PREFACE

This manual is intended for the use of students in BS Medical Technology, BS Biology and
other related courses enrolled in a one-semester subject in Qualitative & Quantitative
Chemistry (Analytical Chemistry). It is expected that the students taking up this
laboratory course must have basic knowledge and proper laboratory skills necessary to
perform the experiments from this laboratory manual. All of the experiments are
quantitative in nature. It will require the students to observe, analyze and compute in
order to determine the amount of species in a sample.

The experiments from this manual were carefully chosen and made based on the
availability of the reagents, materials, and apparatus in the College of Arts & Sciences
(CAS) stockroom. The number of the experiments is also enough to cover the entire one-
semester of this laboratory course. Moreover, each experiment is designed so that the
students can accomplish the laboratory work in one to two meetings.

The main objective of this manual is to further improve and polish the laboratory skills of
the students. It also aims to develop their analytical skills in order for them to be
proJicient and conJident in solving a problem. Furthermore, it also intends to develop the
student’s intellectual honesty in reporting results and foster teamwork within the group.
This manual also intends or allows the students to aapply and verify their knowledge read
from the textbooks.

The success of the activity or work depends on the preparedness of each of the members
in conducting the experiment. It is expected that each member of the group should have
read the experiment way ahead before performing it. Also, it is important that the student
should have a clear understanding of the objectives of the experiment and as well as its
underlying principle.

Lastly, this manual will undergo revisions to further improve the experiments and its
contents. This manual might have errors in the procedure. Any corrections or suggestions
from the students or faculty will highly be valued and appreciated.

The Authors

2
GENERAL POLICIES:
1. Strictly Personnel Protective Equipment (PPE) such as labgowns and goggles/ safety
eyeglasses together with experiment data sheets are required every experiment. Non-
compliance means NO EXPERIMENT.
2. Visitors are not allowed during experiments unless it is an emergency.
3. No make-up experiments.
4. Arrival in class after Jifteen (15) minutes will be marked as LATE. However, if you
arrive beyond the given grace period and the experiment has started, you are allowed to
perform the experiment (provided you comply with #1) but you will get ZERO for the lab
performance grade.

GRADING OF THE LABORATORY REPORT:

Each experiment will be graded based on the results, laboratory report, laboratory
performance, and answers to the questions posted at the end of the activity. It is expected
that each student should accomplish their own laboratory report and should refrain from
just copying the results or data from their group mates.

SAFETY CONSIDERATIONS & LABORATORY RULES:

1. To prepare for the experiment, always make sure that you have read and
understood the experiment assigned for the day. As a group, you may also prepare
for a work plan so that you may perform the experiment efJiciently.

2. Always wear your personal protective equipment such as lab gown, goggles,
gloves, and facemask (if handling powder and volatile reagents) during the entire
period of the experiment.

3. During the experiment, students should NOT eat, drink or smoke inside the
laboratory at all times.

4. Remove contact lenses before performing the experiment. Contact lenses might
react with the fumes of chemicals like concentrated acids and bases.

5. Closed shoes are required to serve as protection for any possible chemicals spills
or broken glasswares.

6. To avoid interference as you perform the experiment. loose clothing and long hair
should be properly secured.

7. Remove all clutter like bags, books and other material from the working table.
Place your belongings in an area where it will not block the movement of the
students.

3
8. In every experiment, the class should open the windows to provide adequate
ventilation.

9. Smoking is strictly prohibited in the laboratory since some reagents are

Jlammable. Flammable chemicals such as organic solvents and volatile reagents
must be handled under the fume hood.

10. Do not sniff chemicals directly. Just fan the vapors or fumes toward your nose.

11. Do not conduct or proceed with the experiment if the procedure is not clear. Ask
your instructor for further clariJication about the procedure.

12. Using a cellphone or similar gadget during the experiment is prohibited.

13. Do not shout, scream, talk loudly or discuss things not related to the experiment.

14. Do not bring the reagent bottles to your table. There will be a designated area in
the classroom for the reagents.

15. Do not contaminate the reagents. Each reagent bottle has its own dropper. Do not
use the same dropper from one reagent to another. If you are going to use your
own dropper, make sure that it is clean and dry.

16. Do not use your hands in retrieving solid chemicals. Use a spatula to scoop the
chemicals. At all times, do not allow the chemicals to get in contact with any part of
your body.

17. Always make it a habit to label your glass wares containing the chemicals.

18. Always keep your working area neat and clean. Clean your working area at the end
of the experiment.

19. Do not perform unauthorized experiments or any procedures that are not in your
manual or instructed by your teachers.

20. Do not leave any on-going set-up unattended especially if you are using bunsen
burners or hotplates.

21. When using an instrument, read the manual for instructions. Ask instructions or
guidelines from your instructor on how to operate the instrument or machine.

22. Return all borrowed glasswares and apparatus to the monitors and report any
breakage or damage present.

23. Dispose all solid wastes like Jilter paper, burned matches and cottons in the trash
bins.

4
24. Dispose organic wastes and inorganic wastes in their respective waste glass
jars/containers. Read the manual for any related instructions on waste disposal.

25. For data recording and calculations, make sure to present your values in proper
signiJicant Jigures unless otherwise speciJied by the laboratory instructor.

26. Do not use any correction pen/ tape for data changes, rather just simply cross out
with a single line, countersign and record the new data.

27. Always maintain your lockers and work area clean. Take note that lockers are for
laboratory glasswares and materials that you will use for the semester. You may
also leave your labgowns and goggles in here but never use it for your other
personal things.

28. Be mindful of your time, as much as possible, Jinish all assigned tasks at least thirty
(30) minutes before the end of the period so that you will have enough time to
clean your glasswares and work area as well as to Jinalize your data sheets for
checking.

29. In relation to Jire safety:

a. Laboratory rooms or nearby areas must be equipped with Jire extinguisher.
b. For small container Jires, extinguish it by inverting a small beaker or any
applicable glasswares over the burning container. You may also cover the burning
set-up with soaking wet towels. Do not use dry towels.
c. Remove Jlammable reagents from the area of the Jire.
d. If in case, a person inhaled toxic fumes or smoke, transfer him/her to a well-
ventilated space.
e. Use safety shower in case your clothing is caught on Jire.

30. Monitors are assigned each experiment and here are the duties that you need to
take note of:
a. Borrow the necessary glasswares/ apparatus and reagents needed for the
experiment.
b. Arrange the reagents in the designated area, ensure that each chemical will have
its assigned dropper (for solutions & liquids) and spatula (for solids)
c. Distribute all Jloating glasswares/apparatus.
d. Ensure that reagents are sufJicient otherwise request for reJill the main
laboratory/ preparation room.
e. If needed, perform any additional task/s assigned by the instructor.
f. At the end of the laboratory period, remember to:
- return all borrowed glasswares/ apparatus and reagents to the main laboratory
- electrical equipments are turned off and unplugged
- droppers/ spatulas and glasswares are complete and cleaned
- water and gas outlets are closed
- iron stands are in the designated area
- tabletops and sinks are all clean and dry
- lockers are all secured

5
MATERIALS NEEDED IN THE ANALYTICAL LABORATORY

Laboratory gown
Safety glass/goggles
Rubber gloves
Facemasks
Rags
Tissue paper
Permanent marker
Masking tape or labeling tape
Liquid detergent
Soap
Glass droppers
Scissors/ Cutter
Stapler
Kitchen Lighter/ Matches
First aid kit
Test tube Brush
Sponge

6
Name_________________________________________________________Date Performed__________________
Section & Group Number___________________________________Date Submitted___________________

1
Experiment No.____
Preparation & Standardization of 0.100 M NaOH & HCl solutions

Standardization is a method in determining the actual concentration of a solution. One

type of analytical procedure frequently used in standardization is titration. In titration, an
analyte is determined based on its stoichiometric reaction with a reagent of known
concentration. The reagent is added gradually in portions until the analyte is consumed
quantitatively. In a titration, the point at which the reaction is complete is referred to as
the endpoint. An appropriate indicator is used to signal the endpoint of the reaction. The
indicator to be used in this experiment is phenolphthalein. This indicator is colorless in an
acidic solution but displays a pink color in a basic solution.

This experiment involves two separate acid and base standardization procedures. In the
Jirst procedure, the concentration (in Molarity) of the NaOH solution will be standardized
by titrating with samples of a primary standard acidic substance called, Potassium
Hydrogen Phthalate (KHP). KHP has a chemical formula of C8H5KO4 and a molar mass of
204.2 grams/mole. It has one acidic hydrogen atom, which reacts with the NaOH on a 1:1
stoichiometric relationship.

C8H5KO4 + NaOH → NaC8H4KO4 + H2O

In the second procedure, the standardized NaOH solution will be used to standardize the
concentration (in Molarity) of the HCl solution. The HCl is the analyte while the
standardized NaOH is the titrant or reagent of known concentration. Phenolphthalein is
also the appropriate indicator for this titration.

OBJECTIVES
1) To prepare 0.100 M Sodium Hydroxide (NaOH) and 0.100 M Hydrochloric acid
(HCl) solutions.
2) To standardize the prepared solutions by titration.

APPARATUS
(1) Base burette, (1) Iron stand, (1) burette clamp, (1) glass funnel, (1) 100 mL graduated
cylinder, (1) stirring rod, (1) 10 mL pipette, (3) 250 mL Erlenmeyer Jlasks, (1) watch
glass, (1) plastic/porcelain spatula, (1) wash bottle, (2) 500 mL Volumetric Jlasks with
plastic cover/stopper, (1) rubber aspirator, (1) 1L beaker, (1) thermometer, (1) 25 ml
beaker, & (1) test tube brush.

REAGENTS/MATERIALS
Sodium Hydroxide pellets (AR) Potassium Hydrogen Phthalate (KHP)
Concentrated HCl (12 M) Phenolphthalein Indicator
Distilled water

7
PROCEDURES
I. Preparation of Standard Solutions
A. Preparation of 0.100 M NaOH solution
1. Assemble a heating set-up and boil about 600 mL of distilled water in a
1 L beaker. Cool the boiled distilled water until it reaches the
temperature of 25 °C.
2. Weigh accurately 2.00 grams of NaOH pellets in a 50 mL beaker by
using an analytical balance. Record the data.
3. Dissolve the NaOH pellets with a small amount of pre-boiled distilled
water. Stir the solution and transfer the mixture into a 500 mL
volumetric Jlask.
4. Rinse the beaker with a small amount of pre-boiled distilled water and
transfer the residual NaOH solution into the 500 mL volumetric Jlask.
Repeat the process for about two times to ensure that all of the NaOH
solution is completely transferred.
5. Fill the 500 mL volumetric Jlask with the pre-boiled distilled water up
to the mark of the glassware. Cover the Jlask with a plastic stopper and
mix well the solution.
6. Transfer the NaOH solution to a polyethylene (PET) container. Label
the container.

B. Preparation of 0.100 M HCl solution

1. Half Jill a clean 500 mL volumetric Jlask with distilled water.
2. Using a 10 mL volumetric pipette, carefully transfer a 4.17 mL of
concentrated HCl (12.0 M) into the 500 mL volumetric Jlask.
3. Dilute the solution up to the mark of the Jlask. Cover the Jlask with a
plastic stopper and mix well the solution. Transfer and label the HCl
solution to a reagent bottle.

II. Standardization of the solutions

A. Standardization of the 0.100 M NaOH solution
1. Transfer about 1.00-2.00 grams of Potassium Hydrogen Phthalate
(KHP) [C8H5KO4] in a 25 mL beaker. Oven dry the KHP for about 2 hours
at 120°C. Cool the KHP. Skip this part if your lab instructor has already
prepared the KHP prior to the standardization experiment.

2. Weigh 0.100 grams of KHP accurately into each of the 3 Erlenmeyer

Jlasks in an analytical balance. Record the weights in 3 signiJicant
Jigures.
3. To each Jlask, transfer 50 mL of distilled water using a 100 ml graduated
cylinder.
4. Swirl the Jlask until the KHP is dissolved.
5. Afterwards, add about 2 drops of phenolphthalein indicator.
6. Prepare the base burette by rinsing it twice with a small amount of
0.100 M NaOH solution. Remove the solution and transfer it to the
waste bottle.

8
 7. Fill the base burette with the NaOH solution up to the zero mark (Initial
volume). Make sure that the burette does not contain air bubbles.
8. Titrate the KHP solution in the Jirst Jlask with the 0.100 M NaOH
solution (titrant) to the Jirst permanent faint pink color. Record the
Jinal volume.
9. The volume of NaOH used is the difference between its Jinal and initial
volume (VJinal – Vinitial).
10. Repeat the titration with the other two samples. Record the data in
proper signiJicant Jigures.
11. Calculate the molarity (M) of the three samples/trials. Get the average
molarity of the NaOH solution. Always remember to record calculated
data in proper signiJicant Jigures.

B. Standardization of the HCl solution

1. Pipette 10.0 mL of the HCl solution and transfer the solution into a 125
mL clean Erlenmeyer Jlask.
2. Add about 2 drops of phenolphthalein indicator into the solution.
3. Fill the base burette with NaOH solution up to the zero mark. (Initial
volume).
4. Titrate the HCl solution with the titrant (NaOH solution) until a
permanent faint pink color persists. Record the Jinal volume.
5. Determine the NaOH volume used.
6. Perform or make three trials and record all data proper signiJicant
Jigures.
7. Calculate the molarity of the three samples/trials. Get the average
molarity of the HCl solution.

9
 1
Experiment No.____
Preparation & Standardization of 0.100 M NaOH & HCl solutions

Name:_____________________________________ Instructor’s Signature___________

Group number:___________________________ Date Performed:_________________
Section:___________________________________ Score:_____________________________

DATA AND RESULTS

Part 1. Standardization of NaOH solution

TRIAL 1 TRIAL 2 TRIAL 3

Weight of KHP in grams
Initial volume of NaOH in mL (Vi)
Final volume of NaOH in mL (Vf)
Volume of NaOH used (Vf - Vi)
Molarity of NaOH
Average Molarity

Calculations

Part 2. Standardization of HCl solution

TRIAL 1 TRIAL 2 TRIAL 3

Volume of HCl used
Initial volume of NaOH in mL (Vi)
Final volume of NaOH in mL (Vf)
Volume of NaOH used (Vf - Vi)
Molarity of HCl
Average Molarity

Calculations:

10
QUESTIONS

1. Why is it essential to boil the water in preparing a 0.1M NaOH solution?

2. Cite the other primary standards available for NaOH and HCl.
3. Why is it preferable to titrate HCl with a standardized NaOH solution rather than
the other way around (NaOH with HCl)?
4. DeJine brieJly the following terms:
(a) Concentration
(b) Standardization
(c) Standard Solution
(d) Indicator
(e) Back titration
(f) Over titration
(g) Secondary standard solution.
5. Why is it essential to store the standardized NaOH solution in a polyethylene
terephthalate (PET) bottle?
6. In a Jlow diagram, show you are to prepare the following solutions:
Show the necessary calculations needed.
a. 1M NaCl (from solid NaCl)
b. 0.1 M NaCl (from 1M NaCl solution)

11
Name_________________________________________________________Date Performed__________________
Section & Group Number___________________________________Date Submitted___________________

2
Experiment No.____
Chemical Kinetics:
Effect of Concentration and Temperature on Rate of Reaction

On the basis of experiments you've performed, you probably have already noticed that
reactions occur at varying speeds. There is an entire spectrum of reaction speeds,
ranging from very slow to extremely fast. For example, the rusting of iron is reasonably
slow, whereas the decomposition of TNT is extremely fast. The branch of chemistry that
is concerned with the rates of reactions is called chemical kinetics.

Experiments show that rates of reactions in solution depend upon:

1. The nature of the reactants
2. The concentration of the reactants
3. The temperature
4. Catalysis.

Before a reaction can occur, the reactants must come into direct contact via collisions of
the reacting particles. However, even then, the reacting particles (ions or molecules) must
collide with sufJicient energy to result in a reaction; if they do not, their collisions are
ineffective and analogous to collisions of billiard balls. With these considerations in mind,
we can quantitatively explain how the various factors inJluence the rates of reactions.

Concentration:
Changing the concentration of a solute in solution alters the number of particles per unit
volume. The more particles present in a given volume, the greater the probability of them
colliding. Hence, increasing the concentration of a solute in solution increases the number
of collisions per unit time and therefore, increases the rate of reaction.

Temperature:
Since temperature is a measure of the average kinetic energy of a substance, an increase
in temperature increases the kinetic energy of the reactant particles. The results in an
increase in the velocity of the particles and therefore, increases the number of collisions
between them in a given period of time. Thus, the rate of reaction increases. Also, an
increase in kinetic energy results in a greater proportion of the collisions having the
required energy for reaction.

Catalyst:
Catalysts, in some cases, are believed to increase reaction rates by bringing particles into
close just a position in the correct geometrical arrangement for reaction to occur. In other
instances, catalysts offer an alternative route to the reaction, one that requires less
energetic collisions between reactant particles. If less energy is required for a successful
collision, a larger percentage of the collisions will have the required energy, and the
reaction will occur faster. Actually, the catalyst may take an active part in the reaction, but
at the end of the reaction, the catalyst can be recovered chemically unchanged.

12
Order of Reaction De\ined
Consider the hypothetical reaction:
A+B→C+D [1]
The rate of reaction is measured by observing the rate of disappearance of the reactants A
or B, or the rate of appearance of the products C or D. The species observed is a matter of
convenience. For example if A, B, and D are colorless and C is colored, you could
conveniently measure the rate of appearance of C by observing an increase in the
intensity of the color of the solution as a function of time. Mathematically, the rate of
reaction may be expressed as follows:

Rate of disappearance of A = −change in the concentration of A time required for change

=−Δ[A] /Δt

Rate of appearance of C= change in the concentration of C time required for change

=Δ[C]/ Δt

In general, the rate of the reaction depends upon the concentration of one or more of
the reactants. Thus, the rate of the reaction above is expressed as

Rate = k[A]x [B]y [2]

where [A] and [B] are the molar concentrations of A and B, x and y are the powers to
which the respective concentrations must be raised, and k is the rate constant. The
values of x and y must be determined experimentally. For example, if x = 2 and y = 1,
then the rate law is:

Rate = k[A]2 [B] [3]

This reaction is Jirst order in B, meaning that doubling the concentration of B while
keeping A constant causes the reaction rate to double. Simultaneously, this reaction is
second order in A, meaning that doubling the concentration of A while keeping B constant
causes the rate to increase by a factor of four, since the rate of the reaction is proportional
to the square of the concentration of A. The overall order of the reaction is the sum of the
exponents: or third order in this case. The orders are determined experimentally by
noting the effects of changing reagent concentrations on the rate of the reaction. The rate
constant, k, is independent of the concentration. The rate constant is characteristic for a
given reaction and varies only with temperature. Once the rate is known for a given set of
concentrations, the value of k can be calculated.

Reaction of Sodium thiosulfate and Hydrochloric acid

In this experiment you will measure the rate of the reaction between a sodium
thiosulfate solution and hydrochloric acid:

2HCl(aq) + Na2S2O3(aq) → 2NaCl(aq) + SO2(aq) + S(s)↓ + H2O (l)

The precipitate of sulfur formed gradually and makes the solution cloudy. The formation
of cloudy mask a cross marked on paper. The rate of reaction, and consequently the time

13
taken to obscure the cross, depends on a number of variables such as temperature,
concentration and volume. The rate of reaction can be measured by timing how long it
takes for the solution to become cloudy and the precipitation of sulfur. In other words the
time taken for a certain quantity of sulphur to form and cause the ‘X’ mark to disappear is
used to determine the rate of reaction. The rate of this reaction directly proportional with
the inverse of the time taken for a formation of precipitation of sulfur.

OBJECTIVES
To observe the effect of concentration and temperature upon the rate of the reaction of
sodium thiosulfate with hydrochloric acid.

SAFETY PRECAUTIONS

1. Wear your eye protection.

2. Do not inhale any fumes.
3. Sulfur dioxide is toxic and corrosive. Dispose of the solution immediately after the
experiment following your teacher's instructions.
4. Wash your hands when Jinished.

APPARATUS
(1) Iron stand, (1) burette clamp, (1) glass funnel, (1) 100 mL graduated cylinder, (1)
stirring rod, (1) 10 mL pipette, (3) 250 mL Erlenmeyer Jlasks, (1) watch glass, (1)
plastic/porcelain spatula, (1) wash bottle, (1) thermometer (1) white paper (1) 25 ml
beaker, & (1) test tube brush.

REAGENTS/MATERIALS
0.10 0M Sodium Thiosulfate Solution
0.050 M Sodium Thiosulfate Solution
1.00 M Hydrochloric Acid
Distilled water

PROCEDURES
I. Effect of concentration
1. Using a pencil, draw a cross in the middle of the Jilter paper.
2. Place 20 mL of the 0. 100 M sodium thiosulfate solution into a conical Jlask.
3. Add 20 mL of 1 M hydrochloric acid to the Jlask, while starting the stop clock at the same
time.
4. Swirl the Jlask and place it on a paper marked with a cross.
5. Record the time taken for the cross to disappear.
6. Repeat the experiment using 10,12, 14, 16 and 18 mL of sodium thiosulfate solution
respectively. In each case, add water to make the volume up to 20 mL and mix before
adding HCl.
7. Record the results in data sheet.

14
II. Effect of temperature
1 . Place 20 mL of 0.050 M sodium thiosulfate solution into a conical Jlask.
2. Warm or cool the Jlask gently until the temperature is about 20 0C.
3. Add 20.0 mL of 1.00 M HCl, starting a stop clock at the same time, before
proceeding.
4. Without delay, swirl the Jlask, place it on a paper marked with a cross, and record
the exact temperature of the contents of the Jlask.
5. Record the time taken for the cross to disappear.
6. Repeat the experiment, heating or cooling the thiosulfate solution to temperatures
of approximately 100C, 300C, 400C, 500C and 600C respectively (before adding the HCl).
7. Record the results in data sheet.

15
 2
Experiment No.____
Chemical Kinetics:
Effect of Concentration and Temperature on Rate of Reaction

Name:_____________________________________ Instructor’s Signature___________

Group number:___________________________ Date Performed:_________________
Section:___________________________________ Score:_____________________________

DATA AND RESULTS

Part 1. Effect of Concentration

Volume of Volume Volume of Conc. of Reaction 1/ Time

1.00M HCl of . H2O (mL) Na2S2O3 (M) Time (s) (s-1)
(mL) 0.100M
Na2S2O3
(mL)
1
2
3
4
5
6

Using MS Excel, draw a graph of 1/time against concentration of thiosulfate solution and
reaction time and concentration of thiosulfate solution using excel. Write your comments
about the graph. (Hint: 1/time for this reaction is the measure of reaction rate.)

Calculations:

16
Part 2. Effect of Temperature

Volume of Volume of . Temperature (oC) Reaction 1/ Time

1.00M HCl 0.050M Na2S2O3 Time (s) (s-1)
(mL) (mL)
1
2
3
4
5
6

Using MS Excel, draw a graph of 1/time against temperature and reaction time against
temperature using excel and write your comments about the graph. (Hint: 1/time for this reaction
is the measure of reaction rate.)

Calculations:

QUESTIONS

1. What is the meaning of directly proportionality of two quantities ?

2. What is the effect of increasing the concentration on the reaction time and reaction
rate?
3. What is the effect of raising the temperature on the reaction time?
4. What is the effect of raising the temperature on the reaction rate? Suggest two factors
responsible for the result observed.
5. Suggest a reason why it is not recommended to carry out the experiment at
temperatures higher than about 60 0C.
6. Which is the limiting reactant in the temperature experiment.

17
Name_________________________________________________________Date Performed__________________
Section & Group Number___________________________________Date Submitted___________________

3
Experiment No.____
Chemical Equilibrium and Le Chatelier’s Principle

There are certain reactions that does not Jinish completely, or in some cases not all
reagents are consumed. In some chemical reactions, there are always some products and
some reactants left over. Considering these chemical systems,two competing reactions
are happening: one is the forward reaction and the other is the reverse reaction of that
system. Both the forward and backward reactions are happening at the same time. When
the speed of the forward reaction matches the speed of the reverse reaction, the system is
balanced. The amounts of the products and reactants stay the same. That doesn't mean
the system stays the same. Both reactions are happening at the same speed, therefore, the
amounts of the starting reagents and the results stay the same. When writing an equation
for a reaction that is balanced, you use a double arrow(↔) or two arrows pointing in
opposite directions. These representation show that both the forward and backward
reactions are happening at the same time.

Equilibrium is dynamic. When a system is balanced, a reaction still takes place. When two
opposing forces are happening at the same rate, a balanced system doesn’t show any
visible signs of change. But this balance can change if stress is added.

Le Chatelier's principle, also referred to as the equilibrium law help predict how changes
like temperature,concentrations of reactants/products, volume, pressure or presence of
catalyst will affect a system that is in balance.The idea is named after a French chemist
called Henry Louis Le Chatelier.

In this experiment, you will analyze two equilibrium systems. The reaction for the Jirst
system is shown below and produces one colored complex ion.

Fe3+ (aq) + 6 SCN-(aq) ⇄ [Fe(SCN)6]3-(aq)

The [Fe(SCN)6]3- complex ion creates s bloody red solution. We can add stress to the
equilibrium which will cause the solution to change color. We can visually observe this or
measure the absorbance using a spectrophotometer.

The reaction for the second system is shown below and has two colored complex ions.

[CoCl4]-2(alc) + 6 H2O(l) ⇄ [Co(H2O)6]2+ (alc) + 4 Cl-(alc)

For this reaction, the [CoCl4]2- ion produces a bright blue color, while the [Co(H2O)6]2+ ion
is a pink colored solution. By observing how the color changes or even by checking the
absorbance when stress is applied, we can see how the system is affected.

OBJECTIVE:
To examine equilibrium systems and the effects of stresses placed on those systems.

18
SAFETY PRECAUTIONS

1. Wear your eye protection.

5
2. Wash your hands when Jinished.

APPARATUS
(2) 100 mL graduated cylinder, (1) stirring rod, (1) 10 mL pipette/ droppers, (3) 250 mL
Erlenmeyer Jlasks, (1) plastic/porcelain spatula, (1) wash bottle, (1) thermometer (1)
white paper (2) 250 ml beaker, & (1) test tube brush.

REAGENTS/MATERIALS
0.002 M Potassium Thiocyanate solution
0.20 M Potassium Thiocyanate solution
0.20 M Ferric nitrate solution
0.10 M Silver nitrate solution
0.010 M Tetrachlorocobalt ion solution
12 M Hydrochloric Acid
Sodium Jluoride solids
Sodium hydrogen phosphate solids
Deionized water
Distilled water
Ethanol
Ice

PROCEDURES
I. Fe(NO3)3 + KSCN Equilibrium

1. In 250 mL beaker, mix 50 mL of 0.002 M KSCN and 4 drops of 0.20 M Fe(NO3)3. Observe
the color of the solution. This is your Jirst equilibrium solution.

2. Prepare 8 clean and dry test tubes. Add 5 mL of the equilibrium solution to each test
tube and label them 1-8. The Jirst test tube is your control or reference test tube.

3. Treat each solution as follows:

Test Tube Treatment
1 As is (Control Solution)
2 Add 1mL 0.20M KSCN
3 Add 1mL 0.20M Fe(NO3)3
4 Add pinch of NaF solids
5 Add 1mL distilled water + pinch of Na2HPO4
6 Add 1 mL 0.10M AgNO3
7 Hot water bath (5 minutes)
8 Ice water bath (5 minutes)

19
3. Compare each of the treated solutions with respect to the control solution. Indicate if
the treated solution is lighter, darker or same as the reference.

4. If UV-VIS Spectrophotometer is available, measure the absorbance of all the solutions at

475 nm. [Cuvette control solution contains deionized water]

II. [CoCl4]2-(alc)/ [Co(H2O)6]2+ (alc) Equilibrium

1. In a clean and dry 250 mL beaker, mix 40 mL of 0.01 M [CoCl4]-2 and 30 drops of
deionized water. Observe the color of the solution. This is your second equilibrium
solution.

2. Prepare 6 clean and dry test tubes. Add 5 mL of the equilibrium solution to each test
tube and label them 1-6. The Jirst test tube is your control or reference test tube.

3. Treat each solution as follows:

Test Tube Treatment
1 As is (Control Solution)
2 Add 1 drop 12M HCl
3 Add 1mL deionized water
4 Add 1 mL 0.10M AgNO3
5 Hot water bath (5 minutes)
6 Ice water bath (5 minutes)

3. Compare each of the treated solutions with respect to the control solution. Indicate if
the treated solution is lighter, darker or same as the reference.

4. If UV-VIS Spectrophotometer is available, measure the absorbance of all the solutions at

655 nm. [Cuvette control solution contains ethanol]

20
 3
Experiment No.____
Chemical Equilibrium and Le Chatelier’s Principle

Name:_____________________________________ Instructor’s Signature___________

Group number:___________________________ Date Performed:_________________
Section:___________________________________ Score:_____________________________

DATA AND RESULTS

Part 1. Fe(NO3)3 + KSCN Equilibrium

Test Treatment Color Observation Equilibrium Shift *Absorbance

Tube (forward, backward or @ 475 nm
no shift)
1
2
3
4
5
6
7
8

Part 2. [CoCl4]2-(alc)/ [Co(H2O)6]2+ (alc) Equilibrium

Test Treatment Color Observation Equilibrium Shift *Absorbance

Tube (forward, backward or @ 655 nm
no shift)
1
2
3
4
5
6

* Disregard if UV-VIS Spectrophotometer is not available

QUESTIONS

1. Explain how each change affected the equilibrium in terms of Le Châtelier’s

principle.
2. Consider the equilibrium systems in the experiment, is the forward reaction
endothermic or exothermic?
3. What are the factors that affect equilibrium?

21
Name_________________________________________________________Date Performed__________________
Section & Group Number___________________________________Date Submitted___________________

4
Experiment No.____
Determination of the Ionization Constant of a Weak Acid and Weak Base

The Swedish chemist Arrhenius said that solutions that can conduct electricity are
referred as electrolytes, they are able to ionize into charged particles. These compound
are commonly, acids, bases and salts. Furthermore they can be classiJied as strong
electrolytes or weak electrolytes. Strong electrolytes dissociate almost completely into
ions when mixed with water (aqueous system). Weak electrolytes only dissociate a small
amount, with 10% or less of the substance turning into ions in the solution.

Acids are substances that ionizes to give off hydrogen ions (H+) while bases are
substances that accept hydrogen ions.

The equation for the ionization of a weak acid may be expressed as:
HA ↔ H+ + A-

This indicates that protons (H+) is present freely in solution. In reality, protons mix with
water molecules when they are in a solution. Since water s the most common solvent, the
way a weak acid (or base) dissociate into ions is better shown by:
his equation:
HA + H2O ↔ H3O+ + A-

The dissociation of weak electrolytes can happen in both directions. When cations and
anions meet in the solution, they can come together again to produce a molecule. Just
like in any process that can proceed reversibly, equilibrium is achieved as well.

Quantitatively it can be characterized by the equilibrium constant, called dissociation

constant Ka, which for dilute solutions of the weak acid is expressed by the formula.

Ka = [H3O+] [A-]
[HA]

where:
[H+] = concentration of H+ ions
[A-] = concentration of anions
[HA] = concentration of unionized acid

The bracket notation indicates that molar concentration of ionized and non-ionized
species present in solution at equilibrium.

OBJECTIVE:
To determine the ionization constant of a weak acid or weak base

22
APPARATUS
(4) 100 mL volumetric Jlask, (2) 50 mL graduated cylinder, (1) stirring rod, (1) 10 mL
pipette/ droppers, (3) 250 mL Erlenmeyer Jlasks, (1) plastic/porcelain spatula, (1) wash
bottle, (1) pH meter/ pH pen (1) white paper (2) 250 ml beaker, & (1) test tube brush.

REAGENTS/MATERIALS
1.00 M Acetic acid solution
1.00 M Ammonia solution
Distilled water

PROCEDURES

1. Prepare the following stock solutions for the class:

(a) 100. mL of 1.00 M CH3COOH
(b) 100. mL of 1.00 M NH3

2. Each group must prepare 0.100M and 0.150 M concentrations of CH3COOH and NH3
using 100 mL volumetric Jlask. Apply knowledge on dilution calculations and solution
preparation.

3. Using a calibrated pH meter/ pH pen, measure the pH of the solutions.

4. Using the measured pH, calculate for the ionization constant of the weak acid and
weak base.

23
 4
Experiment No.____
Determination of the Ionization Constant of a Weak Acid and Weak Base

Name:_____________________________________ Instructor’s Signature___________

Group number:___________________________ Date Performed:_________________
Section:___________________________________ Score:_____________________________

DATA AND RESULTS

Part 1. CH3COOH

[CH3COOH] 0.100 M 0.150 M

pH
[H+]
[CH3COO-]
Experimental Ka
Theoretical Ka
% Error Ka

0.10 M CH3COOH
CH3COOH ↔ H+ CH3COO-
Initial
Concentration
Upon Ionization
(change)
Equilibrium
Concentration

0.15 M CH3COOH
CH3COOH ↔ H+ CH3COO-
Initial
Concentration
Upon Ionization
(change)
Equilibrium
Concentration

Ka = [CH3COO-] [H+]
[CH3COOH]

CALCULATIONS:

24
Part 2. NH3
[NH3] 0.100 M 0.150 M
pH
pOH
[OH-]
[NH4+]
Experimental Kb
Theoretical Kb
% Error Kb
0.10 M NH3
NH3 + H2O ↔ NH4+ OH-
Initial
Concentration
Upon
Ionization
(change)
Equilibrium
Concentration

0.15 M NH3
NH3 + H2O ↔ NH4+ OH-
Initial
Concentration
Upon
Ionization
(change)
Equilibrium
Concentration

Kb = [OH-] [NH4+]
[NH3]

CALCULATIONS:

QUESTIONS:
1. Compare the test solutions in terms of pH and degree of ionization.
2. How does dilution affect: (a) pH (b)degree of ionization (c) Ka or Kb
3. If Ka of the substance is 1.75 x 10-5 what is the value of Kb? What is the value for pKa
and pKb?

25
Name_________________________________________________________Date Performed__________________
Section & Group Number___________________________________Date Submitted___________________

5
Experiment No.____
Determination of Acidity in Vinegar and Fruit Juice

Vinegar is a solution, which contains about 4-5% acetic acid (C2H4O2 or HAc) in water. It
also contains some fruit acids, coloring matter, salts and a little amount of other
fermentation products, which impart a Jlavor and aroma to the vinegar. It is produced by
a two-step bioprocess. In the Jirst step, the fermentable sugars are transformed into
ethanol or ethyl alcohol by yeasts. This process is called as alcoholic fermentation.

C6H12O6 (Glucose) + yeast → 2C2H5OH (Ethanol) (Anaerobic process)

In the second step, the acetic acid bacteria (AAB) will oxidize the ethyl alcohol into acetic
acid in an aerobic manner. This process is called as acetiJication, which is the key step in
making a vinegar.

C2H5OH (Ethanol) + O2 → CH3COOH (Acetic acid) + H2O (Aerobic process)

One of the objectives of this experiment is to measure the total acid concentration in
terms of % acetic acid in a commercial brand of vinegar. Acetic acid is the main acid in the
vinegar. It is a weak organic acid and has a molar mass of 60g/mole. This weak acid has
one acidic Hydrogen, which then reacts with the NaOH solution.

CH3COOH (Acetic acid) + NaOH → NaCH3COO + H2O (Balanced equation)

The % acetic acid will also be compared to the total acetic acid concentration declared by
the commercial vinegar. According to the Philippine Department of Health (DOH), all
vinegar shall have an acidity of not less than 4% by weight of absolute acetic acid.
Therefore, it is also important to know if the commercial vinegar meets the minimum
requirement for acetic acid concentration.

The standardized 0.1M NaOH solution prepared from the previous experiment will be
used to determine the acidity of the commercial vinegar, fruit juice, and unknown
solution. The determination of the acidity will be done through titration. It is a common
analytical technique used to measure or determine the amount of a certain compound in a
solution. In this experiment, Phenolphthalein is also the appropriate indicator for
titration.

On the other hand, the sour taste of the citrus fruits is due the presence of an acid called
Citric acid. This acid has a molecular formula of C6H8O7 or C3H5O(COOH)3 and a molar
mass of 192. 12 g/mole. It has three acidic hydrogens coming from the three carboxylic
groups present in the acid, which then react with the NaOH solution.

C3H5O(COOH)3 + 3 NaOH → C3H5O(COONa)3 + 3 H2O (Balanced equation)

26
The total citric acid concentration from the citrus juice can be determined by using the
stoichiometric relationship as stated above.

OBJECTIVES
1) To determine the acidity of the commercial vinegar & fruit juice samples using the
titration method.
2) To determine whether the commercial vinegar meets the minimum concentration
set by the Department of Health.
3) To determine the acidity of the unknown solution by titration method.

APPARATUS
(1) Base burette, (1) Iron stand, (1) burette clamp, (1) glass funnel, (1) 50 mL graduated
cylinder, (1) stirring rod, (2) 5 mL pipettes, (3) 250 mL Erlenmeyer Jlasks, (2) rubber
aspirators, (1) test tube brush, (2) 250 ml beakers, & (1) glass dropper.

REAGENTS/MATERIALS
Standardized 0.100 M NaOH Phenolphthalein indicator
Commercial vinegar (10pcs/group) of calamansi or 1 pc. Orange fruit
Distilled water Unknown soln. (to be determined by the instructor)

PROCEDURES

I. Acetic Acid Content in Commercial Vinegar

1. Use a 5 mL volumetric pipette and deliver 2.00 mL of commercial vinegar

into a 250 mL Erlenmeyer Jlask.
2. Add 20.0 mL of distilled water to the Jlask using a graduated cylinder.
3. Afterwards, add about 3 drops of phenolphthalein indicator to the sample
solution.
4. Assemble a titration set-up.
5. Rinse the base burette twice with a small amount of NaOH solution.
Remove the solution and transfer it to the waste container.
6. Fill the base burette with the 0.100 M NaOH solution up to the zero mark
(Initial volume). Make sure that the burette does not contain air bubbles.
7. Titrate the sample solution with the 0.1M NaOH solution with constant
swirling of the Jlask until a permanent light pink color persists.
8. Record the Jinal volume of the NaOH solution.
9. The volume of NaOH used in the titration is the difference between its Jinal
and initial volume. Record the data.
10. Calculate the mg of acetic acid in the sample solution.
11. Calculate the % acetic acid (in terms of % g/mL) in the sample solution.
12. Make triplicate samples/trials.
13. Get the average % acetic acid for the three trials.

27
II. Citric Acid Content in Fruit Juice

1. Use a 5 mL volumetric pipette and deliver 3.00 mL of pure fruit juice into a
250 mL Erlenmeyer Jlask.
2. Add 20.0 mL of distilled water to the Jlask using a graduated cylinder.
3. Afterwards, add about 3 drops of phenolphthalein indicator to the sample
solution.
4. Fill the base burette with the 0.100 M NaOH solution up to the zero mark
(Initial volume).
5. Titrate the sample solution with the 0.100 M NaOH solution with constant
swirling of the Jlask until a permanent light pink color persists.
6. Record the Jinal volume of the NaOH solution.
7. The volume of NaOH used in the titration is the difference between its Jinal
and initial volume. Record the data.
8. Calculate the g of citric acid in the sample solution.
9. Calculate the % citric acid (in terms of % g/mL) in the sample solution.
10. Make triplicate samples/trials.
Get the average % acetic acid for the three trials.

III. Determination of the % acidity of the unknown solution

1. Pipet about 5.00 mL of the acid solution (to be obtained from your
instructor) into a 250 mL Erlenmeyer Jlask.
2. Add about 20.0 mL of distilled water to the Jlask using a 50 mL graduated
cylinder.
3. Afterwards, add 3 drops of the phenolphthalein indicator to the acid
solution. Swirl the mixture.
4. Fill the base burette with the 0.100 M NaOH solution up to the zero mark
(Initial volume).
5. Titrate the acid solution with 0.100 M standardized NaOH solution with
constant swirling of the Jlask until a permanent light pink color persists.
6. Record the Jinal volume of the NaOH solution.
7. Determine the volume of NaOH used during the titration.
8. Perform three trials.
9. Calculate the g of the acid, % g/mL of the acid solution and the average %
acidity of the three trials.

28
 5
Experiment No.____
Determination of Acidity in Vinegar and Fruit Juice

Name:_____________________________________ Instructor’s Signature___________

Group number:___________________________ Date Performed:_________________
Section:___________________________________ Score:_____________________________

DATA AND RESULTS

Part 1. Acidity content in Commercial Vinegar

Trial 1 Trial 2 Trial 3
Brand/ Type of Vinegar
Commercial value of %acetic acid
(see product label)
Volume of vinegar (mL)
Concentration of NaOH (M)
Initial volume of NaOH (mL)
Final volume of NaOH (mL)
Volume of NaOH used (mL)
Acetic acid in grams
% Acetic acid in % g/mL
Average % Acetic acid

Calculations:

Part 2. Acidity content in Fruit Juice

Trial 1 Trial 2 Trial 3
Fruit used
Volume of the fruit juice (mL)
Concentration of NaOH (M)
Initial volume of NaOH (mL)
Final volume of NaOH (mL)
Volume of NaOH used (mL)
Citric acid in grams
% Citric acid in % g/mL
Average % Citric acid

Calculations:

29
Part 3. Determination of the % acidity of an unknown solution

Trial 1 Trial 2 Trial 3

Acid Solution
Volume of the acid solution (mL)
Concentration of NaOH (M)
Initial volume of NaOH (mL)
Final volume of NaOH (mL)
Volume of NaOH used (mL)
Acid in grams
% Acid in % g/mL
Average % acid

Calculations:

QUESTIONS

1. Cite at least three (3) different uses of vinegar.

2. Does vinegar made from synthetic acetic acid have an adverse effect on the
human body?
3. Based on your data, does the commercial vinegar meet the minimum
concentration of acetic acid set by the DOH?

30