Chemistry Lab Manual

Download as pdf or txt
Download as pdf or txt
You are on page 1of 32

School of Biotechnology, International University-HCMC

Department: Applied Chemistry

Laboratory Manual
General Chemistry

LABORATORY MANUAL
FOR
GENERAL CHEMISTRY FOR ENGINEERING
STUDENTS

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

This laboratory is designed for internal use only. Its content is collected and composed by Dr
Hoang Le Son; edited by Dr Huynh Kim Lam for Laboratory Module.
*Some of its contents are extracted from references as indicated.

References:
[1] Experiments in General Chemistry: Inquiry and Skill buildingby ickie Williamson (Author), Larry
Peck, (Brooks/Cole Laboratory Series for General Chemistry), 2008.
[2] Introduction to Chemical Principles: A Laboratory Approach by Susan A. Weiner, Blaine Harrison
(Brooks/Cole Laboratory Series for Introductory Chemistry) 7Edition, 2009.
[3] Laboratory Experiments for General, Organic and Biochemistryby Frederick A. Bettelheim
(Brooks/Cole Laboratory Series for General Chemistry) 7th Edition, 2009.
[4] Experiments in General Chemistry by Bobby Stanton, Lin Zhu, Charles H. Atwood (Featuring
MeasureNet), 2nd Edition, 2009.
[5] Laboratory Manual for Principles of General Chemistry by Jo Allan Beran, 9th Edition, 2010.

Common Laboratory
Glassware and Equipment

buret clamp

beaker

Bunsen burner

crucible tongs

evaporating dish

crucible and lid

funnel

graduated
cylinder

thermometer

clay triangle

Erlenmeyer flask

glass rod with rubber policeman

Bobby Stanton/Wadsworth/Cengage Learning

electronic balance

ix

Common Laboratory Glassware and Equipment

ring stand and iron ring

scoopula

test tube clamp

test tube

watch glass

wire gauze

pipets

volumetric
flask

test tube rack

utility clamp

buret

Bobby Stanton/Wadsworth/Cengage Learning

Practice Safe Laboratory

A few precautions can make the laboratory experience relatively hazard


free and safe. These experiments are on a small scale and thus many of the
dangers found in the chemistry laboratory have been minimized. In
addition to specic regulations that you may have for your laboratory, the
following DO and DONT RULES should be observed at all times.

DO RULES
q Do wear approved safety glasses or goggles at all times.
The rst thing you should do after you enter the laboratory is to put on
your safety eyewear. The last thing you should do before you leave the
laboratory is to remove them. Contact lens wearers must wear
additional safety goggles. Prescription glasses are not suitable safety
glasses; you must wear safety goggles over them.
q Do wear protective clothing.
Wear sensible clothing in the laboratory (i.e., no shorts, no tank tops, no
sandals). Be covered from the neck to the feet. Laboratory coats or
aprons are recommended. Tie back long hair, out of the way of ames.

COPYRIGHT 2010 Brooks/Cole, Cengage Learning

q Do know the location and use of all safety equipment.


This includes eyewash facilities, re extinguishers, re showers, and
re blankets. In case of re, do not panic, clear out of the immediate
area, and call your instructor for help.
q Do use proper techniques and procedures.
Closely follow the instructions given in this laboratory manual. These
experiments have been student tested; however, accidents do occur but
can be avoided if the steps for an experiment are followed. Pay heed to
the Caution! signs in a procedure.
q Do discard waste material properly.
Organic chemical waste should be collected in appropriate waste containers and not ushed down sink drains. Dilute, nontoxic solutions may be
washed down the sink with plenty of water. Insoluble and toxic waste
chemicals should be collected in properly labeled waste containers. Follow
the directions of your instructor for alternative or special procedures.
q Do be alert, serious, and responsible.
The best way you can prepare for an experiment is to read the
procedure carefully and be aware of the hazards before stepping foot
into the laboratory.

xi

xii

Practice Safe Laboratory

D O N T R U L E S
q Do not eat or drink in the laboratory.
Consume any food or drink before entering the laboratory. Chemicals
could get into food or drinks, causing illness. If you must take a break,
wash your hands thoroughly before leaving.
q Do not smoke in the laboratory.
Smoke only in designated smoking areas outside the laboratory.
Flammable gases and volatile ammable reagents could easily explode.
q Do not taste any chemicals or breathe any vapors given off by a
reaction.
If there is a need to smell a chemical, you will be shown how to do it
safely.
q Do not get any chemicals on your skin.
Wash off the exposed area with plenty of water should this happen.
Notify your instructor at once. Wear gloves as indicated by your
instructor.
q Do not clutter your work area.
Your laboratory manual and the necessary chemicals, glassware, and
hardware are all that should be on your benchtop. This will avoid
spilling chemicals and breaking glassware.
q Do not enter the chemical storage area or remove chemicals from the
supply area.
Everyone must have access to the chemicals for the days experiment.
Removal of a chemical from the storage or supply area only complicates the proper execution of the experiment for the other students.
q Do not perform unauthorized experiments.
Any experiment not authorized presents a hazard to any person in the
immediate area.
q Do not take unnecessary risks.
These DO and DONT RULES for a safe laboratory are not an exhaustive
list, but are a minimum list of precautions that will make the laboratory a
safe and fun activity. Should you have any questions about a hazard, ask
your instructor rstnot your laboratory partner. Finally, if you wish to
know about the dangers of any chemical you work with, read the Material
Safety Data Sheet (MSDS). These sheets should be on le in the chemistry
department ofce. A sample sheet is included here so you know what one
looks like. This is the MSDS for glucose. Read it and see the kind of data
included in there. Imagine all the additional cautions and precautions that
the sheets would contain were you dealing with a chemical that is toxic or
carcinogenic.

Name . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

Section . . . . . . . . . . . . . . .

Date . . . . . . . . . . . . . . .

Instructor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

Safety Quiz
Indicate whether each of the following statements is true or false by writing the word TRUE or FALSE in
the space provided.
_____

1. If chemicals come into contact with your skin, immediately wash the affected area with
copious quantities of water.

_____

2. Fume hoods are used in the chemical laboratory when using volatile or poisonous
chemicals.

_____ 3. It is permitted to leave a lit Bunsen burner unattended.


_____ 4. Always return unused chemicals to a reagent bottle to avoid wasting chemicals, you will
not contaminate the entire reagent bottle.
_____ 5. When heating a liquid in a test tube, always point the test tube in a direction away from
any other person in the laboratory.
_____ 6. Always add boiling chips to a hot solution.
_____ 7. The wearing of shorts, tank tops, mid-riffs and sandals is permitted in the laboratory.
_____ 8. Drinking soda in the lab is permitted as long as the soda can is at least 10 feet away from
all chemicals.
_____ 9. I am not required to wear safety goggles while in the laboratory unless I am actually
performing an experiment.
_____ 10. It is a violation of Federal Law to leave a Waste Container uncapped.

xiii

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

EXPERIMENT 1: CHEMICAL REACTIONS


1.

OBJECTIVES

2.

To perform different types of chemical reactions including acid-base, precipitation, gas


forming, complex compound forming and oxidation-reduction reactions.
To identify the products in these reactions and describe the chemical changes.
To write and balance the chemical equations for the reactions observed.

INTRODUCTION

Matter can undergo both physical and chemical changes. Chemical changes result in the
formation of new substances. When a chemical reaction occurs, substances called reactants
are transformed into different substances called products that often have different
appearances and different properties. In this experiment, you will perform nd observe a
number of chemical reactions. Observable signs of chemical reactions can be a change in color,
the formation of a solid, the release of gas, and the production of heat and light. You will also
learn how to classify the chemical reactions. One classification system involves five general
types of reactions: synthesis, decomposition, single displacement, double displacement, and
combustion.

3.

PROCEDURE

1. REACTIONS OF Cu2+
Step1: Put 10 drops of 0.5M CuSO4 into each of three test tubes.
Step 2:
o Test tube #1: add 10 drops of 2M NaOH
o Test tube #2: add 10 drops of 2M NH4OH
o Test tube #3: add 10 drops of 0.5M K4[Fe(CN)6].
Step 3: Record your observations (Remember to shake the test tubes gently).
2. REACTIONS OF SILVER HALIDES
Section 1: Reactions of KCl
Step 1: Prepare 03 test tubes each containing 10 drops of KCl.
Step 2: Add 10 drops of 0.1M AgNO3 to each of test tube above.
Step 3:
o Add nothing to test tube #1 for control .
o Add 5 drops of 2M NH4OH to test tube #2.
o Add 5 drops of 2M KCN to test tube #3.
Step 4: Record your observations. Remember to shake the test tubes well and wait for at
least 02 minutes.
Revision: October 1, 2013

Page 1

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

Section 2: Reactions of KBr


Repeat Section 1 with KBr instead of KCl at Step 1. Record your observations.
Section 3: Reactions of KI
Repeat Section 1 with KI instead of KCl at Step 1. Record your observations.
3. REACTIONS OF H2O2
Section 1: Place 5 drops of 0.1M KMnO4 solution into a test tube. Acidify this solution with 5
drops of 2M H2SO4 and then add 5 drops of 3% H2O2 solution. Record your observations.
Remember to shake the test tubes well and wait for at least 02 minutes.
Section 2: Place 5 drops of 0.1 M KI solution into a test tube. Acidify this solution with 5
drops of 2M H2SO4 and then add 5 drops of 3% H2O2 solution. Record your observations.
Section 3: Place 10 drops of 3% H2O2 solution into a test tube, then, add a pinch of solid
MnO2. Record your observations.
4. REACTIONS OF NITRATE BROWN RING TEST
Section 1
Step 1: Prepare a test tube containing 10 drops of 0.1M NaNO3.
Step 2: Add 10 drops of saturated FeSO4 to test tube above.
Step 3: Pour concentrated sulfuric acid, H2SO4, (96%) carefully down the inside wall of
the test tube. Wait for a few seconds and record the change of color at the interface
between the nitrate solution and the concentrated sulfuric acid.
Note: The nitric acid is reduced to nitrogen monoxide by the iron (II) ion and the brownish violet
nitroso complex compound is then found by nitrogen monoxide with the excess iron (II) ions.
Section 2
Repeat Section 1 with NaNO2 instead of NaNO3 at Step 2. Record and compare the
observations.
Section 3
Repeat Section 1 with acetic acid (CH3COOH) instead of H2SO4 at Step 3. Record and
compare the observations.
5. REACTIONS OF KMnO4
Step 1: Obtain 3 clean test tubes
o Test tube #1: 10 drops of 0.5M Na2SO3 and 5 drops of 2M H2SO4.
Revision: October 1, 2013

Page 2

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

o Test tube #2: 10 drops of 0.5M Na2SO3 and 5 drops of 6M NaOH.


o Test tube #3: 10 drops of 0.5M Na2SO3 and 5 drops distilled water.
Step 2: Add 5 drops of 0.1M KMnO4 to each of test tubes. Record your observations.
6. REACTION OF POTASSIUM DICHROMATE (K2Cr2O7)
Step 1: Place 10 drops of 0.5M K2Cr2O7 into a test tube.
Step 2: Add 10 drops of 6M H2SO4.
Step 3: Add 5 drops of C2H5OH. Record your observations.
7. REACTIONS OF Fe2+ and Fe3+
Section 1
Step 1: Place 10 drops of 0.5M FeCl3 solution in each of five test tubes.
Step 2:
o Test tube #1: Add 5 drops of 0.5M KCN.
o Test tube #2: Add 5 drops of 0.1M KSCN.
o Test tube #3: Add 5 drops of 2M KOH.
o Test tube #4: Add 5 drops of 0.5 M K4[Fe(CN)6].
o Test tube #5: Add 5 drops of 2M NH4OH.
Step 3: Record your observations
Section 2
Repeat Section 1 using FeSO4 instead of FeCl3 at Step 1. Record and compare the results.
8. REACTIONS OF Al3+
Step 1: Place 10 drops of 0.5M Al2(SO4) to each of 2 test tubes
Step 2: Add 5 drops of 2M NaOH to each test tube above.
o Test tube #1: Add 20 drops of 2M HCl
o Test tube #2: Add 20 drops of 2M NaOH
Step 3: Record your observations.
9. FLAME TEST
Step 1: Light the alcohol lamp.
Step 2: Dip a looped wire into one of the five solutions supplied (LiCl, NaCl, KCl, CaCl2
and BaCl2), and then hold it in the flame.
Step 3: Record the dominant flame color observed.
Step 4: Using the wavelengths shown below, calculate the frequency and energy of
the photons emitted during the flame tests.
Dominant color
Red
Red-orange
Revision: October 1, 2013

Wavelength (nm)
701
622
Page 3

School of Biotechnology, International University-HCMC


Department: Applied Chemistry
Orange
Orange-yellow
Yellow
Yellow-green
Green
Green-blue
Blue
Blue-violet
Violet

Laboratory Manual
General Chemistry

609
597
587
577
535
492
474
455
423

Wavelength values are given for mid-range of the color indicated. relationship between the
wavelength, frequency and speed of an electromagnetic wave is given by the
equation:
C=
And the energy per photon (in Joules) is given by the equation:
Ephoton = h
Where h is Plancks constant, which has a value of 6.626 x 10-34 J.s.

4. REPORT
Prepare the report in the following order:
Summary of theory
Describe your experiments and observation
Name the reaction type for each experiment

5. CHEMICALS AND EQUIPMENTS

Revision: October 1, 2013

Page 4

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Revision: October 1, 2013

Laboratory Manual
General Chemistry

Page 5

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

EXPERIMENT 1: LAB STRUCTURE

Revision: October 1, 2013

Page 6

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

EXPERIMENT 2: pH AND BUFFERS


1. OBJECTIVES

To distinguish between strong and weak acids


To learn how to calculate and prepare a buffer solution and test its buffering ability.

2. INTRODUCTION
Acids are proton donors and bases are proton acceptors. Acids primarily serve as sources of
hydrogenions (H+ ) or hydronium ions (H3O+ ) while bases mainly provide hydroxide ions (OH-).
Water is amphoteric because it can play a role as either an acid or a base. In other words,
water can donate and accept protons. Water undergoes auto-ionization to form H3O+ and OH-

2H2O H3O+ (aq) + OHThe extent of dissociation of water is very small; therefore pure water has no electrical
conductivity. At the equilibrium, the ion product of water is only 1 10-14 at 25o C.

Kw = [H3O+][ OH-]= 10-14


In pure water, the concentration of the [H3O+] and [ OH-] are equal:

[H3O+] = [ OH-] = 1 10-7 M


+

In acidic solutions, H3O+ ions predominate: [H3O ] > [ OH ]


+

In basic solution, OH- ions predominate: [H3O ] < [OH ]


+

For convenience the negative value of the log [H ] is used to express the concentration of H+.
Therefore the pH can be defined as:

pH=-log[H3O+]
In neutral solutions, pH = 7
In acidic solutions, pH < 7
In basic solutions, pH > 7
As a consequence, pH denotes the strength of acids or bases. The lower pH, the more acidic
the solution whereas the higher pH the more basic the solution. Strong acids and strong bases
are completely dissociated in water to produce hydrogen ions or hydroxide ions respectively.

Revision: October 1, 2013

Page 7

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

Weak acids dissociate only partially and form little or very little H+. This means that an
equilibrium is
established between the dissociated and un-dissociated forms:

HA(aq) H + A
[H ][A ]
=
[HA]

Where HA is the weak acid and A- is its conjugate weak base, of HA. The equilibrium constant
(Ka) is called the acid dissociation constant or acid ionization constant. pKa is defined in a way
comparable to pH, i.e. pKa = - lgKa.
A buffer is a solution of a weak acid and its conjugate weak base. Buffers have the function
that resists large change in pH on the addition of H+ or OH-. This is because the weak base, A-,
will react with added H+ and the weak acid, HA, will react with added OH. Changes in pH of
buffer solutions can be determined using the Henderson-Hasselbach equation:

[A ]
pH = pK + log

[HA]

A pH meter can be used to measure the pH of prepared solutions. Different classes of


chemicals behave differently when dissolved in water. By doing this experiment, you will gain a
better understanding of strong acids and strong bases, weak acids and weak bases, salts and
buffers.

3. PROCEDURE
Note: Please make sure you rinse the pH meter after each measurement.
3.1 DEIONIZED WATER
Pour about 50 mL of the room temperature deionized water into a 150 mL beaker.Stir
the water. Assemble pH meter. Record the pH value.
Stir the water for about 20 seconds. Record the pH again
Repeat the stirring and measurement process at 20 second intervals, recording each
time and pH value, until there is no appreciable change in the pH.
Repeat the experiments at least 02 times.
3.2 STRONG ACID
Pipet 10 mL of 0.1M HCl into a 100 mL beaker. Measure the pH.
Add 90 mL of distilled water. Measure the pH.
Revision: October 1, 2013

Page 8

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

Add 10 mL of 0.10M NaOH. Record the pH.


Add 90 mL of 0.01M NaOH. Record the pH.
Repeat the experiments at least 02 times
3.3 WEAK ACID
Prepare three 250-mL beaker
o Beaker 1: Place 20 mL of 0.1M acetic acid (CH3COOH). Measure the pH and
calculate Ka.
o Beaker 2: Place 20 mL 0.01M CH3COOH. Measure the pH and calculate Ka.
o Beaker 3: Place 20 mL 0.001M CH3COOH Measure the pH and calculate Ka.
Repeat the experiments at least 02 times
3.4 SALTS : prepare 3 beakers
Place 50 mL of 0.1M NaCl into a 250 mL beaker. Measure the pH.
Place 50 mL of 0.01M CH3COONa into a 250 mL beaker. Measure the pH.
Place 50 mL of 0.1M NH4Cl into a 250 mL beaker. Measure the pH.
Repeat the experiments at least 02 times
Note: in this experiment, you should prepare CH3COONA and NH4Cl solution with the
correct concentrationy by yourself.
3.5 BUFFERS
Prepare 02 150 mL beakers each containing ~100 mL of 0.1M CH3COOH and 100 mL of
0.1M CH3COONa, respectively.
Section 1:
Prepare 50 mL buffer A in a 100 mL beaker by mixing 10 mL of 0.1M CH3COOH and 40
mL of 0.1M CH3COONa
Measure the pH of the buffer solution.
Repeat the experiments at least 02 times.
Section 2:
Divide buffer A into 2 equal parts (25 mL of each). Label them.
For part 1:
o Add 10 drops of 0.1M HCl. Measure the pH.
o Add enough to change the pH by one unit from the start. Record the
volume.
Note: roughly 10 drops ~ 1 mL

For part 2:
o Add 10 drops of 0.1 M NaOH. Measure the pH.
o Add enough to change the pH by one unit from the start. Record the
volume.

Revision: October 1, 2013

Page 9

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

Section 3:
Prepare 50 mL buffer B in a 100 mL beaker by mixing 40 mL of 0.1M CH3COOH and 10
mL of 0.1M CH3COONa
Measure the pH of the buffer solution.
Repeat Section 2 with buffer B instead of buffer A.
Section 4:
Prepare 50 m buffer C in a 100 mL beaker by mixing 25 mL of 0.1M CH3COOH and 25
mL of 0.1M CH3COONa
Measure the pH of the buffer solution.
Repeat Section 2 with buffer C instead of buffer A.

4. CHEMICALS AND EQUIPMENTS

5.

LAB REPORT

Present your observation and obtained data for each part


Present your explanation and conclusions

Revision: October 1, 2013

Page 10

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

EXPERIMENT 2: LAB STRUCTURE

Revision: October 1, 2013

Page 11

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

EXPERIMENT 3: OXIDATION/REDUCTION
TITRATION WITH KMnO4
1. OBJECTIVES

Learn about the term of gram equivalent weight.


Review of oxidation-reduction reactions.
Standardize the concentration of KMnO4 solution and determine the oxalic acid
normality.

2. INTRODUCTION
In an oxidation-reduction or redox reaction, there is an exchange of electrons between to
reactants, resulting in the changes of oxidation number. The substance that gains electrons is
said to be reduced; therefore, it is called the oxidizing agent. The substance that loses
electrons is said to be oxidized; thus, it is called the reducing agent.
One gram equivalent weight (GEW) of oxidizing agent is the weight that gains 6.02x1023
electrons and one gram equivalent weight of reducing agent is the weight that loses 6.02x1023
electrons. According to the definition of gram equivalent weight, one GEW of oxidizing agent
reacts with one GEW of reducing agent:

GEWox = GEWred
Consider the reaction of potassium permanganate (KMnO4) with oxalic acid (H2C2O4) in the
presence of excess sulfuric acid (H2SO4). The balanced molecular and net ionic equations are as
follows, respectively.

2KMnO4 + 5H2C2O4 + 3H2SO4 10CO2 + K2SO4 + 2MnSO4 + 8H2O


2MnO4 + 5H2C2O4 + 6H+ 10CO2 + 2 Mn2+ + 8H2O
The oxidation number of Mn in MnO4- is +7 while it is +2 in Mn2+ . Hence, each Mn undergoes a
change in oxidation number of five. Since each formula unit of KMnO4 contains one Mn, and
each Mn gains five electrons, one mole of KMnO4 is five gram equivalent weights in this
reaction. As a result, KMnO4 produces 5 moles of electrons per mole of KMnO4 or has five
equivalents per mole of KMnO4. Thus, the gram equivalent weight of KMnO4 in this reaction is
31.60 grams.

=
Revision: October 1, 2013

Page 12

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

The oxidation number of carbon in H2C2O4 is +3 while it is +4 in CO2. Thus each carbon
undergoes a change in oxidation number of one. However, each formula unit of H2C2O4
contains two carbons, and since each carbon loses one electron, one mole of oxalic acid is two
gram equivalent weights in this reaction.
Consequently, H2C2O4 produces 2 moles of electrons per mole of oxalic acid or has two
equivalents per mole of oxalic acid. The gram equivalent weight of H2C2O4 is 45.0 grams

In this experiment, you will prepare an approximately 0.05N KMnO4 solution and standardize
this solution by titrating against a standard solution of H2C2O4 (primary standard). Then the
standardized KMnO4 solution (secondary standard) will be used to determine the
concentration of unknown oxalic acid solution and unknown Fe2+ solution. For redox titrations,
the number of equivalents of oxidizing agent must be equal to the number of equivalents of
reducing agent. For the reaction of KMnO4 with H2C2O4:

Eq. of KMnO4 = Eq. of H2C2O4


Alternatively, this relationship can be expressed as follows:

Voxidizing Noxidizing=Vreducing Nreducing


where V is the volume of oxidizing or reducing agents used in titrations and N is the normality
of oxidizing or reducing agents.
At the end of a titration, three of the four variables will be known and the unknown variable
can be determined.

3. PROCEDURE
3.1. HANDLING WITH BURET:

Clean the buret with distilled water


Rinse it three times with ~5 mL of the prepared KMnO4 solution. Discard the
rinse solution.
Fill the buret with the KMnO4 solution and allow it to drain through the buret tip
until no air bubbles remain in the tip.
Record the buret reading before beginning the titration.

Note: as the KMnO4 solution is dark color, read the buret at the top of the meniscus.

Revision: October 1, 2013

Page 13

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

3.2. STANDARDIZATION OF PREPARED KMNO4 SOLUTION:

Pipette 10 mL of standard oxalic acid solution into each of two 250 mL erlenmeyer
flasks.
Use cylinder to add approximately 40 mL of distilled water to each flask.
Use cylinder to add approximately 20 mL of 6N H2SO4 solution to each flask (This step
must be done in the fume hood).
Warm the flasks in the water bath 85oC 90oC (Use the thermometer to check the
temperature)
Titrate the hot solution against the KMnO4 solution.

Note: the KMnO4 solution should be added very slowly initially. Endpoint for this experiment
refers to the titrate volume needed to keep the faint pink color throughout the stirred
solution for at least twenty seconds. Record the buret reading and calculate the normality of
the KMnO4 solution.
3.3. DETERMINATION OF UNKNOWN CONCENTRATION H2C2O4 SOLUTION:
Prepare 10 mL of the unknown concentration solution of H2C2O4 into each of
two 250 mL Erlenmeyer flasks.
Use cylinder to add ~40 mL of distilled water to each flask.
Use cylinder to add ~20 mL of 6N H2SO4 solution to each flask (fume hood).
Warm the flasks in water bath 85oC 90oC. (Use the thermometer to check the
temperature)
Titrate the hot solutions agains the KMnO4 solution.
Calculate the normality of the unknown concentration H2C2O4 solution; determine the
average and the standard deviation.
3.4. DETERMINATION OF UNKNOWN CONCENTRATION FESO4 SOLUTION:
Prepare 10 mL of unknown concentration solution of FeSO4 solution into each of
three 250 mL Erlenmeyer flasks.
Add 40 mL of distilled water to each flask.
Add 20 mL of 6N H2SO4 solution to each flask (fume hood).
Warm the flasks in water bath 85oC 90oC.
Titrate the hot solutions.
Calculate the normality of the unknown concentration FeSO4 solution; determine the
average and the standard deviation.

6. CHEMICALS AND EQUIPMENTS

Revision: October 1, 2013

Page 14

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

7.

Laboratory Manual
General Chemistry

LAB REPORT

Present your observation and obtained data for each part


Present your explanation and conclusions

Revision: October 1, 2013

Page 15

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

EXPERIMENT 3: LAB STRUCTURE

Revision: October 1, 2013

Page 16

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

EXPERIMENT

Laboratory Manual
General Chemistry

4: CHEMICAL EQUILIBRIUM

1. OBJECTIVES

To observe the effect of applying stresses on chemical systems at equilibrium.


To apply Le Chateliers Principle to explain the changes in the system

2. INTRODUCTION
A reversible reaction is at equilibrium when the rate of the forward reaction becomes equal to
the rate of the backward reaction. Reversible reaction:

A reversible reaction at equilibrium can be disturbed if a stress is applied to it. Stresses can be
changes in concentration, temperature or pressure. The composition of the reaction mixture
will shift until equilibrium has been reestablished. This is known as Le Chateliers Principle. In
this experiment, the effect of applying stresses to a variety of chemical systems at equilibrium
will be observed and we also see if the results are consistent with Le Chateliers Principle.

3.PROCEDURE
1. SYSTEM 1: ACID/BASE EQUILIBRIA
Place 10 drops of 0.5M K2CrO4 to a clean test tube.
Add 05 drops of concentrated HCl. Observe the change of color.
And then add 10 drops of 6N NaOH. Record your observations.
Equilibrium System:

2CrO42- + 2H+ (aq) Cr2O72- + H2O(l)


2. SYSTEM 2: EQUILIBRIA OF ACID/BASE INDICATORS
Place 2 drops of methyl violet to a clean test tube. Add 20 mL of distilled water, mix
well. Divide the solution evenly into two test tubes. Save one as a reference. Note the
color.
Test tube #1 (reference): add nothing
Test tube #2:
o Addition #1: add the 6M HCl solution drop wise until further addition
results in no significant change. Observe the change.
o Addition #2: add the 6M NaOH solution drop wise until further addition
results in no color change. Observe the change.

Revision: October 1, 2013

Page 17

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

o Addition #3: again add the 6M HCl solution drop wise until further addition
results in no significant change. Observe the change.
Equilibrium System:
H(MV)(aq) + H2O(l) H3O+ (aq) + MV(aq)
3. SYSTEM 3: COMPLEX ION FORMATION
Preparation of iron (III) thiocyanate solution: in a 250 mL beaker, place 10 mL of 0.01
M FeCl3 and 10 mL of 0.01 M KSCN, and then add 50 mL of distilled water, mix well.
Use a pipet, divide the solution evenly among 07 similarly-sized test tubes (#1-7).
Test tube #1 (control): add nothing
Test tube #2: add 2 mL of 0.01 M FeCl3 to the solution. Observe the change.
Note that 1 mL 1012
Test tube #3: add 2 mL of 0.01 M KSCN to the solution. Observe the change.
Test tube #4: add 10 drops of 6 M NaOH to the solution. Describe the change in
the solution.
Test tube #5: cool the test tube in an ice bath.
Test tube #6: warm the test tube in a hot water bath. Compare the intensity of
the color in test tubes #1(control room temperature), #5 (cold), and #6 (hot).
Test tube #7: add 0.1 M AgNO3 solution drop by drop until all the color
disappears. Record your observations
Equilibrium System:

Fe3+ (aq) + SCN-(aq) [Fe(SCN)]2+(aq)


Pale yellow

Clear

Red

4. SYSTEM 4: EQUILIBRIA OF PRECIPITATION REACTIONS


Place 5 mL of 0.05 M CaCl2 into each of the two test tubes labeled #1 and #2
Test tube #1: add 1 mL of 0.1M Na2C2O4 solution. Observe the change.
Test tube #2:
o Addition #1: add 1 mL of 0.1M H2C2O4. Observe the change, comparing to
test tube #1.
o Addition #2: add 10 drops of 6M HCl. Observe the change.
o Addition #3: add 10 drops of 6M NH4OH. Observe the change.
Equilibrium System:

Ca2+ (aq)

C2O42- (aq)

CaC2O4(s)

5. SYSTEM 5: TEMPERATURE EFFECTS ON EQUILIBRIA


Place 3 mL (~30 drops) of 0.1 M CoCl2 into a test tube. Add concentrated HCl drop
wise until the solution turns a purple-violet color. If the system turns a deep

Revision: October 1, 2013

Page 18

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

blue, indicating too much chloride, discard the solution and start again. Note:
this practice should be performed under the fume hood.
Divide the solution equally into three test tubes labeled #1-3.
Test tube #1(control): keep at room temperature.
Test tube #2: place in a hot water bath. Observe the change.
Test tube #3: place in an ice-water bath. Observe the change.
Switch test tubes 2 and 3. Observe the change. Allow them both to cool to room
temperature. Compare to the control.
Equilibrium System:

[Co(H2O)6]2+(aq)

+ 4Cl-(aq)

4.

CHEMICAL AND EQUIPMENTS

8.

LAB REPORT

[CoCl4]2-(aq)

+ 6H2O(l)

Present your observation and obtained data for each part.


Present your explanation and conclusions.

Revision: October 1, 2013

Page 19

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

EXPERIMENT 4: LAB STRUCTURE

Revision: October 1, 2013

Page 20

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

EXPERIMENT 5: REACTION RATE


1.

OBJECTIVES

2.

To examine the effect of concentration, temperature, and catalysts on reaction rates.

INTRODUCTION

The rate of a chemical reaction describes how fast the reaction occurs. The rate of a chemical
reaction is affected by a number of factors including temperature of the reaction, the nature of
the reactants, concentration of the reactants, the surface area of the reactants, the presence
of a catalyst and the pressure the reaction is under. The greater the rate of a chemical
reaction, the less time is needed for a specific amount of reactants to be converted to
products. The rate of a reaction can be determined one of two ways; either measure the time
it takes for one or more of the reactants are used up, or for the products to be formed.

3.

PROCEDURE

PART 1: EFFECT OF CONCENTRATION ON REACTION TIME


The solutions to be used are as follows:
Preparation of Solution A: 0.20M potassium iodide (KI)
Preparation of Solution B: 0.005M sodium thiosulfate (Na2S2O3). This solution also
contains starch that will act as an indicator to detect the presence of iodine.
Preparation of Solution C: 0.10M ammonium peroxydisulfate ((NH4)2S2O8)
In this reaction, solution B will be the limiting reagent. The reactions involved are these:

2I- + S2O82- I2 + 2SO42

Reaction 1:

Iodide ions + peroxydisulfate ions iodine + sulfate ions

I2

Reaction 2:

2S2O32 2I + S4O62

Iodine + thiosulfate ion

iodide ion + tetrathionate ion

Reaction 1 is relatively slow. As the iodine is formed it is quickly used in reaction 2, which is
relatively fast. The limiting reaction (solution B) is a source of the thiosulfate ions. When
solution B is used up, the excess iodine formed will react with starch to form a deep blue
solution.
In this experiment, you will vary the concentrations of solutions A and C. The temperature will
remain constant at room temperature.
Combine the solution in 11 different combinations. The procedure for each of the reactions is
the same
Revision: October 1, 2013

Page 21

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

o Step 1: label 11 test tubes #111 with the corresponding amount of solution A (see
the table below).
o Step 2: place 5.0 mL of solution B in each test tube and add 12 drops of starch
o Step 3: label another 11 test tubes with the corresponding amount of solution C
(see the table below).
o Step 4: add solution C into test tube containing solution A+B with the volume as
shown in the table below. Begin timing using stopwatch. Sir the solution with a
clean stirring rod. At the first sign of color, stop timing. Record the results on the
data table.
o Step 5: Calculations
Calculate the initial concentrations of iodide and peroxydisulfate ion for each of the
mixtures.
For example: mixture 1
Iodide ion:

( )(. /)

Peroxydisulfate:

= 0.080 mol/L

( )(. /)

= 0.040 mol/L

o Step 6: Built the graphs


Plot the concentration of iodide ion versus time for mixtures # 16. Time should
be on the X axis and the concentrations should be on the Y axis.
Plot the concentration of peroxydisulfate ion versus time for mixtures # 1, 7, 8, 9,
10, and 11. Again, time should be on the X axis and the concentrations should be
on the Y axis.
Number
1
2
3
4
5
6
7
8
9
10
11

Revision: October 1, 2013

Solution A
10.0
8.5 + 1.5 distilled water
7.0 + 3.0 distilled water
5.5 + 4.5 distilled water
4.0 + 6.0 distilled water
2.5 + 7.5 distilled water
10.0
10.0
10.0
10.0
10.0

Solution B
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0

Solution C
10.0
10.0
10.0
10.0
10.0
10.0
8.5 + 1.5 distilled water
7.0 + 3.0 distilled water
5.5 + 4.5 distilled water
4.0 + 6.0 distilled water
2.5 + 7.5 distilled water

Page 22

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

PART 2: EFFECT OF TEMPERATURE ON THE REACTION RATE


The reaction rate for the oxidationreduction reaction between potassium permanganate,
KMnO4, and oxalic acid, H2C2O4, can be measured by observing the time elapsed for the purple
color of the permanganate ion, MnO4 , to disappear.
5H2C2O4(aq) + 2KMnO4(aq) + 3H2SO4 2MnSO4(aq) + K2SO4(aq) + 10CO2(g) + 8H2O
Prepare the reaction system (use cylinder to get the chemicals):

o Place 1 mL of 0.01M KMnO4 and 5 mL of 3M H2SO4 into a clean test tube (3


tubes)
o Place 5 mL of 0.33M H2C2O4 into a second, clean test tube. (3 tubes)
o
Observe the reaction at room temperature:
Pour the H2C2O4 solution into the KMnO4 solution. Observe and record the time for the
purple color of the permanganate ion to disappear.

Observe the reaction at high temperature:


o Place a second KMnO4H2C2O4 pair of test tubes in warm water (500 C) bath
until thermal equilibrium is established. Pour the H2C2O4 solution into the
KMnO4 solution, mix well and return the reaction system to the warm water
bath. Record the time for the purple color to disappear.
o Repeat the same procedure, but increase the temperature of the water bath to
about 900 C. Record the change

PART 3: EFFECT OF A CATALYST ON THE REACTION RATE


Hydrogen peroxide is relatively, but readily decomposes in the presence of a catalyst. In this
part, you will observe which reagent(s) act as a catalyst for the decomposition of hydrogen
peroxide.

2H2O2 2H2O + O2

Label 7 test tubes # 17


Place 5 mL of the 3% H2O2 solution into each of the 8 test tubes.
Add a pinch of each of the following reagents to separate test tubes:
MnCl2 MnO2 NaCl CaCl2 Zn KNO3 Fe(NO3)3
Mix well and observe the change with the production of gas bubbles.
Record each reaction rate as fast, slow, very slow, or none in your data table.

Revision: October 1, 2013

Page 23

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

4.

5.

Laboratory Manual
General Chemistry

CHEMICALS AND EQUIPMENTS

LAB REPORT

Present your observation and obtained data for each part


Plot the graph in excel and prepare your report in Microsoft Word
Present your conclusions

Revision: October 1, 2013

Page 24

School of Biotechnology, International University-HCMC


Department: Applied Chemistry

Laboratory Manual
General Chemistry

EXPERIMENT 5: LAB STRUCTURE

Revision: October 1, 2013

Page 25

You might also like