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CHM 107 Manual

Practical Manual

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CHM 107 Manual

Practical Manual

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You are on page 1/ 41

DEPARTMENT OF CHEMISTRY

FACULTY OF SCIENCES
FEDERAL UNIVERSITY OF HEALTH SCIENCES OTUKPO

CHM 107 PRACTICAL MANUAL

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STUDENT PERSONAL DATA

Name of Student: ______________________________________________________________

Matric Number:_______________________________________________________________

Department:__________________________________________________________________

Programme:__________________________________________________________________

Group Number:_______________________________________________________________

Locker Number:_______________________________________________________________

Signature:____________________________________________________________________
Page 3 of 41

TABLE OF CONTENTS

Cover Page
Student’s Personal Data
Table of Contents
General Chemistry Laboratory Safety
Introduction to Chemistry Practical
Classification of Analytical Method
Method of Expressing Concentrations

Experiment 1: Preparation and Standardization of NaOH Solution

Experiment 2: Titration of strong acid with a strong base using methyl
Orange and phenolphthalein as indicators
Experiment 3: Standardization of dilute H2SO4 solution using a standard
Solution of Na2CO3 solution
Experiment 4: Standardization of dilute sodium hydroxide solution using a

Standard solution of ethanedioic acid (H2C2O4.2H2O)

Experiment 5: Determination of the percentage of ammonia in an ammonium
Salt by back titration
Experiment 6: Determination of the concentration of Na2CO3 and NaHCO3 in a
Mixture

Experiment 7: Standardization of FeSO4.XH2O using KMnO4

Experiment 8: Determination of the number of molecules of water of crystallization

in FeSO4.XH2O using a standard solution of KMnO4

Experiment 9: Standardization of ammonium ferrous sulphate using K2Cr2O7
Experiment 10: Analysis of a simple drug (antacid)
Page 4 of 41

GENERAL CHEMISTRY LABORATORY SAFETY

The chemistry laboratory can be a place of discovery and learning. However, by the very nature
of laboratory work, it can be a place of danger if proper common-sense precautions aren't taken.
While every effort has been made to eliminate the use of explosive, highly toxic, and
carcinogenic substances from the experiments which you will perform, there is a certain
unavoidable hazard associated with the use of a variety of chemicals and glassware. You are
expected to learn and adhere to the following general safety guidelines to ensure a safe
laboratory environment for both yourself and the people you may be working with. Additional
safety precautions will be announced in class prior to experiments where a potential danger
exists. Students who fail to follow all safety rules may be asked to leave the lab or suffer grading
penalties.

Dressing code

1. Safety goggles must be worn at all times while in the laboratory. This rule must be
followed whether you are actually working on an experiment or simply writing in your
lab notebook. You must wear safety goggles provided by the chemistry department. (we
will get you informed when this is available at the department)
2. Contact lenses are not allowed in the laboratory. Even when worn under safety goggles,
various fumes may accumulate under the lens and cause serious injuries or blindness.

3. Closed toe shoes and long pants must be worn in the laboratory. Sandals and shorts are
not allowed.

4. Long hair must be tied back when using open flames.

Conduct in Laboratory

1. Eating, drinking, and smoking are strictly prohibited in the laboratory.

2. No unauthorized experiments are to be performed. If you are curious about trying a
procedure not covered in the experimental procedure, consult with your laboratory
instructor.
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3. Never taste anything. Never directly smell the source of any vapour or gas; instead by
means of your cupped hand, waft a small sample to your nose. Do not inhale these
vapours but take in only enough to detect an odour if one exists.

4. Coats, backpacks, etc., should not be left on the laboratory benches and stools. There is a
hook rack along the back wall at either end of the laboratory. There are coat racks just
inside each entrance to the balance room at the back of the lab. Beware that laboratory
chemicals can destroy personal possessions.

5. Always wash your hands before leaving laboratory.

6. Learn where the safety and first-aid equipment is located. This includes fire
extinguishers, fire blankets, and eye-wash stations.

7. Notify the instructor immediately in case of an accident.

Proper Handling of Chemicals and Equipment

1. Consider all chemicals to be hazardous unless you are instructed otherwise. Material
Safety Data Sheets (MSDS) are available in laboratory for all chemicals in use. These will
inform you of any hazards and precautions of which you should be aware.
2. Know what chemicals you are using. Carefully read the label twice before taking anything
from a bottle. Chemicals in the laboratory are marked with NFPA hazardous materials
diamond labels. Learn how to interpret these labels.

3. Excess reagents are never to be returned to stock bottles. If you take too much, dispose of
the excess.

4. Many common reagents, for example, alcohols and acetone, are highly flammable. Do
not use them anywhere near open flames.

5. Always pour acids into water. If you pour water into acid, the heat of reaction will cause
the water to explode into steam, sometimes violently, and the acid will splatter.

6. If chemicals come into contact with your skin or eyes, flush immediately with copious
amounts of water and consult with your instructor.

7. Never point a test tube or any vessel that you are heating at yourself or your neighbour, it
may erupt like a geyser.
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8. Dispose of chemicals properly. Waste containers will be provided and their use will be
explained by your instructor. Unless you are explicitly told otherwise, assume that only
water may be put in the laboratory sinks.

9. Clean up all broken glassware immediately and dispose of the broken glass properly.

10. Never leave burners unattended. Turn them off whenever you leave your workstation. Be
sure that the gas is shut off at the bench rack when you leave the laboratory.

11. Beware of hot glass; it looks exactly like cold glass.

INTRODUCTION TO CHEMISTRY PRACTICAL

1. CLASSIFICATION OF ANALYTICAL METHODS
Chemistry practical is usually divided into qualitative and quantitative analyses, the goal
of qualitative analysis is to determine what the constituents in a sample are, while
quantitative analysis determines how much of each constituent is in a sample. A
qualitative analysis is conducted largely with a solution of the substance, and for that
reason, reaction tests are carried to determine the presence of certain ions. The methods
of qualitative analysis involve, therefore the detection of ions or radicals and not the
identification of specific compounds, unless the substance under analysis is a single
compound. This is usually classified on the basis of different techniques such as
gravimetric, volumetric and instrumental analyses.

Gravimetric Analysis
In gravimetric analysis, the constituent to be determined is isolated, either as an element
or as a compound of definite composition. This element or compound is weighted, and
from its weight and its known chemical composition the amount of the desired
constituent is determined. In most cases, the elements or compounds is separated by
precipitation with a chemical reagent. In a few cases, it is deposited on an electrode by
electrolytic means.

Volumetric Analysis
A volumetric method of analysis comprises of two techniques in which the volume of a
gas is measured to the volume of a solution of known concentration. The later technique
is known as titrimetric analysis. Titrimetric analysis consists of titration. Titration is the
procedures by which a solution of known concentration is added to another solution until
the chemical reaction between the two solutes is complete. The solute whose
concentration is known is called the standard solution or the titrate. The standard (titrate)
is slowly added from a burette to a solution which contains a known volume or known
mass of solute. The later solution is commonly referred to as the unknown.

The point at which stoichiometrically equivalent quantities of substance have been

brought together is known as the equivalent point of titration in order to titrate an
unknown when the equivalent point of titration has been reached. It is usually done by
using what is called an indicator which in most cases are organic substances (dyes)
which changes colour or gives some other obvious physiochemical changes in the
titration solution when an amount of the standard solution (titrate) added is equivalent, or
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with negligible error almost equivalent to the sample. The moment at which the indicator
changes the colour of the titrate solution is called the end point of titration. In other
words the observable experimentally determined position of the stoichiometric point of
the titration is called the end point, while the actual theoretical stoichiometric point of the
titration is the equivalent point. A successful titration is a titration with good quantitative
results, which is possible only if the end point as established by the indicators occurs at
the equivalence point in the titration. The difference between end point and equivalent
point is the titration error.
There are four types of titration each of which is based on a certain type of reaction, i.e.;
a.) Acid–base titration
b.) Oxidation–reduction titration
c.) Precipitation titration
d.) Complexometric titration

There are three different techniques for determination of an unknown sample in titration
analysis;
a.) Direct titration: It is when standard solution directly reacts with the substance being
determined.
b.) Indirect titration: It is when standard solution does not react with the substances
being determined, but instead with another substance that is produced in the same
equivalent amount to the determined substances.
c.) Back titration: It is an accurately measured amount of one standard solution is added
to the sample, in excess of the stoichiometric amount of the substance to be
determined in the sample then, the uncorrected excess is titrated with another
standard solution. For this type of titration, two standard solutions are needed.

Instrumental Analysis
This form of analysis generally includes all physiochemical methods which involve the
use of some sophisticated instruments. For example, instrument involving:
a.) Optical method: Based on how the same acts towards electromagnetic radiation.
Some important techniques utilizing this method are colorimetric, spectroscopy,
nuclear magnetic resonance.
b.) Electrical method: In which progress and completion of the chemical reaction is
indicated by electrical means. Some important techniques utilizing this method are
potentiometric titration, conductor, polarography, etc.

2. METHOD OF EXPRESSING CONCENTRATIONS

The term concentration is used to denote the amount of solute dissolved in a given
quantity of solvent or in a solution. The concentration of a solution can be expressed
either qualitatively or quantitatively. The term dilute and concentrated are used
quantitatively to describe solution. A solution with a relatively small amount of solute is
said to be dilute. One with a large amount is said to be concentrated.
Several quantitative expressions of concentration are employed. They include:
i.) Molarity (M): The molarity of a solution is defined as the number of moles of
solute in one cubic decimetre (dm3) or litre (L) of solution;
Molarity =
ii.) Normality (N): Normality is defined as the number of gram–equivalent weights
of solute per dm3 of solution. This term is no longer encourage, but will be found
in a number of older books;
Page 8 of 41

Normality =
iii.) Weight percentage (%): Weight percentage is defined as the ratio of the weight of
solute to the total weight of solute plus solvents;
wt/wt (%) =
iv.) Volume percentage (%): Volume percentage is defined as the ratio of volume of
solute to total volume of solute plus solvent;
vol/vol (%) =
v.) Weight volume percentage (%w/v): Weight/volume percentage is defined as the
number of grams of solute per one hundred cm3 of solution;
wt/vol (%) =
vi.) Molality: It is number of moles of solute in 1000 g solvent;
Molality =
These are the most commonly used ways of expressing concentration in analytical
chemistry. But there are others such as: mole fraction, parts per thousand (ppt), parts per
million (ppm), gram per unit volume, specific gravity and volume ratios. It must be
stressed that regardless of concentration unit, the concentration of standard solution is
usually expressed in molarity. The advantage of expressing concentration in terms of the
molar solution is that volumes of reacting solution of the same concentration bear simple
ratio to one another.

It is rarely possible to find an indicator that will indicate exact equivalence point, hence
the change in colour. It has been observed that the end point of any titration is the end of
the titration, although the end point of titration does not coincide exactly with the
equivalence point, the error is negligible.
Page 9 of 41

EXPERIMENT 1
TITLE: PREPARATION AND STANDARDIZATION OF NaOH SOLUTION
Aims and Objectives
i.) Learning to use a pipette
ii.) Learning to use a burette
iii.) Learning to prepare standard solutions
iv.) Learning to do a titration correctly
v.) Learning to calculate the concentration of solutions from titration data.

Equipment and Reagents

i.) 1 burette, 50 cm3
ii.) 1 pipette, 25 cm3
iii.) 3 conical flask, 250 cm3 each
iv.) 3 beakers, 250 cm3 each
v.) 1 retort stand
vi.) 1 white tile
vii.) 5M NaOH solution
viii.) Standard solution of 0.1M HCl

Procedure
 Dilute 2 cm3 of 5M NaOH with 100 cm3 distilled water in an appropriate container.
Mix the solution thoroughly to homogenize.
 Transfer accurately, using a pipette 25 cm3 of your NaOH solution into a clean 250
cm3 conical flask.
 Rinse a burette twice with a few cm 3 of your HCl solution and fill it with the same
solution to above the zero mark, making sure the burette tip is full.
 Titrate the solution of 0.1M HCl with the solution of NaOH with an indicator. During
the titration, thoroughly swirl the conical flask to ensure good mixing of acid and
base.
 Repeat the titration using a flask with sample of NaOH solution until at least two
titrations are within the accuracy of ±0.2 cm3 of the titrant used.
 The equation for the reaction is as follows;
NaOH + HCl  NaCl + H2O

Questions
1.) Tabulate your burette reading and calculate the average volumes of HCl solution
used.
2.) Calculate the concentration in mol/dm3 of the NaOH.
3.) If it takes 38.70 cm3 of 1.90M NaOH to neutralize 10.30 cm3 of H2SO4 in a
battery, what is the concentration of the H2SO4?
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Unit Objectives (please state or describe)

Lab Report (the space provided below is for experimental report and general answer to
questions)
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For Office Use

Marks Obtained:________________________________
Comment:______________________________________
Name of Instructor:_______________________________
Signature and Date:________________________________
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EXPERIMENT 2
TITLE: TITRATION OF STRONG ACID WITH A STRONG BASE USING
METHYL ORANGE AND PHENOLPHTHALEIN AS INDICATORS
Aims and Objectives
i.) Learning how to use a pipette
ii.) Learning how to use a burette
iii.) Learning how to do a titration accurately
iv.) Learning how to calculate the concentration of a solution from titration data.

Theory
Titration of strong acid and strong base gives an almost neutral salt. However, since the
indicators used have acid and base and end points first occurs before an acid is
neutralized but the second is neutralized after the presence of excess alkali.

Equipment and Reagents

a.) 1 burette 50 cm3
b.) 1 pipette 25 cm3
c.) 3 conical flask 250 cm3 each
d.) 3 beakers 250 cm3 each
e.) 1 retort stand with a white title
f.) 0.1 mol/dm3 HCl
g.) NaOH solution
h.) Methyl orange indicator
i.) Phenolphthalein indicator

Procedures
– Transfer accurately using a pipette 25 cm 3 of NaOH solution into a clean 250 cm 3
conical flask.
– Rinse a clean burette twice with few cm 3 of 0.1M HCl solution and fill it with the
same solution to above the zero mark, making sure the burette tip is full.
– Add about 2 to 3 drops of methyl orange indicator to the 25 cm 3 NaOH solution in
the flask, mix thoroughly.
– Titrate the changes to orange as the end point.
– Then add 2 to 3 drops of phenolphthalein to the content of the conical flask and
continue with the titration drop by drop until the colour changes to pink.
– Take note of end point of the two titrations.
– Repeat the titration using fresh samples of NaOH solution until at least two titrations
are with the accuracy of +0.02 cm3 of the titrant used.

Questions
1. Tabulate your burette reading and calculate the average volume of HCl used in
each sets of titrations.
2. Write a balanced equation for the reaction
3. Calculate the concentration of NaOH in mol/dm 3 and g/dm3 used, using methyl
orange as indicator.
4. Calculate the concentration of NaOH in mol/dm3 and g/dm3 used, using
phenolphthalein as indicator.
5. Compare and contrast the accuracy of the indicators used.
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Unit Objectives (please state or describe)

Post Lab Activities (please, refer to the questions in the manual and provide answers)

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For Office Use

EXPERIMENT 3
TITLE: STANDARDIZATION OF DILUTE H2SO4 SOLUTION USING A
STANDARD SOLUTION OF Na2CO3 SOLUTION
Aims and Objectives
i.) Learn how to prepare standard solutions
ii) To standardize dilute H2SO4
iii) To assess the amount of Na2CO3 in a known volume of solution equation:
H2SO4 + Na2CO3  Na2SO4 + H2O + CO2

Equipment and Reagents

Pipette, 5.3 g/dm3 Na2CO3, conical flasks, methyl orange, burette.

Procedure
Wash the glassware thoroughly with soap and distilled water. Rinse the pipette and
burette twice with base and acid, respectively. Fill the burette with the dilute H 2SO4
solution using a glass funnel. Clamp the burette onto a retort stand and note the initial
burette reading. Ensure that air bubbles are not trapped in the burette. Pipette 20 or 25
cm3 of the 5.3 g/dm3 Na2CO3 solution into a clean but not necessarily dry conical flask
and add 2 drops of methyl orange to the solution. Note the colour of the indicator in the
base. Slowly run the acid from the burette into the base in the conical flask while
swirling the contents until a permanent faint pink colour is obtained. Consider this first
titration as a rough titration. Carry out two more titrations using fresh solutions of acid
and base until you obtain fairly constant results that do not differ by more than ±0.2 cm3.

Questions
1. The number of moles of Na2CO3 in volume used.
2. The concentration of Na2CO3 solution in mol/dm3.
3. Equivalent mole of H2SO4 used.
4. Calculate the concentration in mol/dm3 of H2SO4 solution.
5. Calculate the concentration in g/dm3 of the H2SO4.
[H = 1, C = 12, O = 16, S = 32, Na = 23]
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Unit Objectives (please state or describe)

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For Office Use

EXPERIMENT 4
TITLE: STANDARDIZATION OF DILUTE SODIUM HYDROXIDE SOLUTION
USING A STANDARD SOLUTION OF ETHANEDIOIC ACID
(H2C2O4.2H2O)
Aims and Objectives
i.) To learn about reactions involving weak acid and strong bases.
ii.) To learn about indicator appropriate for reactions involving weak acid and strong
base.
iii.) To standardize dilute NaOH.

Theory: This is an acid–base reaction in which a strong base neutralizes a weak acid.
Phenolphthalein is the suitable indicator for this titration. The neutralization reaction
proceeds according to the following equation;
H2C2O4.2H2O + 2NaOH  Na2C2O4 + H2O
The indicator colour change is pink to colourless.

Equipment and Reagents

Pipette, burette, 1.50 g/250 cm3 ethanedioic acid, phenolphthalein indicator.

Procedure
Wash all your glassware as in the previous titration exercises. Put the 1.50 g/250 cm 3
ethanedioic acid into the burette and titrate it against 20 or 25 cm 3 potions of the NaOH
solution in a conical flask containing two drops of phenolphthalein indicator. Record
your results as before. Repeat the titration twice using fresh solutions in each case until
the readings are fairly constant.

Questions
Calculate the following;
1. Concentration of the ethanedioic acid in mol/dm3.
2. Concentration of NaOH solution in mol/dm3.
3. Concentration of NaOH solution in g/dm3.
[H = 1, C = 12, O = 16, Na = 23]
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Unit Objectives (please state or describe)

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(ii) ____________________________________________________________________
(iii) ___________________________________________________________________
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(v) ____________________________________________________________________
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For Office Use

EXPERIMENT 5
TITLE: DETERMINATION OF THE PERCENTAGE OF AMMONIA IN AN
AMMONIUM SALT BY BACK TITRATION
Aims and Objectives
i.) Learning the use of pipette and burette
ii.) Learning the concept of back titration
iii.) Learning how to calculate % of a compound in its salt.

Theory
Ammonium ions in ammonium salts react with sodium hydroxide according to the
equation:
NH + NaOH  NH3 + H2O + Na

In this reaction, a volatile product ammonia is formed. If excess of NaOH is used, all
ammonium ions in the salt are converted to ammonia which is expelled by boiling. The
excess sodium hydroxide is then found by titrating with a standard acid. This technique
in which a substance reacts with an excess of a standard and the unreacted amount is
determined using another standard is called a back titration.

Equipment and Reagents

Weighing bottle, 1.70 g/250 cm3 ammonium salt, conical flask, Bunsen burner, litmus
paper, 250 cm3 volumetric flask, distilled water, methyl orange, 0.2 mol/dm 3 HCl
solution.

Procedure
Weigh accurately in a weighing bottle 1.70 g of the ammonium salt provided and transfer
to a 250 cm3 conical flask. Pour in 50 cm3 of 1.25 mol/dm3 solution of sodium hydroxide
and swirl gently to dissolve the salt. Heat the flask gently to boiling on a Bunsen burner
to drive off the ammonia released. Continue boiling till all the ammonia is released
(about 15 min) as evidenced by negative test of the vapour with red litmus paper (do not
allow the paper to touch the walls of the flask). Cool the flask under the tap then pour its
content into a 250 cm3 volumetric flask. Rinse the conical flask twice and transfer the
washings to the volumetric flask. Make up the volume to 250 cm 3 using distilled water.
Shake properly to homogenize the solution. Titrate 25 cm 3 portions of this solution
against 0.2 mol/dm3 solution of HCl to a methyl orange endpoint. Record your results.

From your results, calculate;

a.) The mole of NaOH in the original 50 cm 3 of 1.25 mol/dm3 solution of NaOH and
hence the concentration of sodium hydroxide in the 250 cm3 of solution provided.
b.) The concentration of residual NaOH after reaction with the ammonium salt.
c.) The amount hence percentage in ammonia in the salt.
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Unit Objectives (please state or describe)

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For Office Use

EXPERIMENT 6
TITLE: DETERMINATION OF THE CONCENTRATION OF Na2CO3 AND NaHCO3
IN A MIXTURE
Aims and Objectives
i.) To estimate individual components in a mixture.
ii.) Use of two indicators in a titration.
iii.) To relate the choice of indicator to type of reaction.

Background
The equations for the reactions taking place during the titration of NaHCO3;
1.) HCl + NaCO3  NaCl + NaHCO3 Step I
2.) HCl + NaHCO3  NaCl + H2O + CO2 Step II

There are two steps in the above titration. In step I, using phenolphthalein as indicator, only the
carbonate is reacting. The bicarbonate remains un–reacted. Two times the burette reading
contained in this titration is therefore the amount of acid required to completely neutralize the
carbonate portion of the mixture. When titration is continued after the phenolphthalein
endpoints, methyl orange is then used as indicator for the bicarbonate to be neutralized.
Step II: In this step, both bicarbonate produced from partial neutralization of carbonate (step I),
and bicarbonate originally present in the mixture is neutralized since the bicarbonate from the
original carbonate would require the same amount of acid for neutralization as in step I. the
mixture is total acid used (steps I and II), less two times acid used in step I, the amount of acid
required for neutralization of original bicarbonate in mixture is total acid used (steps I and II),
less two times acid used in step I;
 To find the concentration of sodium carbonate we have to use two times volume used
during titration with phenolphthalein as indicator (a)
 To find the concentration of sodium bicarbonate present originally in the sample, we
have to use the volume of HCl required in step II, while using methyl orange as
indicator (b) less volume used in step (a), of this volume, i.e. (b – a).
PROCEDURE
1.) Rinse a burette twice with a few cm 3 of standard HCl and then fill it with the same
solution above zero mark and drain to the same making sure the burette tip is full.
2.) Using a pipette, transfer 10 cm3 of your given sodium carbonate and NaHCO3
solution into a conical flask, dilute it to about 55 cm 3 with distilled water, and three
drops of phenolphthalein indicator and titrate until the solution in the flask becomes
colourless. During the titration, swirls the conical flask thoroughly to ensure good
mixing.
3.) Take the reading of the burette and record the amount of acid used as (a).
4.) To the same solution in the conical flask, add three drops of methyl orange and
demonstrate as instructed in part 2 above, until the first change of colour from yellow
to yellow–orange.
5.) Read burette and record the volume of acid used for the second titration (with methyl
orange as indicator) only as b.
6.) Repeat the titration using a fresh sample of mixture until at least two titrations are
within the accuracy of 0.2 cm3 of the titrant used.
Questions
1. Tabulate your reading and calculate the average volume of the HCl used.
2. Write a balanced equation for the complete neutralization of Na 2CO3 and
NaHCO3.
3. Calculate the concentration of NaHCO3 and Na2CO3 in mol/dm3 using mole
concept.
Page 25 of 41

Unit Objectives (please state or describe)

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For Office Use

EXPERIMENT 7
TITLE: STANDARDIZATION OF FeSO4.XH2O USING KMnO4
Aims and Objectives
i.) Learning to standardize using KMnO4.
ii.) Expose students to titrations that do not require indicators.
iii.) Learning to calculate concentrations from redox reactions.

Background
Potassium permanganate (KMnO4) is a powerful oxidizing agent and is used for the
determination or many reducing agents, especially acidic to prevent the formation of
manganese (IV) oxide.

Equipment and Reagents

HCl, Acidified solution FeSO4.XH2O, a burette, a pipette, 3 conical flasks, a retort stand
with a white tile, IM solution of H2SO4

Procedure
a.) Take 25 cm3 of the solution of acidified iron (II) sulphate using a pipette into a clean
conical flask.
b.) Add about 10 cm3 of the dilute H2SO4 the titrate with KMnO4 solution in the burette
until first permanent pink colour is observed (no brown precipitate should appear).
c.) Repeat the process 2 more times. Tabulate your burette readings and find the average
volume of KMnO4 used.
d.) Write a balance equation for the reaction.

Questions
1. Calculate the concentration of FeSO4 solution in mol/dm–3.
2. Calculate the concentration of FeSO4 solution in g/dm–3.
3. The number of water of crystallization (X) in more of FeSO 4.XH2O if 3.2 g of
FeSO4.XH2O was dissolved in 1 dm3.
4. Why should FeSO4 be acidified?
5. Identify the oxidizing and reducing agents in the reaction.
Page 29 of 41

Unit Objectives (please state or describe)

Lab Report (the space provided below is for experimental report and general answer to
questions)
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For Office Use

EXPERIMENT 8
TITLE: DETERMINATION NUMBER OF MOLECULES OF WATER OF
CRYSTALLIZATION IN FeSO4.XH2O USING A STANDARD
SOLUTION OF KMnO4
Aims and Objectives
i.) To learn about reactions involving oxidizing and reducing agents.
ii.) To determine the number of molecules of water of crystallization of an iron salt.

Theory
Fe2+ ion in hydrated iron (II) tetraoxosulphate (VI) reacts with permanganate (MnO )
ions in acid solution according to the equation;
5Fe2+ + MnO + 8H+  5Fe3+ + Mn2+ + 4H2O

Fe2+ is oxidized to Fe3+ while the Mn in MnO is reduced to Mn2+. If a standard solution
of MnO is used in titrating a FeSO4.XH2O solution, the concentration of the latter may
be determined. From this result, the mass of anhydrous FeSO 4 and of water are
determined. X ... the water of crystallization is given by:
X=

Equipments and Reagents

7 g/250 cm3 of hydrated salt, 0.5 mol/dm3 H2SO4, 250 cm3 volumetric flask, 20/25 cm3
pipette and burette, 0.02 mol/dm3 KMnO4 solution.

Procedure
Weigh accurately approximately 7 g of the hydrated salt and make up to 250 cm 3 in a
beaker using the 0.5 mol/dm3 H2SO4 solution provided. Stir gently to dissolve the salt.
Transfer the solution to a clean 250 cm3 volumetric flask. Rinse the beaker twice with 5
cm3 portions of distilled water and transfer the washings to the volumetric flask. Make up
the volume (250 cm3) with distilled water. Stopper the flask and shake well to
homogenize the solution. Pipette 25 cm 3 (or 20 cm3) of this solution into a clean conical
flask and titrate against 0.02 mol/dm 3 KMnO4 solution from the burette till a permanent
pink colour is obtained.
From your results, calculate;
a.) The concentration of the solution in mol/dm3.
b.) The mole of Fe2+ present in the 250 cm3 of solution.
c.) The mass of both FeSO4 and of water in the hydrated salt and hence X in the formula
FeSO4.XH2O.
Page 32 of 41

WORKSHEET
Date:_____________________
Experiment Number:_____________
Experiment Title:__________________________________________________________
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Unit Objectives (please state or describe)
(i) ____________________________________________________________________
(ii) ____________________________________________________________________
(iii) ___________________________________________________________________
(iv) ___________________________________________________________________
(v) ____________________________________________________________________

For Office Use

EXPERIMENT 9
TITLE: STANDARDIZATION OF AMMONIUM FERROUS SULPHATE USING
K2Cr2O7
Aims and Objectives
i.) Learning to do oxidization titration correctly.
ii.) Learning to calculate the concentration of solution from titration data.

Theory
Like KMnO4, K2Cr2O7 is also used as an oxidizing agent in titration involving iron (II)
salts. Unlike KMnO4, K2Cr2O7 is used with chlorides. K 2Cr2O7 has the problem of
difficulty in judging the colour change quantitatively unless an indicator is added. This is
because, the Cr–3 salt produced is deep green in colour and effectively masks the colour
of any excess of potassium dichromate, which cannot act (like potassium permanganate)
as its own indicator.

The indicator used for titration involving K 2Cr2O7 is diphenylamine. Its solution in
concentrated K2SO4 has no influence on the colour of the mixture, but when oxidized by
a slight excess of K2Cr2O7, it produces an intensely coloured blue compound. Phosphoric
acid is added to present the iron (II) ions during the titration of an iron (II) salt from
oxidizing the diphenylamine prematurely, i.e. before the K2Cr2O7 is in excess.

Equipments and Reagents

a.) 1 burette 50 cm3
b.) 1 pipette 25/20 cm3
c.) 3 conical flask 250 cm3 and 50 cm3
d.) 3 beakers 250 cm3 each
e.) 1 measuring cylinder (10 ml)
f.) Solution of 1 g diphenylamine in 50 cm3 of concentrated H2SO4
g.) Phosphoric acid in ratio of 1:2 with distilled water
h.) 0.1M solution of ammonium ferrous sulphate (acidify with 50 cm 3 concentration
(H2SO4)
i.) 0.01M solution of K2Cr2O7

Procedure
– Make a solution of 1 g of diphenylamine in 50 cm 3 of concentrated H2SO4 dilute a
given volume of phosphoric acid in the ratio of 1:2 with distilled water.
– To 25 cm3 of 0.1M ammonium ferrous sulphate add one drop of the diphenylamine
solution and 5 cm3 of phosphoric acid.
– Titrate with K2Cr2O7 solution till the mixture changes from green to intensive blue
colour.
– Repeat the titration 2 more times.

Questions
1. Write a balanced equation for the reaction
2. Tabulate your burette reading and calculate the average volume of the K 2Cr2O7
used.
3. Calculate the concentration of ammonium ferrous sulphate in mol/dm3.
4. Calculate the concentration of ammonium ferrous sulphate in g/dm 3. Percentage
purity of ammonium ferrous sulphate if 6.5 g of the impure sample were used for
the preparation of the solution.
Page 35 of 41

Unit Objectives (please state or describe)

Post Lab Activities (please, refer to the questions in the manual and provide answers)
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For Office Use

EXPERIMENT 10
TITLE: ANALYSIS OF A SIMPLE DRUG (ANTACID)
Aims and Objectives
i.) To determine active ingredients in a drug sample using titrimetry.
ii.) Learning to calculate concentration of active ingredients from bulk samples.

Theory
Antacids are drugs taken to relieve the effect of excess acids resulting from indigestion
and other causes. As a result, they are principally weakly acidic or slightly basic.
Compounds with these properties include salts of weak acids and strong bases such as
silicates, carbonates or hydrogen carbonates and weak acids that may be easily
protonated. In this experiment, you will be required to determine the type and amount of
the active ingredients in the given tablets.

The tablets supplied contain sodium salt of tetraoxocarbonate (IV) acid or the
hydrogentrioxocarbonate (IV) ion. These are distinguished by their action on Ca 2+ ions.
Whereas CaCO3 is insoluble, Ca(HCO3)2 is soluble but easily precipitated on heating.
The amount of ions resent may be estimated by titrating with a standard acid solution.

Equipments and Reagents

CaCl2, drug sample, HCl, methyl orange, beakers, centrifuge, volumetric flasks, burette,
pipette

Procedure
Crush about half a tablet of the drug in beaker. Pour in 5 cm 3 of distilled water and swirl
gently to dissolve. Centrifuge the contents of the beaker to sediment un–dissolved
particles. Transfer the clear solution above to a test tube (be careful not to disturb the
sediments). To the clear solution add few drops of CaCl 2 solution observe and report
what happens. If nothing happens, warm the solution gently on a Bunsen flame. Again
observe and report what happens. Now put seven tablets of the drug into a clean beaker.
Add about 100 cm3 of distilled water and stir gently until dissolved. Transfer the contents
of the beaker to a 250 cm3 volumetric flask. Wash the beaker twice with 10 cm 3 portions
of distilled water and transfer the washings to the standard flask. Make the volume up to
the mark and shake properly to homogenize the solution. Titrate 25 cm 3 portions of this
solution with 0.1 mol/dm3 solution of HCl to a methyl orange endpoint. Record your
results.

Questions
From the results;
1. Identify the sodium salt present in the antacid.
2. Determine the concentration (in mol/dm3) of the active ingredient in the solution
prepared.
3. Calculate the milligrams of the ingredient per tablet of the drugs.
Page 38 of 41

For Office Use

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