethanol and acetic acid.
According to the rules of Mass Action Law by Goldberg and Waage,
the esterification reaction equilibrium constant can be expressed by the
following formula:
[ethyl acetate][H2 O] (2⁄3)(2⁄3)

𝐾= = =4
[acetic acid][ethanol] (1⁄3)(1⁄3)

If a certain amount of ethanol and acetic acid are reacted, then the
amount of ethyl acetate formed after equilibrium can be calculated. For
example ethanol is a mole and acetic acid b mol. When the equilibrium is
reached:
𝒙𝒈𝒙 𝒙𝟐
𝑲= =
(𝒂 − 𝒙)(𝒃 − 𝒙) (𝒂 − 𝒙)(𝒃 − 𝒙)
To enlarge the esterification yield, the equilibrium must be shifted to

the right. This can be achieved by enlarging the concentration of acetic acid
or alcohol as well as by binding to water molecules with the addition of
concentrated sulfuric acid and dry hydrochloric acid (HCl gas).
The esterification mechanism can be described as follows.
Step 1:
The proton (H+) of mineral acids is bounded on by a pair of electrons of
oxygen atom from organic acids to generate oxonium ions.
Step 2:
There oxonium ions react with alcohols and the release of water
molecules to form substituted another oxonium ions.
Step 3:
The substituted oxonium ions release the proton to produce the ester.

The proton used in the first step will be released in the last step.
According to the Lewis acid-base theory, the function of protons is as
electron receptors. Boron fluoride which is a strong electron receptor
substance can be also used as an effective catalyst.
- Insert 25 mL of acetic acid-alcohol mixture to the 50 mL of
volumetric flask. Add some drops of concentrated sulfuric acid
(based on instruction). Then, add 1-2 boiling stones.
- Carefully set the reflux apparatus.
- Heat the mixture with low heat (about 5 minutes).
- After the reflux is complete, the mixture is briefly cooled.
- Distil the mixture at (approximately at 70 C) for 10 minutes and
collect the distillate.
- Neutralize the distillate with 5% Na2CO3 (drops), then check with
pH paper.
- Move the neutralized distillate to the separation funnel and add
dropwise saturated solution of CaCl2 to separate the ester layer.
- Collect the ester layer into the 50 mL of Erlenmeyer and add 1 gr of
MgSO4 crystal.
- The ester obtained should be moved to the 10 mL of pre-weighed-
graduated cylinder.
- Record the volume, density, colour and odour of the result obtained.
- Compare the result obtained with the other groups.
Discussion
1. What are the uses of the concentrated sulfuric acid and boiling stones in
this reaction?
2. What are the uses of the addition of saturated CaCl2 solution and
MgSO4 crystal in the purification process of ester?
3. What are the differences between reflux and distillation process?

4. How to determine density of the product?
5. What is the maximum theoretical results can be obtained? Calculate the
yields!

Glacial acetic acid is a weak acid that has irritating and pungent odour.
Students are advised to use mask. Ethanol is a solvent that is volatile, can
cause headache if inhaled and flammable in the open air. Concentrated
sulfuric acid is a strong acid, strong oxidant, very irritating and should be
used under the fume hood.

EXPERIMENT B-1:
ANALYSIS OF ASPIRIN AND CAFFEINE IN TABLETS
Experimental Objectives: To determine the concentration of aspirin and

caffeine in tablets.
Basic Theory
A. Aspirin
Aspirin is a widely used drug ingredient. This compound is effective
as antipyretic drugs (lower the fever), anti-inflammatory, analgesic, relieve
headache, neuralgia and rheumatism. Aspirin is an ester derivative of
salicylic acid and is prepared via the acetylation of salicylic acid with acetyl
chloride or acetic acid anhydride. The the preparation of this compound is as
follows:
Aspirin is an acidic compound. To determine the concentration of

aspirin, the titration with 0.1 N NaOH using phenolphthalein as indicator
may be conducted. Acetyl group in this neutralization reaction is hard to
remove.

Titration with Phenolphthalein Indicator is terminated when the
colour changes within 1 minute. If NaOH is excess, the following reaction
will occur:
B. Caffeine
Caffeine is an alkaline compound. Another name for caffeine is 1,3,7-
trimethyl xanthine which has the structure as follows:
Caffeine is present in coffee beans (0.5%) and tea (2.4%). In

addition, it has physiological effect as a stimulant and is often found in
some medicinal tablets such as aspirin tablets.
The double bond (C=C) in caffeine can undergo the addition
reaction with iodine. To determine the content or concentration of caffeine,
the solution containing caffeine is added to standard Iodine solution which
has been known volume and concentration. The excess Iodine, after the
addition reaction, is titrated with standard sodium thiosulfate solution
(Na2S2O3).. The reaction is as follows:

Experimental Method
A. Analysis of Aspirin
- An aspirin tablet to be analysed is weighed and inserted into
porcelain, crushed until smooth and then fed into 125 mL
Erlenmeyer.
- Wash the porcelain with 25 mL of alcohol until clean, then pour the
alcohol to that Erlenmeyer.
- Shake the Erlenmeyer for 5 minutes, then heat the mixture with the
spirit lamp until boiling.
- Insert the mixture to the 100 mL of volumetric flask, add distilled
water until the limit mark.
- Take 10 mL of the mixture with volumetric flask then place into the
Erlenmeyer. Add 2 drops of PP indicator to the solution.
- Titrate with 0.1 M NaOH until the pink colour remained in 1
minute.
- Note the volume of NaOH used. Repeat the titration for 3 times. (1
mL 0.1 M NaOH = 0.01802 gr of aspirin)
B. Analysis of Caffeine
- An aspirin tablet to be analysed is weighed and inserted into
porcelain, crushed until smooth and then fed into 125 mL
Erlenmeyer.
- Wash the porcelain with 25 mL of neutral alcohol until clean, then
insert the mixture to the 100 mL volumetric flask. Shake it and
remain for 10 minutes.
- Add 5 mL of 10% H2SO4, 20 mL of 0.1 M I2 and add the distilled
water until the limit mark.
- Shake again, allow stand for 10 minutes. Then, filter it.
- Take 10 mL of the filtrate with volumetric pipette then insert to the
125 mL of Erlenmeyer. Add 3 drops of starch and titrate with
Na2S2O3 until the blue colour disappeared.
- Note the volume of Na2S2O3 used. Repeat the titration for 3 times.
(1 mL 0.1 M Iodine = 0.01802 gr of aspirin)

Discussion
1. What is the definition from neutralization reaction, redox reaction,
volumetric analysis and alkalimetry titration?
2. How does the colour change of PP indicator at the acidic condition into
alkaline condition?
3. Write the redox reaction between Iodine and sodium thiosulfate!
Weight of Tablet (g) 0.1 M NaOH (mL) 0.1 M Na2S2O3 (mL)
Calculation of aspirin concentration

VNaOH (mL)x 0.01802 x 100%
=…%
weight of tablet
Calculation of Caffeine concentration

[𝑉𝐼𝑜𝑑 (𝑚𝐿) − 𝑉𝑁𝑎2𝑆2 𝑂3 (𝑚𝐿)]x 0.00485 x 100%
=…%
weight of tablet

NaOH solution is a strong base, feels slippery on the skin. Alcohol is
volatile solvent, can cause headache if inhaled and flammable to the open
air. H2SO4 solution is a strong acid and very irritating. I2 solution is a
brown solution, irritating and leave brown scars on skin. Starch solution is
an easily damaged materials, should be used in fresh conditions.

EXPERIMENT B-2
SEPARATION OF COMPOUNDS USING CHROMATOGRAPHY
Experimental Objectives: 1. To understand the use of Thin Layer

Chromatography as separation method
2. To use the TLC to separate the components of
essential oil.
Basic Theory
A. Chromatography
Chromatography is one of separation methods based on the difference
on distribution of components between two different phases (stationary and
mobile phases). Stationary phase is a fixed phase that does not move within
the system, while the mobile phase is a phase which moves through a layer
that covers the surface of the stationary phase. The different matter
interaction of samples between stationary and mobile phase cause the
moving rate of those components becomes different.
Stationary phase might be a solid or liquid that eluted in a supported
solid, while the mobile phase is either a solution or a gas. Based on the
difference of the stationary phase and the mobile phase, it is known as the
absorption chromatography and partition chromatography. Absorption
chromatography is a chromatography that uses a stationary solid phase, such
as TLC, ion exchange chromatography and column chromatography.
Partition chromatography uses a stationary phase of a liquid, such as paper
chromatography.
The adsorption chromatography is based on the retention of the solute
adsorption by surface absorbent. Separation is affected by the equilibrium
occurring in the interface plane between the solid stationary phase and the
liquid mobile phase. As the sample is adsorbed, the solute is forced to move
by the mobile phase stream, so that large affinity molecules will be
selectively retained in the stationary phase.

B. Thin Layer Chromatography (TLC)
Thin Layer Chromatography (TLC) is one type of chromatography
which uses a stationary phase in the form of a solid subject attached to a
glass plate or plastic plate. In TLC, the separated sample component is
absorbed by the solid phase of the solid adhered to a thin plate by a mobile
phase that flows through the solids absorbent. The sample component will
be separated in stationary phase that caused by the difference in the rate of
moving of one component to another which is depend on the solubility of
the sample component.
The mobile phase used for TLC depends on the compound to be
separated. This depends on the degree of polarity of the sample component
to be separated. Components with greater polarity will be better or separate
easily using a large polarity solvent as well. If the sample is non polar, it
will be more easily separated using a solvent that is not or less polar.
The identification of separated compounds on TLC is based on the
value of Rf (Retardation factor), which is then compared with the standard
Rf value. The Rf value can be formulated as follows:
distance moved of a compound from the initial point
Rf=
distance moved of a solvent from the initial point
The effect of eluent to the separation of sample components.
- Provide some chamber, then fill it with various eluents with
different polarity: PE (2 mL), methanol (2 mL) and mixture of PE-
Methanol (As directed by assistant).
- Take TLC plate (size of 2x6 cm) and put the boundary mark (line)
with pencil on the TLC plate: 0.5 cm from the bottom mark and 0.5
cm from the upper mark.
- Take the sample with capillary pipe.
- Spot the sample on TLC plate on the bottom line. Allow a few
moments to evaporate the solvent.
- Insert the TLC plate into the chamber. Allow a few moments until
the solvent reach the upper line.
- Take the TLC plate and dry it.
- Observe the spot formed on the TLC plate under the UV light.

- Mark with a pencil and calculate the Rf of every spot formed.
- This method can be used also for another compound resulted from
extraction or distillation of various sample.
Discussion and Questions

1. The used eluent may have low or high polarity or a mixture of both.
What is the purpose of mixing two solutions that have different
polarities? Explain!
2. In chromatography, what is the elutropy series?
3. In thin layer chromatography, two spots are found adjacent (attached).
What can be done to keep the two stains separate further?
4. TLC can be used for qualitative and quantitative analysis. Explain!

Methanol is a volatile solvent, can cause headache if inhaled and
flammable to the open air. Benzene is a volatile solvent, can cause
headache if inhaled and flammable to the open air and carcinogenic.

EXPERIMENT C-1
POLYMER - MACROMOLECULE
Experimental Objectives: To describe the polymer forming process

(polymerization) and to identify some
polymer properties.
Basic Theory
Polymers are compounds with high molecular weight, with a range up
to more than 1 million amu (atomic mass unit). Polymers are also often
referred as macromolecules (very large molecules). The process of polymer
formation begins with the incorporation of small molecular units called
monomers. Two monomer units form a dimer structure. Three monomers
will form trimers and oligomers formed from several monomer units. The
arrangement of monomers that make up the polymer can be seen as follows.
The alkenes or substituted alkenes are common examples of monomers.

For example, ethylene can be polymerized to form polyethylene, with the
following reaction:
n [CH2 = CH2] CH2CH2-[-CH2CH2-]n-2-CH2CH2
where n is the symbol that denotes the repetition number of monomers

ranging up to thousands. A clearer example of structure is shown in the
following figure, which describe polypropylene polymer model image,
where its monomer is propylene. The structure is displayed as follows:

Polymers are present in nature and are also present in the form of
synthetic polymers. Examples of natural polymers are starches, glycogen,
cellulose and proteins. Synthetic polymers are widely found and produced
today, including polyethylene, nylon (a polyamide), Dacron, polyvinyl
chloride, Lucite (polymethylmethacrylate) and others. The benefits of
polymers nowadays have expanded widely in supporting human life and
various other needs. Examples of polymer products are plastic articles,
adhesives, fabrics and others.
Various polymers are selected to use due to the superior properties of
these materials. The thermoplastic type polymer will soften if heated and
thus will be easy to make the desired shape. The thermosetting polymer is a
solid that cannot be melted because it does not melt when reheated.
The nature of the polymers is differentiated into their physical properties
and chemical properties.
The physical properties of the polymer include glass transition
temperature, hardness, viscosity and others. Polymer hardness varies, some
are rubbery, some are sticky and some are very hard.
Based on the polymerization reaction, the polymer can be classified into
addition polymer and condensation polymer. The addition polymer is
formed from the repeated addition reactions of the monomer molecules, for
example polymerization of polystyrene formation. The condensation
polymer is formed from the reaction of the monomers followed by the
elimination reaction involving the loss of water molecules or other small
molecules, for example, nylon-forming polymerization. Nylon 6-6 is a
polymer of two different monomers namely adipate and 1,6-diaminohexane.
styrene (monomer) polystyrene (polymer)

Protein is one of the most important natural polymers in life. Proteins
are polymers of amino acids with peptide bonds. The structure of the protein
consists of primary, secondary, tertiary and quaternary structures. The
primary structure of the protein is the main structure of protein consisting of
polypeptide chain, which is a long and straight amino acid polymer. The
secondary structure is the helical shape of the protein strand due to the
hydrogen bond between the H atoms attached to the amine group of an
amino acid with the carboxyl O-atom of the other amino acid. Tertiary
structures are formed due to disulfide bonds so that proteins are globular.
Denaturation of proteins is the breakdown of the natural properties of
proteins that can occur due to the destruction of tertiary and secondary
structures so that the denatured protein has only a primary structure.
Denaturation occurs due to the influence of heat and pH.
Experimental Method
Experiment I
Preparation and identification of polyvinyl alcohol
In this experiment, the formation of polyvinyl alcohol gel is carried out from
PVA solution with the borax solution as a catalyst.
- Take 10 mL of PVA solution and place it on the disposable
container.
- Add 1 drop of food coloring to the solution and stir.
- Add 5 mL of borax solution while stirring.
- The material will clot, do the hand-wringing/ hands-squeezing to
remove the air bubbles.
- Observe what happens if the PVA polymer blob is pushed slowly!
- Observe what happens if the PVA polymer blob is pushed quickly
and suddenly!
- Observe what happens if the PVA polymer blob is spherical and
dropped from a height of about 10 cm.
- Write one word on paper with water ink, cover with a little PVA
clump and close (observe what happens with the writing and on the
polymer). Repeat the same procedure using a regular ballpoint ink.
What is the difference?

- Take a little polymer blob, place it on a watch glass, add 3-4 drops of
0.2 M HCl and do stirring for each drop (observe what happens at the
time of drops on the PVA blob). Next add 3-4 drops of 0.2 M NaOH,
observe the changes.
Experiment II
The influences of pH and heating on the properties and structure of proteins.
1. Provide two test tubes and fill each with water and a solution of pH 1.
2. Heat a tube that contains water to boiling.
3. Put a few drops of albumen/egg white into a test tube containing boiling
water and a solution of pH 1.
4. Observe the changes and explain the phenomena!

Please return Materials such as HCl, NaOH solution and borax
crystal to container (DO NOT THROW TO THE SINK).
Please dispose other chemical material to the available waste bottle.
Although all the solution is in diluted condition, taking the solution must be
used propipette.

EXPERIMENT C - 2
IDENTIFICATION OF THE HYDROCARBON COMPOUNDS
Experimental Objectives : To identify functional groups of hydrocarbon

compounds through chemical reactions
Basic Theory
Functional Group
In the previous section, we have discussed about hydrocarbon
compounds or compounds consisting only carbon atoms and hydrogen
atoms. Can you imagine how many organic compounds can be produced
when nitrogen, halogen, sulfur atoms or other elements come together?
Consider some alcohols, ethyl alcohol (alcohol in beverages), methyl
alcohol (wood alcohol) and isopropyl alcohol (rubber alcohol). They are
very different. However, in the case of chemical reactions, all of these
alcohols undergo the same reaction. All of these reactions involve the -OH
group, just like the double bonds that greatly determine the identity of the
alkenes. In many cases, other parts of the molecule will have no effect, since
the reaction to one alcohol will be the same as the other.
Atoms or atomic groups that determine the molecular reactivity are
called functional groups. For example, the alcohol the functional group is -
OH, the alkene is C = C and so on. The presence of functional groups allows
us to study and characterize the properties of compound. For example, you
can study the general properties of all alcohols rather than you studying any
alcohol present. Descriptions of alcohols, carboxylic acids, esters, aldehydes
and ketones and ethers are presented as follows.
Alcohol
Alcohol is a class of organic compounds containing the -OH functional
group. Alcohol is often expressed in general as R-OH, where R comes from
the abbreviation "Rest of the molecule" or the “Residue of a molecule” (as
the radio host says "rest of the story" which means the other part of a story).
Alcohol is named by using the ol suffix to replace the ane of the
corresponding alkane.

Methanol or methyl alcohol is sometimes called wood alcohol (because
in ancient times the synthesis mainly involves heating wood in air-free
conditions). The synthesis method used today involves the reaction of
carbon monoxide and hydrogen with certain catalysts at elevated
temperatures.
CO(g) + 2 H2(g) → CH3OH(l)
About half of US methanol production is used to produce formaldehyde

used as a liquid / preservative solution and is also used in the plastics
industry. Sometimes, methanol is added to ethanol to make the ethanol not
well consumed by humans and this process is called denaturation. Methanol
has also been considered as a substitute for fuel, although to date there are
still many problems to be faced. New Zealand currently has a similar project
that can generate one-third of its fuel requirements.
Ethanol, also called as ethyl alcohol or grain alcohol, can be produced
in two ways. If the ethanol is to be used as an alcoholic beverage, it must be
produced by fermenting carbohydrates or sugars using enzymes such as
those found in yeast.
C6H12O6(aq) → 2CH3CH2OH(l) + 2CO2(g)
If ethanol is used for industrial purposes such as solvents in perfumery

and drugs or as an additive to fuel (make it into gasohol), this compound is
produced from the hydration reaction of ethylene by using an acid catalyst.
H2C=CH2 + H2O → CH3-CH2-OH
Carboxylic Acid
Carboxylic acid Acetic acid

Chemists often use -COOH or -CO2H to describe this group functional
group. The compounds are named with acidic and oate suffix.
Carboxylic acids can be prepared from the oxidation of alcohols. For
example, if a bottle of wine interacts with air or other oxidizing agent, then
ethanol will oxidize to acetic acid.
CH3CH2OH(l) + O2(g) → CH3COOH(l) + H2O(l)
Formic acid or methanoic acid may also be isolated by distilling ants.

This is easy to do because we often find mounds of ant houses in our yard.
The odor produced by the bite is caused by the presence of formic acid.
Therefore the use of several bases such as baking soda can help neutralize
acid and relieve pain.
Many of these organic compounds have a strong odor. We are sure you
are familiar with the smell of vinegar or acetic acid but other acids have a
strong odor as shown in the following table.
Carboxylic compounds that have a strong odor

Molecular structure Compound name Smell
CH3(CH2)2COOH Butyric acid Rancid of butter
CH3(CH2)3COOH Pentanoic acid Earth worm
CH3(CH2)4COOH Hexanoic acid Goat
Ester
The ester functional group is very similar to the carboxylic acid
functional group unless the existing hydrogen atom has been replaced by
another R group. Esters are prepared by reacting carboxylic acids and
alcohols to produce esters and water. The following reaction shows the ester
compound synthesis.
R–CO–OH + H–O–R’ → R–CO–O–R’ + H2O

Organic acid alcohol esther water

Although carboxylic acids are widely used to make esters have a very
unpleasant odor, but most esters have a pleasant aroma. Wintergreen oil is
an ester and other esters have the aroma of banana, apple, rum, rose and
pineapple. Esters are often used in flavor industries (flavor enhancers in
foods) and perfumes (perfumes).
Aldehydes and Ketones

Both aldehydes and ketones are produced from alcohols. These
functional groups are presented in the following figure.
Aldehida Keton
Formaldehyde, HCHO, is an economically important aldehyde. This

compound is used as a solvent and also to preserve biological preparations.
Formaldehyde is also used to make certain polymers such as Bakelit and
Melmac (which are used for melamine plates). Other aldehydes, especially
those having a benzene benzene, have good odor-like smells and esters are
also used in the perfume and flavor industries.
Acetone, CH3COCH3 is the simplest ketone and has many uses as a
solvent especially for paints. Most people are familiar with wiper blenders
(nail dyes) that use acetone as the base solvent, while ethyl ketone is the
solvent used in adhesives for aircraft models.
Ether
Ether contains an oxygen atom attached to two hydrocarbon groups, R-
O-R. Diethyl ether was once used for anesthesia but in the operating room,
due to its highly flammable nature, this compound must be replaced with
other compounds. Ether is very unreactive (except for combustion), it is
generally used as a solvent in organic reactions. However, these compounds
can also react slowly with oxygen in the air to produce explosive
compounds called peroxides.

Ether can be made from alcohol by removing water (dehydration
reaction). Diethyl ether may also be prepared by reacting ethyl alcohol in
the presence of sulfuric acid:
H SO
2 CH3CH2OH(l) ⎯⎯2 ⎯
⎯4 → CH3CH2 –O–CH2CH3(l) + H2O(l)
If two different alcohols are used, there will be a mixed ether compound
in which the two R groups are not equal.
Experimental Method
ATTENTION!
Use protective goggles when making observations.
The reagents used in this experiment are highly flammable and some
are toxic. Work away from heat and flame and avoid steam exposure,
contact with skin and avoid swallowing. Dispose of the experimental waste
into the organic solvent container provided.
A. Burning of alcohol
Place about 0.5 mL of PE in a vaporizing cup and burn it carefully with
a matching flame. Repeat the same procedure for ethyl alcohol and
isopropyl alcohol. Record the characteristics of the flame!
B. Oxidation of alcohol
B.1 Oxidation of alcohol using potassium permanganate.
Combine 3 mL of methyl alcohol with 12 mL of water and divide the
solution into three equal parts by placing it in three test tubes. Into the fourth
tube add 5 mL of water. Add 1 drop of Sodium Hydroxide (10% NaOH)
into the first tube and 1 drop of H2SO4 into the second tube. Next add 1 drop
of KMnO4 solution into the four test tubes. The fourth tube is used for the
control. The loss of purple permanganate indicates the occurrence of a
reaction (some reactions take a long time). Repeat the oxidation procedure
using isopropyl alcohol.

B.2 Oxidation alcohol using Copper(II)oxide
Place about 2 mL of methyl alcohol in the test tube. Prepare a copper
wire with a spiral tip. Heat alcohol to vaporize a little alcohol in a tube. Heat
the wire spiral in the hottest part of the burner flame to obtain a good copper
(II) oxide layer. Do not overheat the wire. While the wire spiral is still hot,
put it in the tube (not to get into the liquid) and record the results. Reheat the
wire and close it to the tube, and finally dip it into the alcohol. Lift the wire
carefully and smell the vapor from the tube with your nose and the smell of
formaldehyde produced from methyl alcohol.
C. Preparation of Esters
Take 3 test tubes and mix the following reagents in the three tubes.
Tube 1 : 3 mL of ethyl alcohol, 0.5 mL of glacial acetic acid, and 10
drops of concentrated sulfuric acid.
Tubes 2 : 3 mL of isoamic alcohol, 0.5 of mL glacial acetic acid and 10
drops of concentrated sulfuric acid
Tubes 3 : Salicylic Acid Crystals (into about 1 cm in a test tube), 2 mL of
methyl alcohol, and 10 drops of concentrated sulfuric acid.
Heat all tubes by placing them in the boiling water (water bath) for 3
minutes. Products formed:
Tube 1 : Ethyl acetate
Tube 2 : Isoamilacetate
Tube 3 : Methyl salicylate
After heating, pour a small amount of each product on the filter paper
and carefully smell it and mention the type of smell. Dispose of filter paper
that has been used into solid waste disposal.

References
Anonim, 2000, Petunjuk Praktikum Kimia Dasar I, Laboratorium Kimia Dasar

FMIPA UGM.
Anonim, 2000, Petunjuk Praktikum Kimia Dasar II, Laboratorium Kimia Dasar
FMIPA UGM.
Beran, J.A., 2010, Chemistry in the Laboratory, 2nd ed, John Wiley and Son., New
York, USA.
Fiesher, L. F. and Fiesher, M., 1998, Organic Chemistry, 3rd ed., Longman, London.
Heasley, L., Christensen, V. J., Heasley, G. E., 1997, Chemistry and Life in the
Laboratory, 4th ed., Prentice Hall. Inc, USA.

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LABORATORY WORK MANUAL

Laboratory of General Chemistry

Thank God we pray to the presence of Allah SWT, Who has

Yogyakarta, July 2021

General Chemistry I Lab. Work 2

1. All participants must be on site at the appointed time (according to the

3 General Chemistry I Lab. Work

Yogyakarta, July 2021

Dr. Deni Pranowo, M.Si.

General Chemistry I Lab. Work 4

5 General Chemistry I Lab. Work

Laboratory Test and Work in week(s)

I Assistance I A-1 A-2 B-1 B-2 C-1 C-2 Final Test

II Assistance I A-2 A-1 B-2 B-1 C-2 C-1 Final Test

IV Assistance I B-2 B-1 C-2 C-1 A-2 A-1 Final Test

V Assistance I C-1 C-2 A-1 A-2 B-1 B-2 Final Test

VI Assistance I C-2 C-1 A-2 A-1 B-2 B-1 Final Test

General Chemistry I Lab. Work 6

Experimental Objectives : 1. To recognize some simple laboratory

These following will be discussed about simple equipment that used

Figure P.1 Simple glassware for chemistry laboratory work

Here are the description of equipment and function of each

7 General Chemistry I Lab. Work

4. Glass rod/ Stirring rod

General Chemistry I Lab. Work 8

10. Test Tube Rack

9 General Chemistry I Lab. Work

12. Wire Netting

15. Litmus Paper

16. Watch Glass

17. Porcelain Cup

18. Dropping Pipettes/ Pasteur Pipettes

General Chemistry I Lab. Work 10

21. Volumetric Pipette

Several Basic Techniques at Chemistry Laboratory

I. Production of Gas and Introduction of Litmus Paper

11 General Chemistry I Lab. Work

Figure P.2 Technique of gas smelling and pH measurement

Figure P.3 Technique of heating material properly

Information of material properties, Health and Safety

II. Dilution using Volumetric Flask

13 General Chemistry I Lab. Work

General Chemistry I Lab. Work 14

IV. Dilution of Solution

Information of material properties, Health and Safety

15 General Chemistry I Lab. Work

General Chemistry I Lab. Work 16

VI. How to read meniscus

Figure P.6 How to read meniscus

17 General Chemistry I Lab. Work

Experimental Objectives: To understand the use of some equipments at

II. Introduction of Basic Work Techniques at Laboratory

III. Introduction of Titration Technique

General Chemistry I Lab. Work 18

Experimental Objectives : To determine reaction order of MnO4 with

19 General Chemistry I Lab. Work

Reaction order Linear graph

General Chemistry I Lab. Work 20

H2C2O4 Distilled KMnO4 H2C2O4 Distilled KMnO

21 General Chemistry I Lab. Work

Information of material properties, Health and Safety

General Chemistry I Lab. Work 22

Experimental Objectives: A. To determine the constant of molality

23 General Chemistry I Lab. Work