International Islamic University Chittagong (IIUC)

Department of Electrical and Electronic Engineering

Kumira, Sitakunda, Chittagong, Bangladesh

Lab Manual

CHEM-2304
Chemistry Sessional

Chemistry Lab
Program: B.Sc. Engg. (EEE)
International Islamic University Chittagong (IIUC)
Department of Electrical & Electronic Engineering
Syllabus Contents:

List of Experiments: Names:

Experiment No: 1 Introduction to chemistry laboratory and use of equipments:

different units of concentrations, primary and secondary standard
solutions, titrations, qualitative and quantitative analysis etc.

Experiment No: 2 Acidimetri-Alkalimetri: Determination of the strength and amount

of hydrochloric acid.

Experiment No: 3 Preparation of sodium oxalate solution and standardization

of potassium permanganate solution.

Experiment No: 4 Determination of ferrous ion (Fe2+) with standard potassium

permanganate solution.

Experiment No: 5 Preparation of standard potassium dichromate solution and

standardization of sodium thiosulphate solution.

Experiment No: 6 Determination of copper by iodometrically with standard sodium

thiosulphate solution.

Experiment No: 7 Determination of calcium in calcium carbonate.

Experiment No: 8 Conduct metric titration of strong acid with strong base.

Experiment No: 9 Conduct metric titration of weak acid with strong base.

Experiment No: 10 Determination of PH of a solution: PH metric titration of a strong

acid with strong base .

Recommended Books:

Text Books:

1. J Mendham – RC Denney : Textbook of Quantitative and Chemical Analysis

2. S.K Hazari : Principle of Qualitative and Quantitative Chemical
Analysis
 Department of Electrical & Electronic Engineering

CONTENTS

CHEM-2304: Chemistry Sessional

Experiment No. Experiment Name Page No.

Experiment 01 Introduction to chemistry laboratory and use of equipments: 6-14

different units of concentrations, primary and secondary standard
solutions, titrations, qualitative and quantitative analysis etc.

Experiment 02 Acidimerti-Alkalimetri: Determination of the strength and amount 15-17

of hydrochloric acid.

Experiment 03 Preparation of sodium oxalate solution and standardization of 18-19

potassium permanganate solution.

Experiment 04 Determination of ferrous ion (Fe2+) with standard potassium 20-21

permanganate solution.

Experiment 05 Preparation of stardard potassium dichromate solution and 22-23

standardization of sodium thiosulphate solution.

Experiment 06 Determination of copper by iodometrically with standard sodium 24-25

thiosulphate solution.

Experiment 07 Determination of calcium in calcium carbonate. 26-28

Experiment 08 Conductometric titration of strong acid with strong base. 29-33

Experiment 09 Conductometric titration of weak acid with strong base. 34-38

Experiment 10 Determination of PH of a solution: PH metric titration of a strong 39-44

acid with strong base.

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 LESSON PLAN
Weeks No of Lab No: Time
Contact Topics to be covered
Department of Electrical & Electronic Engineering
Hours Subject Name: Chemistry Sessional
Subject Code: CHEM-2304
Semester: Third
01 02 Experiment-1 Introduction to chemistry laboratory and use of 1.40 Hours
equipments: different units of concentrations, primary
and secondary standard solutions, titrations, qualitative
and quantitative analysis etc.

02 02 Experiment-2 Acidimetri-Alkalimetri: Determination of the strength 1.40 Hours

and amount of hydrochloric acid.

03 02 Experiment-3 Preparation of sodium oxalate solution and 1.40 Hours

standardization of potassium permanganate solution.

04 02 Experiment Test (Lab No: 1,2,3) 1.40 Hours

05 02 Experiment-4 Determination of ferrous ion (Fe2+) with standard 1.40 Hours

potassium permanganate solution.

06 02 Experiment-5 Preparation of standard potassium dichromate solution 1.40 Hours

and standardization of sodium thiosulphate solution.

07 02 Experiment-6 Determination of copper by iodometrically with 1.40 Hours

standard sodium thiosulphate solution.

08 02 Experiment Test (Lab No: 4,5,6) 1.40 Hours

09 02 Experiment-7 Determination of calcium in calcium carbonate. 1.40 Hours

10 02 Experiment-8 Conductometric titration of strong acid with strong 1.40 Hours

base.

11 02 Experiment-9 Conductometric titration of weak acid with strong 1.40 Hours

base.

12 02 Experiment-10 Determination of PH of a solution: PH metric titration 1.40 Hours

of a strong acid with strong base.

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13 02 Experiment Test (Lab No: 7,8,9,10) 1.40 Hours

14 02 Quiz Test 1.40 Hours

Distribution of Marks
COURSE: CHEMISTRY SESSIONAL
COURSE CODE: CHEM-2304

1.Class Attendence 10
2. Class Performance 10
3. Lab Report 20
4. Quiz Test 30
5. Experiment Test 20
6. Viva voce 10

Experiment No. 01
INTRODUCTION OF CHEMISTRY LAB

Chemical analysis is carried out to understand the composition of the materials. This will enable to
assess the properties of materials and if necessary, modify the properties for technical and scientific
applications. Chemical analysis is the resolution of a chemical compound into proximate or
ultimate parts. Traditional manual chemical analysis is divided into two types.

a. QUALITATIVE ANALYSIS: It deals with the identification and confirmation of the nature of the
substance or impurities present in a given sample.

b. QUANTITATIVE ANALYSIS: It deals with the estimation of, how much of each component or of

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specified components, are present in a given sample, including in trace quantities. The substance
determined is analyte and the minor or the trace quantities are impurities. The complete quantitative
analysis consists of five steps: sampling, dissolution of the sample, conversion of the analyte into a
form suitable for measurement, measurement, calculation and interpretation of data.
Quantitative chemical analysis is further divided into two types:
a. VOLUMETRIC ANALYSIS: It is based on a chemical reaction and the calculations are on the simple
stoichiometric relations of chemical reactions. It is a quantitative chemical analysis by measure,
which consists essentially in determining the volume of solution of accurately known concentration
required to react quantitatively with solution of substance being determined. The weight of the
substance to be determined is then calculated from the volume of the standard solutions and the known
laws of chemical equivalence/ stoichiometry. The standard solution is usually added from a graduated
glass vessel called a burette. The process of adding the standard solution until the reaction is just
complete is termed as a titration and the substance to be determined is said to be titrated. Hence, this
is also referred to as titrimetric analysis. The point at which the titration is completed is called the
equivalence point or the theoretical (stoichiometric) endpoint. The completion of the titration should,
as a rule, be detectable by some change, unmistakable to the eye, produced by the standard solution
itself or more usually by the addition an auxiliary agent, known as indicator. The indicator should give
a clear visual change in the solution being titrated. In the ideal titration, the visible endpoint will
coincide with the stoichiometric or theoretical endpoint. However in practice, a very small difference
usually occurs, referred to as titration error. Volumetric analysis, which involves the accurate
measurements of volume of solutions, though one or two weighing may also be needed. The indicator
is a chemical substance and choice of the indicator depends on the nature of the chemical reaction.
Volumetric methods need simpler apparatus and the processes are quickly performed. They require a
balance for weighing, calibrated measuring vessels like burettes, pipettes and volumetric flasks and
substances of known purity for the preparation of standard solutions.

b. GRAVIMETRIC ANALYSIS: Unlike volumetric analysis where measurements of volumes are

involved, gravimetric method involves separation of the analyte into a solid form as precipitate. The
measurement step in gravimetry is weighing. The element or a definite compound of the element in
as pure form as possible, is isolated and weighed. The weight of the element or compound may then
be readily calculated from knowledge of the formula of the compound and the atomic weights of the
constituent elements. The isolation of the required species is achieved by precipitation methods,
volatilization, evolution methods or electro analytical methods.

The advantage of gravimetric method over volumetric analysis is that the constituent may be seen
and examined for the presence of impurities. A correction can be applied if necessary. The
disadvantage of gravimetry is that it is more time consuming compared to volumetric analysis. Of
the two methods, gravimetric analysis is accurate, but volumetric analysis is much more readily and
quickly carried out. The error allowed in volumetric analysis is 0.2%.
ESSENTIAL CONDITIONS FOR ACCURATE TITRIMETRY
1. Clean glass apparatus must only be used in titrimetric analysis. Glass apparatus must be free from
grease and thoroughly rinsed with distilled water and dried in an oven before use. Graduated apparatus
need not be dried in oven, as they may cause error due to expansion.
2. The stoichiometric equation governing the reaction must be known.
3. The reaction should be practically instantaneous or proceed with sufficient speed. Addition of a

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 suitable catalyst may help to increase the speed of the reaction. The reaction must go to completion,
without any complicating side reactions.
4. There must be some marked change in some physical or chemical property of the titrate to assess
the completion of the reaction (usually an indicator is employed).
5. An indicator should be available, which should sharply define the end point of the reaction.
6. The standard solution must not alter in its strength during the period of experimentation. The
solution must be stable to light, atmosphere and must not react with the solvent or containers.
7. The balance must be accurate, stable, and sensitive and give the same result in successive
weighing. Calibrated weights must be used. If a digital balance is used, its operation must be fully
understood and proper care be taken to obtain accurate results to the specified decimals.
TERMS USED IN VOLUMETRIC ANALYSIS
a. TITRATION: It is a process of adding one solution from the burette to another known volume of
solution in a conical flask, in order to complete the chemical reaction. Out of the two solutions
one must be standard i.e., whose concentration is known by preparation or by previous
standardization.
b.TITRANT: The reagent being added through a burette is called as titrant.
c.TITRATE: The substance being titrated in the reaction vessel is termed as Titrate. However,
these terms titrant and titrate are relative.
d. EQUIVALENCE POINT or STIOCHIOMETRIC END POINT: It is the point at which the
amount of reagent (titrant) and substance (titrate) being determined are stoichiometrically
equivalent according to the equation representing the chemical reaction or it is the exact stage at
which the chemical reaction involved in the titration is just complete.
e. INDICATOR: The substance which helps in the visual detection of the completion of the reaction
in the titration is known as indicator.
f. PIPETTE: A glass apparatus with which a fixed volume of solution as marked on the pipette can
be delivered. It should be previously rinsed with the solution of titrate
Solution is drawn by suction above the mark and the end is closed with pointing finger tightly,
with three fingers on one side and thumb on the other side. By slow release of pointing finger,
the level is adjusted to the mark and transferred into the titration vessel.
Care must be taken to see that air bubbles are not present while drawing solution and the
solution drop in the nozzle is never released by blow off.

g. BURETTE: Burettes are long cylindrical tubes of uniform bore throughout the graduated
length with a closed bottom with stop cock and nozzle at the end. Titrant is filled into the burette
including the nozzle and clamped to the stand vertically for five minutes before use, to eliminate
air bubbles, if any. Initially the burette is filled with titrant up to its zero mark. The stop cock can
release solution as a continuous flow, but gentle operation will enable drop wise addition.
Burette releases sufficient measured volume of solution into the titration vessel till the reaction
is complete as indicated by change in color of indicator. The volume released can be noted
immediately as titre value. The reading of the lower meniscus coinciding with graduation will be
taken as the burette reading. Burette should be fixed in stand and clamp vertically during and after
use.
h. CONICAL FLASK: It is the reaction vessel containing titrate and indicator solution in distilled
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 water. It should be rinsed with distilled water only before and after each titration.
i. WEIGHING BOTTLE: This is used to weigh a required quantity of specified solid for
preparing standard solutions. The difference in weights before and after use gives the weight of
the substance transferred.
j. ANALYTICAL BALANCE: It is a two pan balance with graduated beam holding
aluminum rider.
It is closed on all sides to prevent air disturbances and all weighings must be carried out while
closing these windows. Gentle lifting of the bottom knob will lift the beam to give f r ee
oscillations of the attached pointer within the scale. Before weighing, it should show equal
oscillations on both sides of the scale failing which, the help of teacher in charge may be sought.
No part of balance must be touched, while the beam is raised with knob and it is on free
oscillations. Usually the balance is supplied with a weight box having weights 200g to 1 g and
fractional weights of 500mg to 10mg. The weights should be handled with forceps only otherwise
errors in weights are likely to interfere. Its accuracy is up to 0.1 mg. i.e., to fourth decimal place
of a recorded weight. Digital balance can also be used for specific decimal places. A digital
balance gives direct reading of weight to specified decimal paces on the panel.
k. MEASURING CYLIDER OR JAR: This is a graduated cylindrical glass vessel to draw
approximate volumes of solution.
l. VOLUMETRIC FLASK: This is a stoppered glass vessel with flat bottom and pear shape
with a long narrow neck containing a thin line mark etched on the neck. The volume specified on
the flask is up to the mark only. This is used to prepare solutions with definite concentrations.
m. PORCELAIN TILE: A ceramic plate of 6”x6” size glazed white on one side and placed under
the conical flask or any titration vessel during titration, which helps for better detection of color
change at the equivalence point.
n. END – POINT: The point at which the colour change of the indicator is visible is called the
end point. Since this depends upon the sensitivity of the eye, the appearance of the first change
in the faint color must be noted carefully, lest errors should creep into the measurement of
volumes of solutions. A glazed white porcelain tile or a white paper in the back ground of the
titration vessel will improve the visibility of the color change in observing and recording the end
point accurately.
o. TITRATION ERROR: Ideally, the visible end – point and the equivalence point should
coincide, but in practice there is always a difference between the two, this difference being
called the titration error. It is because the color change of indicator takes place only after the
completion of the chemical reaction and addition of small excess of the titrant. Also it is possible
that the indicator itself may also cause or join the chemical reaction.
Many errors occur due to analyst or method or reagent or uncalibrated glassware and interference
of the indicator. To avoid these errors statistical treatment of the titration values is necessary.
Hence,‘Most Probable value’ is taken as the result.

MOST PROBABLE VALUE: Even when a quantity is measured with possible accuracy, the results
of a successive observation differ among themselves. The average value of these results is taken as most
probable value. Hence, it is not a true value.
ABSOLUTE ERROR: The difference between observed or measured value to a true or most probable
value is known as absolute error. It is measure of accuracy.
ACCURACY: It is the concordance between measured value and most probable value or true value.
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RELATIVE ERROR: It is the absolute error divided by true or most probable value. It is
usually expressed in terms of % ppm.

……………………………….(1.1)

…………………………[(1.1)a]
MEAN DEVIATION: It is an agreement between a series of results. It can be evaluated by
determining arithmetic means of the results, then calculating the deviation of each individual from the
mean, finally dividing the sum of the deviations by the number of measurements.

Table- 1.1 : Mean deviation calculation

Results Deviations
48.32 0.04
48.36 0.08
48.23 Mean = 0.05 Mean Deviation =
48.11
48.38 0.17
0.10
241.40 0.44

RELATIVE MEAN DEVIATION: It is the mean deviation divided by the mean. It is expressed in
% or ppm.
Relative Mean Deviation = ………………………………(1.2)

=
……………………………….[(1.2)a]
It is a measure of Precision.

PRECISION: Precision is a measure of reproducibility of measurements.

If the values are accurate, they may be precise, but if they are precise, they may not be
accurate.
STANDARD DEVIATION: It measures the closeness of the results with the mean. Smaller the
Standard deviation, more closely are the results to the mean value.

…………………………..(1.3)
Where = individual measurements

= Average of the results.

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 N = Number of Measurements.
RELATIVE STANDARD DEVIATION (RSD): It is a measure of the quality of the sample. Large
the RSD, shows the poor the quality of the sample.

……………………………..(1.4)
STANDARD SOLUTION: A solution of known strength is called as standard solution. It is prepared by
dissolving a definite weighed amount of the substance in a small volume of solvent in a volumetric flask
of prescribed volume. It is dissolved and made up to the mark in the volumetric flask in the total volume
being as stipulated on the volumetric flask. Later it is thoroughly made homogeneous before use and
every reuse by shaking for uniformity in concentration.

PRIMARY STANDARD SUBSTANCE: A Primary Standard Substance should satisfy the

following requirements.
a. The substance used as a primary standard should be available in a state of high purity and
preserved in a pure state. It is known as AnalaR or AR grade.
b. The substance should maintain its composition during storage and unaltered in air during
weighing. It should be neither oxidized by air nor effected by carbon – dioxide.
c. It should not be hygroscopic, deliquescent or efflorescent.
d. The total amount of impurities should not in general, exceed to 0.01 to 0.02%. The impurities to
the trace level must be specified to take necessary precautions to avoid possible interferences.
e. It is preferred to have high equivalent weight so that the errors in weighing are
minimum.
f. The substance should readily be soluble under the conditions in which it is employed.
In practice is difficult to be obtained and a compromise in the above ideal
requirements may be necessary.

PRIMARY STANDARED SUBSTANCES COMMONLY EMPLOYED:

In acidemetri and alkalimetri: Sodium Carbonate (Na2CO3), Borax (Na2B4O7.10H2O) and Potassium
hydrogen phthalate (KHC8H4O4).

In precipitation titrations: Sodium Chloride, Potassium Chloride etc.

In Oxidation-Reduction titrations: Potassium Dichromate, Sodium Oxalate, Arsenious Oxide etc.

SECONDARY STANDARD SUBSTANCES: Those substances which do not loose water of

crystallization such as sodium bicarbonate, ferrous ammonium sulphate, copper sulphate, silver nitrate
etc.

CLASSIFICATION OF REACTIONS IN VOLUMETRIC ANALYSIS:

For convenience sake, reactions in volumetric analysis are classified into four types. However the
classification is not strictly followed and overlap may occur.
1. Neutralization reactions (acidimetry and alkalimetry): These reactions are based on the
principle of neutralization of a free acid or free base. The free bases or those formed from salts of

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 weak acids by hydrolysis are titrated with a standard acid (acidimetry) or vice versa (alkalimetry).
The basic common reaction involves the interaction of hydrogen and hydroxyl ions to form
water molecule. Selective acid base indicators are only employed to mark the sudden change
in pH during these titrations.
2. Oxidation reduction reactions (redox reactions): These reactions involve a change in the
oxidation number or transfer of electrons amongst the reacting substances. The
standard solutions are oxidizing or reducing agents. The oxidation reduction indicator
should mark the sudden change in the oxidation potential in the neighborhood of the
equivalence point.
3. Complex formation reactions: They involve the combination of ions (other than hydrogen and
hydroxyl ions) to form a soluble, slightly dissociated ion or compound. Special
metallochromic indicators are employed here.
4. Precipitation reactions: They involve the combination of ions (other than hydrogen and
hydroxyl ions) to form a simple precipitate. No change in valancy occurs. Special
adsorption indicators help the detection of the equivalence point.
Concentration of a standard solution is generally expressed in following chemical
units.
MOLARITY: Molarity of a solution is defined as the number of gram moles of solute present in one
liter of the total solution solution.

………………..(1.5)

…………………[(1.5)a]

NORMALITY: The normality of a solution is defined as the number of gram – equivalents of solute
present in one liter of the total solution.

……………………………(1.6)

…………….......[(1.6)a]
Ppm: Parts per million (Ppm) is a better notation for expressing concentrations of trace quantities of
species present. This system is convenient for expressing the concentrations of very dilute solutions. It
specifies the number of parts of solute in one million parts of solution and is expressed mathematically
as

Ppm = w X 106/W ……………..(1.7)

where w is the number of grams of solute

and W is no of grams of solvent.

One liter of water at room temperature weighs approximately 106 mg; hence a convenient relationship
to remember is that one milligram of solute in one liter of water is a concentration of 1ppm. For even
more dilute solutions the system parts per billion (Ppb) is employed.
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and Ppb= w X 109/ W …………….(1.8)

CHEMISTRY LAB - GENERAL SAFETY

PRECAUTIONS
1. Every student entering into the lab shall wear a white apron or a protective coat, and shoe.
2.While leaving the lab ensure that all gas tap connections, electrical switches shall be kept in off
mode. All instruments must be properly shut down as per instructions of the teacher in charge.
Water taps, gas connections and fans, lights etc., may kindly be switched off when they are not
required.
3. Students are advised not to tamper electrical or gas connections and they should not touch
electrical main switches. They should seek help of the teacher or lab assistant in handling gas or
electrical connections. Any malfunction of electrical or gas connections shall immediately
be reported to the teacher in charge or lab technician.
4. All water tap connections shall be used as and when needed or be turned into off mode when not
in use. Wastage of water shall be avoided and leakage of gas or water shall be
immediately reported to lab technician or teacher. Laboratory water should not be used for
drinking purposes.
5. All waste solid materials, broken glass, filter papers etc., shall be dumped into dust bins provided.
Disposal of solutions or water or washing of apparatus shall be into the water sink only.
Insoluble solids should be put in dust bins but not in water sinks. The work tables and working
space must be kept neat, dry and clean always before, during and after experiment. Any spilling
of material should be cleaned immediately.
6. The bottles and other apparatus should not be moved from one place to
another unless instructed by teacher. Reagent bottles should be replaced to their
original position soon after use. Otherwise it becomes difficult for another user to
trace it.
7. All doors and windows must be kept open while working in the laboratory. Fans and lights
should be switched off, if they are not required.
8. Solutions containing strong acids should never be poured directly into the sink. They should be
diluted with sufficiently excess water and discharged into the nearby sink slowly.
9. A fuming cup board must be used for handling reactions involving corrosive chemicals like
concentrated acids, ammonia etc., volatile compound having foul smell and certain organic
compounds.
10. Dry alkalis and concentrated acids should never be touched with hands or spilled over on the
skin. In case it happens, the skin exposed must be washed under tap water immediately.
11. The test tubes and open vessels are to be heated with caution. The face of the
vessel being heated should not be kept towards your neighboring colleague in lab, as
the liquid inside may be ejected on to his face.
12. Heating must be done gradually and carefully. The articles, test tubes or others for
heating must be dry or wiped dry to prevent breakage.
13. The nozzles of burettes and pipettes must be protected against casual handling resulting in
breakage, as the entire apparatus becomes useless, if its nozzle is broken. If any of the equipment
supplied to you is found cracked or broken, immediately report to the lab in charge. Never handle
the apparatus carelessly or roughly as it may result in damage or breakage.
14. The glass corks of the volumetric flasks should be tied through a small thread to prevent mixing
of stoppers. Replace caps on bottles immediately after use lest they should be interchanged.
15. All electrical devices should be plugged in with a dry hand only, preferably with dry shoes.
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 16. Students should not sit on the work tables or keep hands for rest on tables for their own
safety.
17. The balance pan must be clean and dry. Chemicals should not be weighed directly on the pan of
the balance. A watch glass or paper may be used and necessary tare may be made.
18. Never return unused solutions or solids to the stock containers as they can contaminate the
stock chemicals.
19. The floor space in the laboratory shall be clean and free from spillage, broken glass or pieces,
straw, cloth pieces or paper to avoid accidents. Leave the laboratory only when your work bench is
cleaned and all the apparatus supplied to you is properly returned to the lab technician.
20. Fire buckets containing sand and water or fire extinguishers should always be available in the
lab in easily accessible places.
21. When fire originates, all gas taps must be cut off immediately.
22. In case of emergency, do not get panicky and be brave enough to handle the situation.
Medical attention should be requested immediately. If skin comes into contact with acid
solutions, it should be washed with water and sodium bicarbonate solution alternately and
continuously till skin is smoothened. Similarly exposure to caustic alkalis may be treated
with dilute acetic or boric acid solutions and water. Fire scar can be washed thoroughly with
water in a tap in the sink and a little oil or pipette be applied. If eyes come into contact with
chemicals, wash them with plenty of water and clean them with a dry fresh cloth.

INSTRUCTION TO STUDENTS

The following instructions are offered to the students for acquiring curriculum based skills in
Chemistry laboratory, since chemical analysis is a basic component in all branches of Engineering &
Technology, which will be useful in later courses of study, research and technical job requirements.
1. The student shall make himself completely familiar with the experiment he/she is about to
perform, its theory, procedure and precautions, before the beginning of the experiment.
2. This lab manual is intended to help in this aspect. Each apparatus is designed to be used in a
specific manner to give expected results. Even if the experiment is performed in a batch of two
or three, each student shall record his/her own observations separately in his observation note
book. Students are advised to familiarize themselves with each of the apparatus with the help of
this lab manual and further supporting instruction from the teacher.
3. All students should carry an exclusive observation note book and make a record of every
observation in it during experimentation immediately. They are advised to perform the experiment
in the manner prescribed in the procedure or as instructed by the teacher. If there is a doubt in
experimentation, they may consult the teacher and follow the instruction.
4. The student should read the procedure of the experiment and conduct it accordingly. For better
results, the precautions to be taken shall be adhered to strictly. Better results are not accidental and
they are due to contiguous effort.
5. Students should not use excess amount of reagents or chemicals. The quantities to be used are
prescribed in the procedure given in this manual. Sometimes use of excess reagents may lead to
adverse results, in addition to wastage of chemicals.
6. After completion of the assigned experiment and proper record of all necessary observations on the
note book, the apparatus may be returned to the in charge. Calculations shall be completed in the
observation note books to arrive at the results. The results shall be shown to the teacher and his
approval in the form of his signature must be obtained on the observation note book for
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 certification on record. Records will not be certified or evaluated unless signed observations are
submitted to the teacher.
7. Students are advised to record observations on the spot of experimentation and after approval of
the concerned teacher, prepare the record in due proforma and submit for grading in the subsequent
week. Every student shall complete the prescribed number of experiments and submit record for
certification & evaluation by the concerned teachers and Head. A student without the certified
record will not be allowed for external examination at the end of the semester.
8. If there is breakage of supplied equipment or abuse of any instrument the concerned student shall
be charged as per present price list. Hence students are advised to verify equipment/ instrument
before they obtain and give satisfactory report to lab in charge.

Experiment No: 02
ACIDIMETRI-ALKALIMETRI: DETERMINATION OF THE STRENGTH AND AMOUNT OF
HYDROCHLORIC ACID

OBJECTIVE:

The objective of this experiment is-

1. To determine the strength of hydrochloric acid.

2. To determine the amount of hydrochloric acid in given volume of solution

APPARATUS AND CHEMICALS REQUIRED:

Burette, pipette, volumetric flasks, funnel, conical flasks, wash bottle with distilled water, burette stand
with suitable burette clamp, a digital balance, anhydrous sodium carbonate AR(solid), watch glass,
methyl orange indicator solution.

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 THEORY:|

2HCl + Na2CO3 2NaCl + H2O + CO2 ……………………………. (2.1)

According to the principle of neutralization reactions, a free acid reacts with a base to form salt and
water, in which the hydrogen ions of the acid combine with the hydroxyl ions of the free base in
stoichiometric proportions, this being common for all acid- base reactions. For example, in the reaction,
two moles of hydrochloric acid react with one mole of sodium carbonate. Sodium carbonate, being a
salt of strong base sodium hydroxide and weak carbonic acid, shows residual alkaline properties and hence
can be considered as a weak base. Since it is available in pure state and satisfies all other required
conditions, anhydrous sodium carbonate is a primary standard.
Thus, the concentration of a solution of acid / base can be estimated by titrating it with a
standardized base / acid solution. One of the above solutions shall be of known concentration (standard
solution). On mixing the two solutions in the process of titration, the reaction goes to completion
instantaneously and for estimation of the unknown, the end point should be detected with a suitable
indicator, methyl orange solution here. On the addition of hydrochloric acid from burette to sodium
carbonate in conical flask, the pH of the solution slowly decreases and crosses the value of 7 at the
end point. Methyl orange solution being yellow in its color above pH 7 shows a pale pink color
at the equivalence point, which indicates the completion of the reaction. During titration, a fixed
volume of standard sodium carbonate solution taken in the titration vessel reacts with a measured volume
of hydrochloric acid at the end point indicated by the initial addition of a drop or two of methyl
orange solution giving a due colour change at the end point. Measurement of these volumes and substitution
in the stoichiometric formula gives the concentration of the unknown species i.e., hydrochloric acid here.

PROCEDURE:

PART- A: Preparation of standard sodium carbonate solution (Primary standard):

About 1.325g of AR grade anhydrous sodium carbonate solid sample is weighed accurately
and transferred into a 250ml volumetric flask through a glass funnel. The substance is dissolved
completely in a minimum amount of distilled water and the solution is made up to the mark. The
solution is made homogeneous by thorough shaking in the stoppered volumetric flask.

CALCULATIONS:
Amount of the sodium carbonate taken = …….. g
Concentration of the sodium carbonate = M
Gram molecular weight (GMW) of sodium carbonate = 106g
PART B: Determination of the concentration of the given hydrochloric acid
solution:
Page 15 of 44
 The given HCl solution is made up to the mark with distilled water (in the 100 mL volumetric flask)
and shaken well to make it homogeneous in concentration. Now, the burette is rinsed with a small volume
of given hydrochloric acid solution and the rinsed solution is discharged into the sink. The burette including
its nozzle portion is filled with hydrochloric solution supplied without air bubbles, up to the zero mark and
allowed to stand vertically for few minutes. 10 ml of the standard sodium carbonate solution is drawn
through a pipette into a 250 ml clean conical flask. To this, 10ml of distilled water, 2-3 drops of methyl
orange indicator solution are added to give a yellow color. This mixture is then titrated with the
hydrochloric acid solution run down from the burette. The contents of the conical flask are swirled
throughout the titration, till the end point is reached. The end point is determined by a change in color of
the solution from yellow to pale pink. The slightest pale pink color obtained at the end point in the white
back drop of the porcelain tile and noting the initial and final burette readings marks the end of the
titration. The difference in the initial and final readings of the burette gives the volume of HCl reacted
with
10 ml of the sodium carbonate solution taken. The same procedure of titration is repeated until
concurrent readings are obtained and all the observations are tabulated.

TITRATION TABLE-2.1:
S.No Volume of sodium Burette reading Volume of HCl rundown in
carbonate taken, in ml ml
IR FR Diff.
CALCULATIONS:
V1 = Volume of HCl consumed =
V2 = Volume of sodium carbonate taken = 10 ml

M1 = Molarity of HCl solution = ?

M2 = Molarity of sodium carbonate =

n1 = No of moles of HCl = 2 (as per the equation)

n2 = No. of moles of sodium carbonate = 1 (as per equation)

………………..( Eq: 2.1)

Concentration of the supplied HCl solution = M

The amount of hydrochloric acid present in supplied solution in the 100 ml volumetric flask
= Molarity of HCl x 36.5/10 = g

RESULT:
The amount of hydrochloric acid present in a given sample of 100ml = g

REPORT:
Page 16 of 44
1. Measure the volume of hydrochloric acid.
2. Also measure the volume of sodium carbonate properly.
3. Calculate the strength of hydrochloric acid.

DISCUSSION:

Write some important notes that we should follow at the time of doing experiment

Experiment No. 03

PREPARATION OF STANDARD SODIUM OXALATE SOLUTION AND STANDARIZATION OF

POTASSIUM PERMANGANATE SOLUTION.

OBJECTIVE:

The objectives of the experiment are –

1. To prepare standard solution.

2. To standardize the unknown solution.

Page 17 of 44
 APPARATUS AND CHEMICALS REQUIRED:

1. Burette and Pipette.

2. Conical flask and volumetric flask.
3. 2N H2SO4.
4. Na2C2O4.
5. KMnO4.
6. Distilled water.

THEORY:
The acidified solution of KMnO4 being an oxidizing agent which can be standardized by titration against a
standard solution of reducing agent like sodium oxalate. Thus KMnO4 in presence of dilute H2SO4 oxidates the
acids to CO2 and H2O in the following ways.

(i) Na2C2O4 + H2O H2C2O4 + 2NaOH

……………………………(3.1)
(ii) 2KMnO4 + 3H2SO4 + 5H2C2O4 K2SO4 + 2MnSO4 + 10CO2 ………….(3.2)

The electronic interpretations of above equations are as follows:

Oxidation reaction: 5C2O42- - 10e- 10CO2 ………………………………...[(3.2)a]

Reduction reaction: 2MnO4- + 16H+ + 10e- 2Mn2+ + 8H2O ………………[(3.2)b]

Final Reaction: 2MnO4- + 5C2O42- + 16H+ 2Mn2+ + 8H2O + 10CO2 …….(3.3)

Potassium permanganate is a versatile and strong oxidizing agent. The advantage ofKMnO 4 is that it serves
as its own indicator. The pink color being distinguishable even if the solution is very dilute. The equivalent
weight of KMnO4 is therefore 1/5 mole of molecular weight i.e 31.61 gm.

PROCEDURE:

Prepare 100 ml of 0.1N sodium oxalate (0.67g) solution by shaking well trough proper mixing and make up
to the mark of volumetric flask. Take 10 ml of sodium oxalate solution in a conical flask and add 40 ml of
2N H2SO4. Heat the solution up to 60-70 0C. Take KMnO4 solution in a burette and 2-3 drops of this solution
into sodium oxalate solution until the color disappears. Add the KMnO4 solution at moderate rate while
stirring the clear solution continuously and we make sure that the temperature is more than 60 0C. Now
continue the adding of KMnO4 solution drop wise until one drop is observed to give a definite pink color to
the solution. This is the end point of titration.

EXPERIMENTAL DATA:

Page 18 of 44
Preparation of 0.2N 100ml Na2C2O4 solution required = 1.34 gm

TITRATION TABLE -3.1:

No. of Volume of Burette Reading Mean reading

observations Na2C2O4 of volume of
solution in ml KMnO4
I. R F.R Difference
solution in ml

CALCULATION:

Calculate the strength of KMnO4 solution by using the following equation:

V1S1 = V2S2 ……………..(Eq: 3.1)

Where, V1= volume of Na2C2O4, V2 = volume of KMnO4, S1 = strength of Na2C2O4,

S2= strength of KMnO4.

RESULT:

The strength of KMnO4 solution is = ………..N

REPORT:

4. Measure the volume of oxalic acid.

5. Also measure the volume of potassium permanganate properly.
6. Calculate the strength of potassium permanganate.

DISCUSSION:
Write some important notes that we should follow at the time of doing experiment.

Experiment No: 04
DETERMINATION OF FERROUS ION (Fe2+) WITH STANDARD POTASSIUM
PERMANGANATE SOLUTION.

OBJECTIVE:

The objective of this experiment is-

Page 19 of 44
 1. To calculate the amount of Ferrous ion (Fe2+) in supplied sample.
2. The percentage of iron in any alloy can also be determined by this experiment.

APPARATUS AND CHEMICALS REQUIRED:

1. Burette and Pipette.

2. Conical flask and volumetric flask.
3. 1N H2SO4.
4. Mohr’s salt.
5. KMnO4.
6. Distilled water.

THEORY:
The acidified solution of KMnO4 being an oxidizing agent which converts Ferrous ions to Ferric ions according to
the following equation:
2KMnO4 + 3H2SO4 = K2SO4 + 2MnSO4 + 3H2O + 5[O] ……………………………...(4.1)
10FeSO4 .(NH4)2.6H2O + 5[O] + 5H2SO4 = 5Fe2(SO4)3 + 10(NH4)2SO4 + 65H2O……..(4.2)
2KMnSO4 + 10FeSO4 .(NH4)2.6H2O + 8H2SO4 = K2SO4 + 2MnSO4 + 5Fe2(SO4)3 +
10(NH4)2SO4 + 68H2O…………..(4.3)
The electronic interpretation of above equation is as follows:
Reduction Reaction: 2MnO4- + 16H+ + 10e- 2Mn2+ + 8H2O……[(4.3)a]
Oxidation Reaction: 10Fe2+ -- 10e- 10Fe3+ ……………………………..[(4.3)b]
Final Reaction: 2MnO4- + 10Fe2+ + 16H+ 2Mn2+ + 10Fe3+ + 8H2O……….(4.4)
Since the oxidation of ions from ferrous to ferric states involves loss of one electron, so the equivalent weight of
the ferrous sulphate or the Mohr’s salt is equal to its molecular weight.
One liter of normal solution of ferrous sulphate of Mohr’s salt contain one gram mole atom of iron.

PROCEDURE:
Dilute the supplied mohr’s salt sample solution with about 70 ml 1N sulphuric acid. Make up to the mark with
distilled water and shaking well through mixing. Pipette out 10 ml of the solution into conical flask and add about
20 ml 1N sulphuric acid in it. Titrate the mohr’s salt solution with standard KMnO4 solution.

EXPERIMENTAL DATA:

1000 ml 1M KMnO4 = 5mol Fe2+

Or; 1000 ml 1N KMnO4 = 55.85 gm of iron

TITRATION TABLE- 4.1:

Page 20 of 44
 No. of Volume of Burette Reading Mean reading
observations Mohr’s salt of volume of
solution in ml KMnO4
IR F R Difference
solution in ml

CALCULATION:
1000 ml 1N KMnO4 = 55. 85 gm of iron ……………..(Eq: 4.1)

RESULT:

The amount of Fe2+ in Mohr’s salt is = …………..gm/ml

REPORT:

1. Measure the volume of Mohr’s salt solution.

2. Also measure the volume of potassium permanganate properly.
3. Calculate the amount of Fe2+ in Mohr’s salt.

DISCUSSION:
Write some important notes that we should follow at the time of doing experiment.

Experiment No: 05
PREPARATION OF STANDARD POTASSIUM DICHROMATE SOLUTION AND
STANDARIZATION OF SODIUM THIOSULPHATE SOLUTION.

OBJECTIVE:

The objective of this experiment is-

Page 21 of 44
 1. To prepare standard solution.
2. To standardize the unknown solution.

APPARATUS AND CHEMICALS REQUIRED:

1. Burette and Pipette.

2. Conical flask and volumetric flask.
3. Sodium carbonate.
4. K2Cr2O7 solution.
5. Na2S2O3 solution.
6. 10% KI solution.
7. Distilled water.

THEORY:
In Iodometric titration, some oxidizing agent liberates iodine and then liberated iodine is titrated against
standard solution of a reducing agent. This principle is employed to determine the strength of sodium
thiosulphate solution. When standard solution of K2Cr2O7 retracts with KI in presence of acid , the
dichromate is reduced to green chromic salt and liberated an equivalent amount of iodine which is titrated
against sodium thiosulphate solution using strong solution as indicator when the end point reached the blue
color of starch iodo complex suddenly disappears and a pure green solution due to chromic salt is left. The
reaction is :
K2Cr2O7 + 6KI + 7H2SO4 Cr2(SO4)3 + 4K2SO4 + 3I2 + 7H2O ………………..(5.1)
The electronic interpretation of above equation is follows:
Reduction reaction: (Cr2O7)2+ + 14H+ + 6e- 2Cr3+ + 7H2O ……………………….[(5.1)a]
Oxidation reaction: 6I- -- 6e- 3I2 …………………………………..[(5.1)b]
2+ -
Final reaction: (Cr2O7) + 6I + 14H +
2Cr3+ + 3I2 + 7H2O ………………...(5.2)

PROCEDURE:
Prepare 100 ml 0.1N K2Cr2O7 solution in volumetric flask. Pipette out 10ml of standard K2Cr2O7 solution.
Dissolve about 10ml of 10% sodium carbonate solution into the conical flask. Add also 10ml of 10% KI
solution and shake well for mixing and pour 10ml of 10% HCl slowly. And add it into the conical flask. Allow
the flask in dark for about 5 minutes. Make up to the mark of supplied sodium thiosulphate solution and fiil up
the burette with it. Take out the conical flask from dark after 5 minutes, reverse the watch glass. Dilute the
solution to about 50 ml with distilled water through inner wall of the conical flask. Titrate the liberate iodine
with sodium thiosulphate solution.. Add Na2S2O3 drop wise until the brown color becomes light yellow. Add
2ml starch solution and gently shake the flask and color becomes deep blue. Wash the inside of conical flask
and complete the titration by adding Na2S2O3 solution.. At the end point the blue color of the starch into
complex will disappear and the color of the solution will become chromic green. The end point is sharp.

EXPERIMENTAL DATA:
Preparation of 0.1N 250ml K2Cr2O7

Page 22 of 44
TITRATION TABLE- 5.1:

No. of Volume of Burette Reading Mean reading

observations K2Cr2O7 of volume of
solution in ml Na2S2O3
I R F R Difference
solution in ml

CALCULATION:
Calculate the strength of Na2S2O3 solution by using the following equation:
V1S1 = V2S2 ……………………………….(Eq: 5.1)

Where, V1= volume of K2Cr2O7, V2 = volume of Na2S2O3, S1 = strength of K2Cr2O7,

S2= strength of Na2S2O3.

RESULT:

The strength of Na2S2O3 solution is = …….N

REPORT:

1. Measure the volume K2Cr2O7.

2. Also measure the volume of Na2S2O3 properly.
3. Calculate the strength of Na2S2O3.

DISCUSSION:
Write some important notes that we should follow at the time of doing experiment.

Experiment No: 06
DETERMINATION OF COPPER BY IODOMETRICALLY WITH STANDARD SODIUM
THIOSULPHATE SOLUTION

OBJECTIVE:

The objective of this experiment is-

Page 23 of 44
 1. To determine the strength of CuSO4 .5H2O and thus to determine the
amount of copper in a supplied copper salt solution.
2. This reaction also helps to study about ‘Iodometric Reaction.
3. The percentage of copper in any alloy can also be determined by this experiment.

APPARATUS AND CHEMICALS REQUIRED:

1. Burette and Pipette.

2. Conical flask and volumetric flask.
3. Sodium carbonate.
4. CuSO4.5H2O solution.
5. Na2S2O3 solution.
6. 10% KI solution.
7. KSCN or NH4SCN solution.
8. Distilled water.
THEORY:
Cupric ion reacts with iodide ion and produces free iodine. The complete reaction is as follows:
2CuSO4 + 4KI Cu2I2 + I2 …………………………………………….(6.1)
Above reaction is a redox reaction. The electronic interpretation of the reaction is-
Reduction reaction: 2Cu2+ + 2I- + 2e- Cu2I2 …………………………[(6.1)a]
Oxidation reaction: -
2I - 2e -
I2 ……………………………...[(6.1)b]
The amount of copper is then calculated by the titration of free iodine with standard sodium thiosulphate
solution.
2Na2S2O3 + I2 2NaI + Na2S4O6 …………………………....(6.2)

PROCEDURE:
Make the sample solution in 100 ml volumetric flask and make up to the mark by distilled water through
mixing well. Pipette out 10ml of the solution in conical a flask and add Na2CO3 drop wise until permanent
precipitation comes. Dissolve the precipitation by adding glacial acetic acid drop wise in conical flask. Then
add 10% of 10ml KI solution and keep in dark for two minutes. Take out the conical flask from dark after 5
minutes, reverse the watch glass. Dilute the solution to about 150 ml with distilled water through inner wall
of the conical flask. Titrate the liberate iodine with sodium thiosulphate solution.. Add Na2S2O3 drop wise
from burette until the brown color becomes light yellow. Add 2ml starch solution and gently shake the flask
and color becomes deep blue. Wash the inside of conical flask and titrate the solution by adding Na2S2O3
solution. When the color of solution will light blue then add 10% of 10ml NH4SCN and shake well. Titrate
the solution by adding sodium thiosulphate solution drop wise. At the end point the color of the solution will
become grey.

EXPERIMENTAL DATA:

2Cu2+ = I2 = 2Na2S2O3
or 1ml 1N Na2S2O3 = 1ml 1N Cu2+ = 0.06354g Cu2+
Page 24 of 44
TITRATION TABLE-6.1:

No. of Volume of Burette Reading Mean reading

observations K2Cr2O7 of volume of
solution in ml Na2S2O3
I. R F. R Difference
solution in ml

TITRATION TABLE-6.2:

No. of Volume of Burette Reading Mean reading

observations CuSO4 of volume of
solution in ml Na2S2O3
I. R F. R Difference
solution in ml

CALCULATION:
2Cu2+ = I2 = 2Na2S2O3
or 1ml 1N Na2S2O3 = 1ml 1N Cu2+ = 0.06354g Cu2+ ……………………….(Eq: 6.1)

RESULT:
The amount of copper ion (Cu2+) is =………gm

REPORT:

1. Measure the volume CuSO4.

2. Also measure the volume of Na2S2O3 properly.
3. Calculate the amount of copper.

DISCUSSION:
Write some important notes that we should follow at the time of doing experiment.

Experiment No: 07
DETERMINATION OF CALCIUM IN CALCIUM CARBONATE.

OBJECTIVE:

The objective of this experiment is-

Page 25 of 44
 1. To determine the amount of Calcium in Calcium carbonate salt..
2. The purity of Calcium carbonate can also be determined by this experiment.

APPARATUS AND CHEMICALS REQUIRED:

1. Burette and Pippete.

2. Conical flask and volumetric flask.
3. Calcium carbonate.
4. Ammonium oxalate.
5. KMnO4 solution.
6. Ammonium hydroxide solution.
7. 2N H2SO4solution.
8. Methyl Orange.
9. Distilled water.

THEORY:
(a) Standardization of permanganate: Potassium permanganate soln. is to be standardized against oxalic
acid, using Na-Oxalate as the primary standard, as Na-Oxalate possesses the required properties of the
primary standard. The ion-electron partial equation for the oxidation of oxalate ion is as follows:

–
OOC – COO– -------- 2CO2 + 2e– ……………………………………(7.1)

This oxidation occurs rapidly at slightly elevated temp. And in the presence of Mn++, which acts as a
catalyst.
(b) Estimation of calcium : Metals such as Ca, Cu, Zn, which give sparingly soluble oxalates, may be
determined by dissolving the washed ppt. in dilute H 2SO4 and titrating with standard KMnO4. This widely
used for the determination of calcium. Calcium is ppt. out as the oxalate by the addition of ammonium
oxalate soln. to a dilute soln. of the element in HCl acid, followed by neutralization of the acid with dilute
ammonia soln. The washed ppt. is dissolved in dil. H 2SO4 and then titrated with standard permanganate
solution.

CaC2O4 + H2SO4 CaSO4 + HOOC ------ COOH …………………………… (7.2)

2MnO4– + 5 HOOC - COOH + 6H+ 2Mn+ +10CO2 + 8H2O ……………. (7.3)

PROCEDURE:
Prepare 100 ml 0.1N Na-oxalate soln. using calculated amount of solute.

Use 10 ml. of this oxalate soln. Per titration. Add 30 ml. of 2N H2SO4 and carry out the titration with potassium
permanganate solution rapidly at room temp. until the first pink color appears throughout the solution. Allow
to stand for some time until the color disappears. Warm the soln. to 50oC–60oC in water bath and continue the

Page 26 of 44
titration to a permanent faint pink persistent for at least 30 seconds (Remember that you cannot back-titrate,
so approach the end point carefully). Repeat thrice. Find out the mean volume reqd. for the titration.

A blank determination is needed in most red-ox titrations for the blank, follow procedure exactly in the same
manner, except that the 10 ml. of oxalate is replaced by equal volume of distilled water. From the difference,
find the actual volume of KMnO4 soln. Hence calculate the strength of KMnO4 soln.

Quantitatively transfer the supplied Calcium sample to a 100 ml. volumetric flask, washing with distilled water
and transferring the washing into the volumetric flask. Then dilute up to the mark with distilled water and mix
to make the solution homogeneous. Transfer 20 ml. of this diluted soln.of calcium to a beaker. Add 30 ml
water and 2 drops of methyl red and then add with stirring an excess of 3% ammonium oxalate soln., (approx
150 ml) while heating the soln. to boiling. Stir well and keep the mixture warm until precipitation is complete.
Add a few drops of dil. NH4OH to neutralize the solution (color changes to yellowish). Cool, filter the ppt.
(Whatman No.40). Wash with 0.5% amm. Oxalate soln. to make it free from chloride (Test for chloride: a few
drops of washing + AgNO3 -------- white ppt.). Then wash with cold distilled water to free from oxalate (Test
a few drops of washing + CaCl2 solution ----- white ppt.

Transfer the ppt. with the filter paper into a beaker & add 40 ml 4N H 2SO4 to dissolve the ppt. Titrate the
solution with standard KMnO4 solution to a faint pink color as before (Warming may be reqd. during titration).
A blank titration is required using a filter paper & 40 ml 4N H 2SO4. Calculate the amount of calcium present
in the supplied solution.

EXPERIMENTAL DATA:
1 ml IN KMnO4  0.02004 g Calcium.

TITRATION TABLE-7.1:

No. of Volume of Burette Reading Mean reading

observations sample of volume of
solution in ml KMnO4
I. R F. R Difference
solution in ml

CALCULATION:

2KMnO4 = 5H2C2O4 = 5CaC2O4 = 5Ca

2KMnO4 = Ca ………..........................(Eq: 7.1)

2 5

Page 27 of 44
1000ml 1N KMnO4 = 1gm eq. KMnO4 = 1/5 mole KMnO4
1000ml 1N KMnO4 = ½ gm atom Ca = 40.02/2 gm Ca = 20.04 gm Ca
1ml 1N KMnO4 = 0.02004 gm Ca

RESULT:

The amount of Calcium (Ca) is =………gm

REPORT:

1. Measure the volume of sample.

2. Also measure the volume of KMnO4 properly.
3. Calculate the amount of Calcium.

DISCUSSION:
Write some important notes that we should follow at the time of doing experiment.

Experiment No-8

CONDUCTOMETRIC TITRATION OF STRONG ACID WITH A STRONG BASE

OBJECTIVE:

Page 28 of 44
The objective of this experiment is-

To determine the concentration of a strong acid solution, hydrochloric acid,

with a strong base, sodium hydroxide solution, by a conductometric titration method.

APPARATUS AND CHEMICALS REQUIRED:

Conductivity meter (with cell connected to the apparatus via jack pins provided), burette (50ml), volumetric
flask (100 ml), conical flask (100 ml), pipette (10 ml, 25 ml), beakers (100 ml), stirrer / glass rod,
hydrochloric acid solution, sodium hydroxide solution.

THEORY:

The neutralization reaction between HCl and NaOH is:

H+ + Cl- + Na+ + OH- Na+ + Cl- + H2O ………………………………..(8.1)

A measured volume of HCl solution is taken in a conductivity cell and NaOH solution is added from the
burette, when the above reaction occurs, forming feebly ionized water molecules by the combination of H +
and OH- ions. Since both the acid and base are strong, their ionization is complete. With the progress of the
titration, as the NaOH solution is gradually added, highly mobile H+ ions disappear and are replaced by less
mobile Na+ ions causing a decrease in the conductance of the solution. This trend of decrease continues till
the end point is reached, when all the H+ ions present in solution due to HCl are neutralized by combination
with OH- ions and disappear, due to addition of NaOH. Beyond end point, further addition of NaOH
solution results in gradual increase in conductance due to unreacted OH- ions and Na+ ions. At the point of
neutralization, the conductance value of the solution is thus minimum. A plot of conductance on Y-axis
measured at each addition versus volume of NaOH solution added on X-axis, gives two straight lines, the
intersection of which indicates the end point. The corresponding value of NaOH added with respect to the
intersection gives the result value.

PROCEDURE:
Part-A: Preparation of standared oxalic acid solution (Primary standared):

About 1.575g of AR grade oxalic acid solid sample is weighed accurately in a clean, dry weighing
bottle and transferred into a 250ml volumetric flask through a glass funnel. The substance is dissolved
completely in a minimum amount of distilled water and the solution is made up to the mark.
The solution is made homogeneous by thorough shaking in the stoppered volumetric flask.
Page 29 of 44
CALCULATIONS:
W1 = Weight of weighing bottle with oxalic acid = g

W2 = Weight of weighing bottle after transferring the oxalic acid = g

Amount of the oxalic acid transferred = W1–W2 = g

Concentration of the oxalic acid = x = = M

Gram molecular weight (GMW) of oxalic acid = 126g

PART B: Standardization of sodium hydroxide solution supplied:

The stoichiometric equation of the neutralization reaction between sodium hydroxide and oxalic acid is:

H2C2O4 + 2NaOH Na2C2O4 + 2H2O …………………………………(8.2)

According to the above equation, two moles of sodium hydroxide react with one mole of oxalic acid.
Exactly 10ml of standard oxalic acid solution is drawn with a pipette into a clean 250ml conical
flask, previously rinsed with distilled water. This solution is mixed with 20ml of distilled water and 2-
3 drops of phenolphthalein indicator solution. The contents of the flask are titrated with the supplied
sodium hydroxide solution taken in a burette. The contents of the conical flask are swirled throughout
the titration till the end point is reached. The end-point of titration can be identified by the color
change of the solution from colorless to pale pink. The slightest pale pink color obtained at the end
point in the white back drop of the porcelain tile and noting the initial and
final burette readings marks the end of the titration. The titration is repeated as above until concurrent
readings are obtained and all the observations are tabulated in the table given below.

OBSERVATIONS TABLE-8.1:
S. No Volume of oxalic acid taken in ml Burette reading Volume of NaOH
Initial Final rundown in ml
1
2
3

CALCULATIONS:

V1 = Volume of oxalic acid taken = V2 = Volume of NaOH rundown =

M1 = Molarity of oxalic acid = M2 = Molarity of NaOH = ?
n1 = No. of moles of oxalic acid = 1 n2 = No. of moles of NaOH = 2
……………………………...(Eq: 8.1)
Page 30 of 44
 …………………………..[(Eq: 8.1)a]
Concentration of the supplied sodium hydroxide solution = M

PART C: Conductometric titration of hydrochloric acid solution with standardized sodium

hydroxide solution.
Conductometric titrations are usually carried out by taking a solution to be titrated in a beaker kept in a
water bath at constant temperature, in which the conductivity cell is immersed. The conductivity cell is
connected to a conductivity bridge (Wheatstone bridge circuit). The titrant is added from the burette,
with continuous stirring and the stable value of conductance is measured after each addition.
The conductivity bridge instrument should be switched on 15 minutes before the start of the
experiment for a warm up. The conductivity cell should be properly connected to the instrument
through the leads and jack pins provided. The temperature knob in the bridge shall be adjusted
to room temperature and reading knob for conductance measurement shall be adjusted to a proper
value. Adjust CAL knob till the display reads 1000. These knobs should not be disturbed or altered
during entire experiment, lest erroneous results should come.
The burette including its nozzle portion is filled with previously standardized sodium hydroxide
solution, up to zero mark without air bubbles and clamped to the stand. The given HCl solution is made
up to the mark with distilled water (in the 100 mL volumetric flask) and shaken well to make it
homogeneous.
50 ml of this solution is taken in a 100 ml beaker and this beaker serving as conductivity cell with leads
is connected to Conductivity Bridge. The black platinized electrode foils should be completely immersed
in the HCl solution. The solution level shall be above the black electrode foils of the cell. After stirring
with glass rod, the reading of initial conductance (zero reading) shall be noted, after attaining
stability in reading. Small volumes of standardized sodium hydroxide solution from the burette are
added into the beaker containing HCl slowly with stirring. After every addition of NaOH, the volume
added and the conductance displayed in the meter should be noted. There will be a gradual fall in the
conductance and soon after neutralization is complete, there will be a raise in the value. All the readings
are to be tabulated.

OBSERVATIONS TABLE-8.2:

Volume of HCl solution taken = 10 ml

Temperature of the solution = oC

S. No Volume of NaOH added, Conductivity measured, mho Corrected Conductance

ml
1
2
3

Page 31 of 44
4
5
6
7
8
9
10
11
12
13
14
15

A graph is plotted to the volume of NaOH added on X-axis and corresponding corrected
conductance
measured on Y-axis and the two straight lines obtained are extrapolated to intersect each other. The
point of intersection is the point of neutralization and the corresponding volume of NaOH gives the
volume
required to neutralize the 50ml of HCl taken. The concentration of HCl is calculated as below.

CALCULATIONS:
V1 = Volume of HCl taken = 10 ml V2 = Volume of NaOH required =
M1 = Molarity of HCl = ? M2 = Molarity of NaOH =
solution
n = No of moles of HCl =1 n2 = No. of moles of NaOH =1
1

……………………………..(Eq: 8.2)

………………………….[(Eq: 8.2)a]
Concentration of the supplied HCl solution = M
The amount of hydrochloric acid present in supplied solution in the 100 ml volumetric flask =
Molarity of HCl x 36.5/10 = g
RESULT:
The amount of hydrochloric acid present in a given sample of 100ml = g

Page 32 of 44
REPORT:

1. Measure the volume of sample.

2. Also measure the volume of sodium hydroxide and oxalic acid properly.
3. Calculate the amount of hydrochloric acid in the given sample.

DISCUSSION:
Write some important notes that we should follow at the time of doing experiment.

Experiment No: 09

CONDUCTOMETRIC TITRATION OF A WEAK ACID WITH A STRONG BASE

OBJECTIVE:

Page 33 of 44
The objective of this experiment is-

To determine the concentration of a weak acid solution, acetic acid, with a strong base, sodium
hydroxide solution, by a conductometric titration method.

APPARATUS AND CHEMICALS REQUIRED:

Conductivity meter (with cell connected to the apparatus via jack pins provided), burette (50ml), volumetric
flask (100 ml), conical flask (100 ml), pipette (10 ml, 25 ml), beakers (100 ml), stirrer / glass rod, acetic
acid solution, NaOH solution.

THEORY:
The reaction between electrolytic solution of CH3COOH and NaOH is:

CH3COO- + H+ + Na+ + OH- CH3COO- + Na+ + H2O …………………..(9.1)

A measured volume of acetic acid solution is taken in a conductivity cell and NaOH solution is
added from the burette, when the above reaction occurs, forming feebly ionized water molecules by the
combination of H+ and OH- ions. With the progress of the titration, as the NaOH solution is gradually
added, highly mobile H+ ions disappear and are replaced by less mobile Na+ ions causing a decrease in
the conductance of the solution. This trend of decrease continues till the end point is reached, when all the
H + ions present in solution due to acetic acid are neutralized by combination with OH- ions due to addition
of NaOH. Beyond end point, further addition of NaOH solution results in gradual increase in conductance
due to unreacted OH- ions and Na+ ions. At the point of neutralization, the conductance value of the
solution is thus minimum. A plot of conductance on Y-axis measured at each addition versus volume of
Na. OH solution added on X-axis, gives two straight lines, the intersection of which indicates the
end point. The corresponding value of NaOH added with respect to the intersection gives the result value.
Unlike a strong acid like hydrochloric acid, acetic acid is a weak electrolyte with around
30% dissociation and hence the number or concentration of dissociated available H+ ions is
comparatively low. Hence the conductance values at zero reading are low and the rate of decrease in
conductance due to addition of NaOH solution is also low, which is clearly represented in the graph.
However, after the end point, the resultant conductance due to freely available OH- is high and a steep
raise in graph can be seen. The intersection of these two lines is also clear with corresponding volume as
the result value.

Page 34 of 44
CALCULATIONS:
W1 = Weight of weighing bottle with oxalic acid = g
W2 = Weight of weighing bottle after transferring the oxalic acid = g
Amount of the oxalic acid transferred = W1–W2 = g

Concentration of the oxalic acid= x = M

Gram molecular weight (GMW) of oxalic acid = 126g

Part B: Standardization of sodium hydroxide solution supplied:

The stoichiometric equation of the neutralization reaction between sodium hydroxide and oxalic acid is

H2C2O4 + 2NaOH Na2C2O4 + 2H2O …………………………..(9.2)

According to the above equation, two moles of sodium hydroxide react with one mole of oxalic acid.
Exactly 10ml of standard oxalic acid solution is drawn with a pipette into a clean 250ml conical flask,
previously rinsed with distilled water. This solution is mixed with 20ml of distilled water and 2-3
drops of phenolphthalein indicator solution. The contents of the flask are titrated with the supplied
sodium hydroxide solution taken in a burette. The contents of the conical flask are swirled throughout
the titration till the end point is reached. The end-point of titration can be identified by the colour
change of the solution from colourless to pale pink. The slightest pale pink colour obtained at the end
point in the white back drop of the porcelain tile and noting the initial and final burette readings marks
the end of the titration. The titration is repeated as above until concurrent readings are obtained and all
the observations are tabulated in the table given below

Page 35 of 44
OVSERVATIONS TABLE- 9.1:

S. No Volume of oxalic acid taken in ml Burette reading Volume of NaOH

Initial Final rundown in ml
1
2
3

CALCULATIONS:
V1 =Volume of oxalic acid = V2 = Volume of NaOH =
M1 = Molarity of oxalic acid = M2 = Molarity of NaOH =

n1 = No. of moles of oxalic acid =1 n2 = No. of moles of NaOH = 2

…………………………..(Eq: 9.1)

………………………….[(Eq: 9.1)a]
Concentration of the supplied sodium hydroxide solution = M

PART C: Conductometric titration of acetic acid with standard sodium

hydroxide solution.
Conductometric titrations are usually carried out by taking a solution to be titrated in a beaker kept in a
water bath at constant temperature, in which the conductivity cell is immersed. The conductivity cell is
connected to a conductivity bridge (Wheatstone bridge circuit). The titrant is added from the burette, with
continuous stirring and the stable value of conductance is measured after each addition.
The conductivity bridge instrument should be switched on 15 minutes before the start of the experiment
for a warm up. The conductivity cell should be properly connected to the instrument through the leads and
jack pins provided. The temperature knob in the bridge shall be adjusted to room temperature and reading
knob for conductance measurement shall be adjusted to a proper value. Adjust CAL knob till the display
reads
1000. These knobs should not be disturbed or altered during entire experiment, lest erroneous results should
come.
The burette including its nozzle portion is filled with previously standardized sodium hydroxide
solution, up to zero mark without air bubbles and clamped to the stand. The given acetic acid solution is
made up to the mark with distilled water (in the 100 mL volumetric flask) and shaken well to make it
homogeneous. 50 ml of this solution is taken in a 100 ml beaker and this beaker serving as conductivity
cell with leads is connected to Conductivity Bridge. The black platinized electrode foils should be
completely immersed in the acetic acid solution. The solution level shall be above the black electrode
foils of the cell. After stirring with glass rod, the reading of initial conductance (zero reading) shall be
noted, after attaining stability in reading. Small volumes of standardized sodium hydroxide solution
Page 36 of 44
 from the burette are added into the beaker containing acetic acid s l o w l y with vigorous stirring.
After every addition of NaOH, the volume added and the conductance displayed in the meter should be
noted. There will be a gradual fall in the conductance and soon after neutralization is complete, there will
be a raise in the value. All the readings are tabulated.

OVSERVATIONS TABLE- 9.2:

Volume of acetic acid solution taken = 25ml

Temperature of the solution = OC

S. No Volume of NaOH added, Conductivity measured, mho Corrected Conductance

ml
1
2
3
4
5
6
7
8
9
10
11
12
13

A graph is plotted to the volume of NaOH added on X-axis and corresponding conductance
measured on Y-axis and the two straight lines obtained are extrapolated to intersect each other. The point
of intersection is the point of neutralization and the corresponding volume of NaOH gives the volume
required to neutralize the 50ml of HCl taken. The concentration of acetic acid (HA) is calculated as below

CALCULATIONS:
V1 = Volume of HA taken = 10 ml V2 = Volume of NaOH required =
M1 = Molarity of HA =? M2 = Molarity of NaOH =
solution
n1 = No of moles of HA =1 n2 = No. of moles of NaOH =1

Page 37 of 44
 …………………………..(Eq: 9.2)

……………………………..[(Eq: 9.2)a]
Concentration of the supplied acetic acid solution = M
The amount of acetic acid present in supplied solution in the 100 ml volumetric flask = Molarity of
acetic acid x 60/10 = g

RESULT:
The amount of acetic acid present in a given sample of 100ml = g

REPORT:

1. Measure the volume of sample.

2. Also measure the volume of sodium hydroxide and oxalic acid properly.
3. Calculate the amount of acetic acid in the given sample.

DISCUSSION:
Write some important notes that we should follow at the time of doing experiment

Page 38 of 44
 Experiment No: 10

pH METRIC TITRATION OF A STRONG ACID WITH A STRONG BASE

OBJECTIVE:
The objective of this experiment is-

To Determination of concentration of a strong acid solution, hydrochloric acid with a strong base,
sodium hydroxide solution, by a pH metric titration method.

APPARATUS AND CHEMICALS REQUIRED:

pH meter with electrode, burette (50ml), volumetric flask (100 ml), conical flask (100 ml), pipette (10
ml/25 ml), beakers (100 ml), stirrer / glass rod, hydrochloric acid solution, sodium hydroxide solution,
oxalic acid AR solid

THEORY:
The neutralization reaction between electrolytic solution of HCl and NaOH is:

H+ + Cl- + Na+ + OH- Na+ + Cl- + H2O …………………………….(10.1)

A measured volume of HCl solution is taken in a 100 ml beaker in which the combined electrode
is immersed without touching the bottom and NaOH solution is added from the burette, when the above
reaction occurs, forming feebly ionized water molecules by the combination of H+ and OH- ions. Since
both the acid and base are strong, their ionization is complete. With the progress of the titration, as the
NaOH solution is gradually added, highly mobile H+ ions disappear and are replaced by less mobile
Na+ ions causing a decrease in the potential of the solution. This trend of decrease continues till the end
point is reached, when all the H+ ions present in solution due to HCl are neutralized by combination
with OH- ions and disappear, due to addition of NaOH. Beyond end point, further addition of NaOH
solution results in gradual change in potential due to unreacted OH- ions and Na+ ions. At the point of
neutralization, the pH value of the solution is constant. A plot of pH on Y-axis measured at each addition
versus volume of NaOH solution added, on X-axis gives a smooth curve and the sudden inflexion (jump
in pH) indicates the end point. The corresponding value of NaOH added with respect to the inflexion gives
the titre value.

PROCEDURE:

Part-A: Preparation of standared Oxalic acid solution.

About 0.315g of AR grade oxalic acid solid sample is weighed accurately in a clean, dry
weighing bottle and transferred into a 250ml volumetric flask through a glass funnel. The substance is
dissolved completely in a minimum amount of distilled water and the solution is made up to the
mark after complete dissolution. The solution is made homogeneous by thorough shaking in the
stoppered volumetric flask.
Page 39 of 44
CALCULATIONS:
W1 = Weight of weighing bottle with oxalic acid = g

W2 = Weight of weighing bottle after transferring the oxalic acid = g

Amount of the oxalic acid transferred = W1-W2 = g

Concentration of the oxalic acid = x = = M

Gram molecular weight (GMW) of oxalic acid = 126g

PART-B: Standarization of sodium hydroxide solution supplied:

The stoichiometric equation of the neutralization reaction between sodium hydroxide and oxalic acid is:
H2C2O4 + 2 NaOH Na2C2O4 + 2H2O ……………………………………..(10.2)
According to the above equation, two moles of sodium hydroxide react with one mole of oxalic
acid. Exactly 10ml of standard oxalic acid solution is drawn with a pipette into a clean 250ml
conical flask, previously rinsed with distilled water. This solution is mixed with 20ml of distilled
water and 2-3 drops of phenolphthalein indicator solution. The contents of the flask are titrated
with the supplied sodium hydroxide solution taken in a burette. The contents of the conical flask
are swirled throughout the titration till the end point is reached. The end-point of titration can
be identified by the color change of the solution from colorless to pale pink. The slightest pale
pink color obtained at the end point in the white back drop of the porcelain tile and noting the
initial and final burette readings marks the end of the titration. The titration is repeated as above
until concurrent readings are obtained and all the observations are tabulated in the table given
below.

OVSERVATIONS TABLE- 10.1:

S.No Volume of oxalic acid taken in ml Burette reading Volume of NaOH

Initial Final rundown in ml
1

Page 40 of 44
CALCULATIONS:
V1 = Volume of oxalic acid taken = V2 = Volume of NaOH rundown =

M1 = Molarity of oxalic acid = M2 = Molarity of NaOH = ?

n1 = No. of moles of oxalic acid =1 n2 = No. of moles of NaOH = 2

……………………………..(Eq: 10.1)

………………………….[(Eq: 10.1)a]
Concentration of the supplied sodium hydroxide solution = M

PART C: pH metric titration of hydrochloric acid solution with standardized sodium

hydroxide solution.
pH metric titrations are usually carried out by taking a solution to be titrated in a beaker kept in a
water bath at constant temperature, in which the glass electrode is immersed without touching the bottom.
The titrant is added from the burette, with continuous stirring and the stable value of pH is measured after
each addition in principle.
The pH meter should be switched on 15 minutes before the start of the experiment for a warm up.
The glass electrode should be properly connected to the instrument through the leads and jack
pins provided. The temperature knob in the instrument shall be adjusted to room temperature and reading
knob for pH measurement shall be adjusted to a proper value. The pH meter is calibrated by immersing the
electrode in a buffer solution of known pH value(usually 4.0/9.0) or it can be calculated by using proper
electronic probe of a definite known pH value.
The burette including its nozzle portion is rinsed and filled with previously standardized sodium
hydroxide solution, up to zero mark without air bubbles and clamped to the stand. The given HCl
solution is made up to the mark with distilled water (in the 100 mL volumetric flask) and shaken well to
make it homogeneous. 10 ml of this HCl solution is taken in a 100 ml beaker and this beaker serving as
the cell with leads of combined electrode connected to the pH meter. Proper care should be taken to see
that the electrode is completely immersed in the HCl solution. The solution level shall be above the black
electrode foils of the cell. After stirring with glass rod, the reading of initial pH (zero reading) shall be
noted, after attaining stability in reading. Small volumes of standardized sodium hydroxide solution
from the burette are added into the beaker containing HCl slowly with stirring. After each addition
of NaOH, the volume added and the pH displayed in the meter should be noted in the table. There will
be a gradual increase in the pH and soon after neutralization is complete, there will be a sudden jump in
the pH value. All the readings are to be tabulated.

Page 41 of 44
OBSERVATIONS:
Volume of HCl solution taken = 10ml
Temperature of the solution = oC

Pilot table: 10.2

S. No Volume of NaOH added, ml. pH measured

1
2
3
4
5
6
7
8
9
10
11

Page 42 of 44
 Table – 10.3:

S. No Volume of NaOH added, pH measured

ml.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18

A graph is plotted to the volume of NaOH added on X-axis and corresponding pH

measured on Y-axis to obtain a smooth curve through the obtained points. The steep
inflexion in pH in the curve causing a change of pH (acid to base) is the point of neutralization
and the corresponding volume of NaOH gives the volume required to neutralize the 10ml of
HCl taken. The concentration of HCl is calculated from the graphically obtained value (V2)
as below.

CALCULATIONS:
V1 = Volume of HCl taken = 10 ml V2 = Volume of NaOH required =
M1 = Molarity of HCl solution =? M2 = Molarity of NaOH =
n1 = No of moles of HCl =1 n2 = No. of moles of NaOH =1

Page 43 of 44
 …………………(Eq: 10.2)

…………….[(Eq: 10.2)a]

Concentration of the supplied HCl solution = M

The amount of hydrochloric acid present in supplied solution in the 100 ml volumetric
flask = Molarity of HCl x 36.5/10 = g

RESULT:

The amount of hydrochloric acid present in supplied solution in the 100 ml = g

REPORT:

1. Measure the volume of sample.

2. Also measure the volume of sodium hydroxide and hydrochloric acid properly.
3. Calculate the amount of hydrochloric acid in the given sample.

DISCUSSION:

Write some important notes that we should follow at the time of doing experiment.

Page 44 of 44