LORDS INSTITUTE OF ENGINEERING AND TECHNOLOGY

(Approved by AICTE, Accredited by NAAC ‘A’ Grade & NBA, Affiliated to Osmania University )
(AUTONOMOUS)
Department of Sciences & Humanities

ENGINEERING CHEMISTRY LAB MANUAL

B.E- I Year
(WITH EFFECT FROM ACADEMIC YEAR 2023-2024)
DEPARTMENT OF CHEMISTRY

Student Name:
Roll no:
Course:
Year/Sem:

Branch:

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GENERAL PRECAUTIONS TO BE TAKEN IN THE LABORATORY:
1. Never work in the laboratory unless a demonstrator or teaching assistant is present.

2. Do not throw waste such as match stems filter papers etc. into the sink. They must be thrown

into the waste jars.

3. Keep the water and gas taps closed expect when these utilities are needed.

4. Never taste any chemical unless instructed to do so and don’t allow chemicals to come in

contact with your skin.

5. While working with gases, conduct the experiment in a fume hood.

6. Keep all the doors and windows open while working in the laboratory.

7. You should know about the hazards and properties of every chemical which you are going to

use for the experiment. Many chemicals encountered in analysis are poisonous and must be

carefully handled.

8. Sulphuric acid must be diluted only when it is cold .This should be done by adding it slowly

to cold water with stirring, and not vice versa.

9. Reagent bottles must never be allowed to accumulate on the work bench. They should be

placed back in the shelves as and when used.

10. Containers in which reaction to be performed a little later should be labelled.

2
CODE OF CONDUCT:
1. Students should report to the concerned lab as per the time-table schedule.
2. Students who turn up late to the labs will in no case be permitted to perform the experiment
scheduled for the day.
3 After completion of the experiment, certification of the concerned staff in charge in the
observation book is necessary.
4. Students should bring a note book of about 100 pages and should enter the readings /
observations into the note book while performing the experiment.
5. The record of observations along with the detailed experimental procedure of the experiment
performed in the immediate last session should be submitted and certified by the staff member
in-charge.
6. The group-wise division made in the beginning should be adhered to, and no mix up of
students among different groups will be permitted later.
7. The components required pertaining to the experiment should be collected from the lab
assistants.
8. When the experiment is completed, students should clean the apparatus, carefully dispose the
leftover chemicals and disconnect the setup made by them, and should return all the
components/instruments taken for the purpose.
9. Any damage to apparatus that occurs during the experimentation should be brought to the
notice of lab in-charge, consequently, the cost of the repair or new apparatus should be brought
by the students.
10. Students should be present in the labs for the total scheduled duration.
11. Students are required to prepare thoroughly to perform the experiment before coming to
Laboratory.
12. Procedure sheets/data sheets provided to the students’ groups should be maintained neatly
and to be returned

3
INSTRUCTIONS FOR RECORD WRITING:
1. Write on the right side of page in the following order:
a) Serial number and date of performance (in the margin)
b) Name and number of the experiment as given in the list.
c) Aim of the experiment.
d) Description of the apparatus.
e) Procedure including sources of error and precautions taken to eliminate or to minimize them.
f) Inference or Result.
g) Explanation, if necessary, of any divergence in the expected result.
2. Left side of page should contain the following in their proper places.
a) Neat diagram of the main apparatus.
b) Observation in tabular form.
c) Calculation in tabular form.
d) Graph sheets and other papers to be attached.
3. Students should submit a record of the previous experiments when they come for practical
work.
4. An experiment is deemed to be complete when it is satisfactorily performed and recorded.

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VISION OF THE INSTITUTE:
Strive continuously for excellence in professional education through Quality, Innovation,
Team Work and Value creation, to emerge as a premier Institute in the State and the Nation.

MISSION OF THE INSTITUTE:

1. To impart quality professional education that meets the needs of present and emerging
technological world.
2. To strive for student achievement and success, while preparing them for life, career and
leadership.
3. To produce graduates with professional ethics and responsibility towards the
development of industry and the society and for sustainable development.
4. To ensure abilities in the graduates to lead technical and management teams for
conception, development and management of projects for industrial and national
development.
5. To forge mutually beneficial relationships with government organizations, industries,
society and the alumni.

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 PROGRAM OUTCOMES (POS)
ENGINEERING GRADUATES WILL BE ABLE TO:
S.No. Program outcomes (POs):

1. Engineering knowledge: Apply the knowledge of mathematics, science, engineering

fundamentals, and an engineering specialization to the solution of complex engineering
problems.

2. Problem analysis: Identify, formulate, review research literature, and analyze complex
engineering problems reaching substantiated conclusions using first principles of mathematics,
natural sciences, and engineering sciences.

3. Design/Development of solutions: Design solutions for complex engineering problems and

design system components or processes that meet the specified needs with appropriate
consideration for the public health and safety, and the cultural, societal, and environmental
considerations.

4. Conduct investigations of complex problems: Use research-based knowledge and research

methods including design of experiments, analysis and interpretation of data, and synthesis of
the information to provide valid conclusions.

5. Modern tool usage: Create, select, and apply appropriate techniques, resources, and modern
engineering and IT tools including prediction and modelling to complex engineering activities
with an understanding of the limitations.

6. The engineer and society: Apply reasoning informed by the contextual knowledge to assess
societal, health, safety, legal and cultural issues and the consequent responsibilities relevant to
the professional engineering practice.

7. Environment and sustainability: Understand the impact of the professional engineering

solutions in societal and environmental contexts, and demonstrate the knowledge of, and need
for sustainable development.

8. Ethics: Apply ethical principles and commit to professional ethics and responsibilities and
norms of the engineering practice.

9. Individual and team work: Function effectively as an individual, and as a member or leader
in diverse teams, and in multidisciplinary settings.

10. Communication: Communicate effectively on complex engineering activities with the

engineering community and with society at large, such as, being able to comprehend and write
effective reports and design documentation, make effective presentations, and give and receive
clear instructions.

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11. Project management and finance: Demonstrate knowledge and understanding of the
engineering and management principles and apply these to one’s own work, as a member and
leader in a team, to manage projects and in multidisciplinary environments.

12. Life-long learning: Recognize the need for, and have the preparation and ability to engage in
independent and life-long learning in the broadest context of technological change.

COURSE OUTCOMES
ENGINEERING CHEMISTRY LAB (U23CH1L1)
The experiments will make the student gain skill on:
C116.1 Estimate the amount of Ferrous ions.
C116.2 Calculate the total hardness and alkalinity of water.

C116.3 Identify the mobility of ions in strong acids and weak acids using
conductivity meter.
C116.4 Analyse cell potential of a given solution and determine the strength of
solution.
C116.5 Apply the principles of Colorimetry and estimate the rate constant.
C116.6 Demonstrate and understand the chemical kinetics of chemical reaction
and determine the amount of synthesized drug.

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 MAPPING
COURSE ARTICULATION MATRIX:

MAPPING OF COURSE OUTCOMES (CO) WITH PROGRAM OUTCOMES (PO)

COURSE TITLE : ENGINEERING CHEMISTRY LAB YEAR & SEMESTER : I YEAR I/II SEM

COURSE CODE : U22CH1L1 YEAR : 2022-23

The experiments will make the student gain skill on:

Course Outcomes (CO) Program Outcomes (PO)

1 2 3 4 5 6 7 8 9 10 11 12
Estimate the amount of Ferrous ions. 3 3 2 3 3

Calculate the total hardness and alkalinity of 3 3 2 3 3

water.

Identify the mobility of ions in strong acids 3 3 2 3 3

and weak acids using conductivity meter.
Analyse cell potential of a given solution 3 3 2 3 3
and determine the strength of solution.
Apply the principles of Colorimetry and 3 3 2 3 3
estimate the rate constant.
Demonstrate and understand the chemical 3 3 2 3 3
kinetics of chemical reaction and
determine the amount of synthesized drug.
AVERAGE 3 3 2 3 3

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 INDEX
S.NO NAME OF THE EXPERIMENT DATE PAGE FACULTY
NO SIGN
1 VOLUMETRIC ANALYSIS:

Determination of strength of Ferrous solution by

Permanganometry.

2 Determination of strength of Ferrous solution by Dichrometry

3 Water Analysis:
Determination of hardness of water by Complexometric
method using EDTA.

4 Determination of strength of Carbonates and bicarbonates

in a given mixture .
5 INSTRUMENTAL ANALYSIS
Conductometry
Determination of strength of given HCl solution
6 Determination of strength of HCl & CH3COOH in given
mixture

7 Potentiometry
Determination of strength of HCl solution
8 Determination of strength of Ferrous solution

9 Colorimetry:
Verification of Beer-Lambert‘s law and determination of
Permanganate.

10 Drug Synthesis
Synthesis of Drug (Aspirin / Paracetamol).

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VOLUMETRIC ANALYSIS
BASIC CONCEPTS OF VOLUMETRIC ANALYSIS
Chemical analysis of the compounds is carried out in two ways
1. Qualitative analysis. 2. Quantitative analysis.
Qualitative analysis shows what element a given contains. Quantitative analysis determines the
quantity of a particular component present in substance. It is carried out in two ways
1. Gravimetric analysis. 2. Volumetric analysis.
Gravimetric analysis involves the DETERMINATION of the amount of a given compound
from the results of weighing. Volumetric analysis is based on the measuring the volume of the
solution of a substance.
Terms involved in volumetric analysis:
1. Titration: The process of finding out the volume of one of the solution required to react
completely with a definite volume of one the other solution of known concentration is called
titration
2. Titrant: The solution of known strength is called titrant.
3. Titrate: The solution whose concentration is to be estimated.
4. Indicator: The reagent which indicates the endpoint or equivalent point of the titration.

The strength of concentration of a solution is expressed in the following ways:

1) NORMALITY: Number of gram equivalents of the substance dissolved per litre of the
solution is called Normality. It is denoted by N
𝒘𝒆𝒊𝒈𝒉𝒕 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒆(𝒘) 𝟏𝟎𝟎𝟎
N = 𝑮𝒓𝒂𝒎 𝒆𝒒𝒖𝒊𝒗𝒂𝒍𝒆𝒏𝒕 𝒘𝒆𝒊𝒈𝒉𝒕 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒆(𝑮𝑬𝑾) X
𝑽𝒐𝒍𝒖𝒎𝒆 𝒐𝒇 𝑺𝒐𝒍𝒗𝒆𝒏𝒕 (𝑽)(𝒎𝒍)

𝑴𝒐𝒍𝒆𝒄𝒖𝒍𝒂𝒓 𝒘𝒆𝒊𝒈𝒉𝒕
Equivalent weight =
𝒏

where ‘n’ denotes the number of H + ions in an acid, OH- ions in a base and charge of the ions in
a salt.

2) MOLARITY: Number of gram moles of a solute dissolved per liter of solution is called
Molarity. It is denoted by M
𝒘𝒆𝒊𝒈𝒉𝒕 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒆(𝒘) 𝟏𝟎𝟎𝟎
Molarity = X
𝑮𝒓𝒂𝒎 𝒎𝒐𝒍𝒆𝒄𝒖𝒍𝒂𝒓𝒘𝒆𝒊𝒈𝒉𝒕 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒆(𝑮𝑴𝑾) 𝑽𝒐𝒍𝒖𝒎𝒆 𝒐𝒇 𝑺𝒐𝒍𝒗𝒆𝒏𝒕(𝑽) (𝒎𝒍)
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VOLUMETRIC ANALYSIS

CHEMICAL ANALYSIS

1. Qualitative Analysis 2. Quantitative Analysis

Ex. Salt analysis a. Conventional Methods (Volumetric and Gravimetric)
b. Modern Method
INTRODUCTION:
Volumetric analysis or Titrimetry analysis, just as gravimetric analysis gives a quantitative
DETERMINATION of species. It involves a measurement of the volume of a solution known as
concentration (standard solution) that is required to react completely with the species to be
estimated. This method is applicable to fast reaction in solutions. Its advantages include: simple
apparatus, simple methods and lesser time with a high accuracy as compared to many other
techniques.
The Chemical Analysis which includes both, Qualitative and Quantitative, can be done using
instruments.
Since two reacting species would react in the same number of equivalents, the following
equation is established:
N1 X V1 = N2 X V2
Where N and V refer to normality and volume respectively and the subscripts refer to species 1
and 2.
Knowing the normality of one of the solutions (the standard solution) and the two reacting
volumes, the normality N of the solution under test can be determined.
DEFINITIONS:
i) Titration: The overall procedure of determining stoichiometric or equivalence point is called
titration or titrimetry .
ii) Titrant: The solution added in a titration.
iii) Titrand: The solution to which the titrant is added.
iv) End point: A point in the progress of the reaction which may be precisely located (almost
coincident with stoichiometric or equivalence point).
v) Indicator: A reagent used to indicate when the end point is reached. (In some cases, one of
the reactants serves as its own indicator (self-indicator) as in the case of titrations involving
KMnO4

11
EXPERIMENTS

12
LAB EQUIPMENTS

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EXPERIMENT (1)
PREPARATION OF STANDARD MOHR’S SALT SOLUTION, STANDARDISATION
OF POTASSIUM PERMANGANATE (KMnO4) & DETERMINATION OF FERROUS
IONS:
PART A: PREPARATION OF STANDARD FERROUS AMMONIUM SULPHATE
[FeSO4. (NH4)2SO4.6H2O] SOLUTION.

PART B: STANDARDIZATION OF KMnO4

Titration of Std. F.A.S. vs. KMnO4

S. No Volume of Standard FAS Burette Readings Volume of KMnO4
(ml) Initial Reading (ml) Final Reading (ml) Consumed (ml)

1. 20

2. 20

3. 20

Calculations:
N1V1 = N2V2
Where, N1 = Normality of Standard F.A.S =______ N
V1 = Volume of Standard F.A.S = 20 ml
N2 = Normality of KMnO4 =________?
V2 = Volume of KMnO4 = _____ (Burette reading)
N1V1 = N2V2
𝑁1 𝑉1
𝑁2 = = __________ =N
𝑉2

Normality of KMnO4 (N2) = ________N

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 VOLUMETRIC ANALYSIS
EXPERIMENT (1)
PREPARATION OF STANDARD MOHR’S SALT SOLUTION, STANDARDISATION
OF POTASSIUM PERMANGANATE (KMnO4) & DETERMINATION OF FERROUS
IONS:
AIM: To standardize KMnO4 solution using Std. FAS solution.
APPARATUS: Conical flask, Burette, Pipette, Burette stand and Dropper
CHEMICALS: H2SO4, KMnO4, FeSO4 (NH4)2SO4.6H2O (Mohr’s Salt)
PRINCIPLE: Potassium Permanganate oxidizes Ferrous Sulphate present in the Mohr’s salt in
the presence of dil. H2SO4 to Ferric Sulphate according to following chemical reaction.
2KMnO4 + 8H2SO4 + 10FeSO4 K2 SO4 + MnSO4 + 5Fe2(SO4)3 + 8H2O

PROCEDURE:
PART-A:
PREPARATION OF STANDARD FERROUS AMMONIUM SULPHATE FeSO4
(NH4)2SO4.6H2O SOLUTION
Exactly ________g of FAS is weighed out in a clean weighing bottle. It is transferred to a 100ml
volumetric flask through a funnel, and 10 drops Conc. H2SO4 is added. Add some distilled water
and shake well to make it homogenous. The solution is made up to the mark with distilled water.
PART-B:
STANDARDIZATION OF GIVEN KMnO4 SOLUTION:
Pipette out 20 ml of the prepared std. Ferrous Ammonium Sulphate solution into a clean conical
flask. Titrate with KMnO4 (taken in the burette) to a faint pink colour which persists for at least a
minute. This is the end point. (Last addition of KMnO4 should be drop wise with particular care
to allow each drop to become decolorized before the next is added). Repeat the process till at
least two concurrent values are obtained.
PART-C:
DETERMINATION OF Fe+2 IN THE GIVEN TEST SOLUTION: Pipette out 20 ml of the
given Ferrous Ammonium Sulphate solution into a clean conical flask and titrate with KMnO4
(taken in a burette) to a faint Pink colour which persists for at least a minute. This is the end
point. The process is repeated till two concurrent titre values are obtained. From the titration data
the amount of Fe2+ in the given test solution is estimated.

15
PART C:
DETERMINATION OF Fe2+ IN THE GIVEN TEST (FAS) SOLUTION
Titration: Fe2+ (Test Solution of FAS) Vs KMnO4
S. Volume of unknown / test Burette Readings Volume of KMnO4 Consumed(ml)
FAS solution) (ml)
No Initial Final (ml)

(ml)

1. 20ml 0

2. 20ml

3. 20ml

Calculations:

Test solution (FAS) VS KMnO4

For Neutralization,
N2V2 = N3V3
Where,
N2 = Normality of KMnO4 ________N(from 2nd Step)
V2 = Volume of KMnO4 _____ (Burette reading)
N3 = Normality of Test solution (FAS) _____?
V3 = Volume of Test solution (FAS) ___
𝑵𝟐 𝑽𝟐
𝑵𝟑 = = __________N
𝑽𝟑

Normality [strength] of Test FAS solution = _______N

Therefore,
Amount of iron present in the given Test solution
N3 X Equivalent weight of Fe2+
N3 X 27.92 = _______________g/litre

16
RESULT:
Strength of Test Solution (FAS) _____ N
Amount of Ferrous Ions (Fe+2) present in the given Test FAS solution ______ gms / litre

17
18
EXPERIMENT-2
DETERMINATION OF FERROUS ION BY DICHROMETRY:
PART A: PREPARATION OF STANDARD FERROUS AMMONIUM SULPHATE
[FeSO4 (NH4)2SO4.6H2O] SOLUTION

PART B : STANDARDISATION OF K2Cr2O7 SOLUTION

Standard FAS vs K2Cr2O7

Burette reading Volume of K2Cr2O7

S.No. Volume of FAS solution[ml]
Initial Final consumed [ml]

Calculations and Observation:

Normality of Standard FAS (N1)= _________N
Volume of Standard FAS (V1) = ____________ml
Normality of K2Cr2O7 (N2) = _______N
Volume of K2Cr2O7 (V2) = __________ml [burette reading from table 1]
N1V1 = N2V2
𝑵𝟏 𝑽𝟏
𝑵𝟐 = 𝑽
𝟐

Normality [strength] of K2Cr2O7 solution = _______N

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EXPERIMENT-2:
Determination of strength of Ferrous solution by Dichrometry:
AIM: To Determine the amount of ferrous ion present of the whole solution with the help of
standard solution of potassium dichromate [oxidizing agent]
APPARATUS: Beaker, burette, burette stand, pipette, conical flask, volumetric flask.
CHEMICALS: Potassium dichromate [K2Cr2O7], Diphenylamine indicator, Conc.H2SO4, and
Ferrous ammonium sulphate [Mohr’s salt]
THEORY AND PRINCIPLE: Ferrous ion is oxidized to ferric ion by potassium dichromate
in acid solution. The completion of the oxidation of reaction is marked by the appearance of
blue violet color of the diphenylamine which is used as internal indicator.
K2Cr2O7 + 4H2SO4 K2SO4 + Cr2[SO4]3 + 4H2O + 3O
[Reduction]
3 x [2Fe2SO4 + H2SO4 + O Fe2[SO4]3 + H2O]
[Oxidation]
K2Cr2O7 + 6FeSO4 + 7H2SO4 K2SO4 + 3Fe2[SO4]3 + Cr2[SO4]3 + 7 H2O

PROCEDURE:
PART A: PREPARATION OF STANDARD FERROUS AMMONIUM SULPHATE
FeSO4 (NH4)2SO4.6H2O SOLUTION.
Exactly ________g of FAS is weighed out in a clean weighing bottle. It is transferred to a
100ml standard Volumetric flask through a funnel, add 10 drops Conc. H2SO4. Add some
distilled water and shake well to make it homogenous. The solution is made up to the mark
with distilled water.
PART B: STANDARDISATION OF K2CR2O7 SOLUTION: The burette is washed with
distilled water & rinsed with K2Cr2O7 and then filled with K2Cr2O7 without any air bubbles up
to zero level. Pipette out 20ml of Std FAS solution in to a clean 250ml conical flask and add 2
drops of diphenylamine indicator. Then titrate the resulting solution with potassium dichromate
[K2Cr2O7] taken in the burette till blue violet color is obtained as end point. Repeat the titration
to get concurrent values.

Part C: Standardization of Ferrous ion:

Rinse the burette with standard K2Cr2O7 solution and take K2Cr2O7 solution up to the zero mark
of the burette. Pipette out 20ml of ferrous solution in to a 250ml conical flask and add 2 drops
of diphenylamine indicator. Titrate the resulting solution with potassium dichromate taken in
the burette till blue violet color is obtained as end point. Repeat the titration to get concurrent
values.

20
PART C: DETERMINATION of Fe+2in the given Test FAS solution:

Standard K2Cr2O7 vs given unknown [Fe+2] solution

Burette reading
Volume of K2Cr2O7
S.No. Volume of FAS [Fe+2] solution[ml]
Initial Final consumed [ml]

1
2
3

Calculation and observation:

Normality of K2Cr2O7 [N2] = _________N
Volume of K2Cr2O7 [V2] = ____________ml
Normality of Ferrous solution [N3] = _______N
Volume of Ferrous solution[V3] = __________ml
For Neutralization,
N2V2 = N3V3
𝑵𝟐 𝑽𝟐
𝑵𝟑 = = __________N
𝑽𝟑

Normality [strength] of given test FAS solution = _______N

Therefore,
Amount of Ferrous ions present in the given test FAS solution
N3 X Equivalent weight of Fe2+
N3 X 27.92 = _______________g/litre

21
RESULT:
Normality of FAS________________N
The amount of ferrous ion [Fe+2] in the given solution is _________g/litre

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23
EXPERIMENT: (3)
DETERMINATION OF HARDNESS OF WATER BY EDTA METHOD:
STRUCTURE OF EDTA

CALCULATIONS AND OBSERVATIONS

PATR A: PREPARATION OF STANDARD MgSO4

PART-B: STANDARDISATION OF EDTA

S.NO VOLUME OF STANDARD BURETTE READING Volume Of EDTA Consumed(ml)
HARD WATER SAMPLE (ml) INITIAL FINAL
1 20 (ml) (ml)
2 20
3 20

CALCULATIONS:
M1 = Molarity of standard Hard water =0.01M
V1=Volume of standard water = 20ml
M2 = Molarity of EDTA = ……...? V2 = Volume of EDTA = Burette Reading =
For Neutralization, M1V1 = M2V2
𝑴 𝟏 𝑽𝟏
𝑴𝟐 = =
𝑽𝟐

24
 WATER ANALYSIS
EXPERIMENT: (3)
Determination of hardness of water by Complexometric method using EDTA
AIM: To determine the hardness of water in given sample of water by EDTA method.
APPARATUS:
1. Conical flask
2. Burette
3. Pipette
4. Burette stand
5. Spatula
CHEMICALS:
1. Buffer solution 2. Eriochrome Black-T indicator (EBT) 3. EDTA Solution

PRINCIPLE:
EDTA forms colorless, stable complexes with Ca2+& Mg2+ ions present in water at pH 9-10.
To maintain pH at 9-10, NH4Cl & NH4OH buffer is used. Eriochrome Black-T (EBT) is used
as Indicator. Hard water sample with EBT indicator forms unstable, wine red coloured
complexes with Ca2+& Mg2+ present in water.

Ca+2 / Mg+2 + EBT pH 9-10 [Ca / Mg –EBT]

(Wine red/unstable)
The metal indicator complex is less stable than Metal-EDTA complex. So, this metal indicator
complex is titrated with std. EDTA solution. Now, colourless Metal-EDTA complex is formed
by releasing EBT indicator which is blue colour. So, the colour change from wine red to blue
indicates the end point.
[Ca / Mg –EBT] + EDTA pH 9-10 [Ca / Mg –EDTA] + EBT
(Wine red/unstable) (Stable) (Blue)

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PART-C: DETERMINATION OF HARDNESS OF WATER

S.No VOLUME OF TEST WATER BURETTE READING VOLUME OF EDTA

SAMPLE (ml)
CONSUMED (ml)
INITIAL FINAL

(ml) (ml)

CALCULATIONS:

M2 = Molarity of EDTA = (from 2nd STEP)

M3 = Molarity of water sample = ………?.
V2 = Volume of EDTA = Burette Reading =
V3 = Volume of water sample = 20ml

For Neutralization,
M2V2 = M3V3
𝑴𝟐 𝑽𝟐
𝑴𝟑 =
𝑽𝟑

M3 = ………… M

Total hardness = M3 x 100 x 1000 mg/lt or ppm = ………… ppm.

26
PROCEDURE:
PART A: PREPARATION OF STANDARD MgSO4 SOLUTION.
Exactly ________g of MgSO4 is weighed out in a clean weighing bottle. It is transferred to a
100ml standard Volumetric flask through a funnel, dissolved with Distilled water. The solution
is made up to the mark with distilled water. It is shaken well to make homogenous.
PART –B: STANDARDISATION OF EDTA:
Pipette out 20 ml standard hard water into a conical flask. To this add 3ml of buffer solution
followed by addition of 3 to 4 drops of EBT indicator. Then the solution turns to wine red in
colour. Now, titrate the wine-red solution against the EDTA taken in the burette until the
solution turns to blue colour. Note down the burette reading. Repeat the titration to get
concurrent values.

PART C: DETERMINATION OF TOTAL HARDNESS OF SAMPLE WATER:

Take 20 ml of sample water into a conical flask. To this add 5ml of buffer solution followed by
addition of 3 to 4 drops EBT indicator. Then titrate against with EDTA which is taken in
burette. Continue the titration till wine red colour to blue colour. Repeat this titration until two
concurrent values are obtained.

RESULT:
Total hardness in given sample is ………………. ppm.

27
28
EXPERIMENT: (4)
DETERMINATION OF CARBONATE AND BICARBONATE ALKALINITY IN
WATER

PART A:
PREPARATION OF 100 ml of 0.02 N Std. Na2CO3 SOLUTION:

𝒘𝒆𝒊𝒈𝒉𝒕 𝟏𝟎𝟎𝟎
𝑵𝐍𝐚𝟐𝐂𝐎𝟑 = 𝑿
𝑬𝒒𝒖𝒊𝒗𝒂𝒍𝒆𝒏𝒕 𝒘𝒆𝒊𝒈𝒉𝒕 𝑽𝒎𝒍

Weight of Na2CO3 = ___________ g

PART B: STANDARDISATION OF HCl
S.No Volume of Burette Reading Volume of HCl consumed (ml)
Na2CO3 Initial Final
(ml) (ml) (ml)
1. 20
2. 20
3. 20
CALCULATION:
Na2CO3 Vs HCl
Normality of Na2CO3 (N1) = ______
Volume of Na2CO3 (V1)
Normality of HCl (N2) = _______ ?
Volume of HCl (V2) consumed, burette reading

As per volumetric analysis,

N1V1 = N2V2
𝑵𝟏 𝑽𝟏
𝑵𝟐 =
𝑽𝟐

= ………..N

Normality (strength) of HCl (N2) =______N

EXPERIMENT: (4)
Determination of strength of Carbonates and bicarbonates in a given mixture
29
AIM: To Determine the strength of Carbonate and Bicarbonate alkalinity in water

APPARATUS: Burette, Pipette, beaker, volumetric flask, conical flask, dropper

CHEMICALS: Standard HCl, Phenolphthalein indicator, Methyl Orange indicator

PRINCIPLE: The reaction taking place may be represented by the following equations.

𝐶𝑂32- + H+ → 𝐻𝐶𝑂3−-------- (1)

𝐻𝐶𝑂3− + H+ → H2CO3 ⇌ H2O + CO2 -------- (2)
The volume of acid run down up to phenolphthalein end-point[P] corresponds to the
completion of equation (1) given above, while the volume of acid run down after [P],
corresponds to the completion of equation (2).
The total amount of acid used from the beginning of the experiment, i.e., [M]
corresponds to the total alkalinity and represents the completion of reactions shown by
equations (1) and (2). Alkalinity is generally expressed as parts per million (ppm) in terms of
CaCO3.

PROCEDURE:
PART A:PREPARATION OF Std. Na2CO3 SOLUTIONS
Weigh out accurately about ------g of (A.R.) Na2CO3 and transfer it to a clean 100 ml.
standard volumetric flask through a funnel, dissolve it in distilled water, shake well to make it
homogeneous and make up the solution to the mark .

PART B: STANDARDISATION OF HCl

Pipette out 20ml of the prepared Std. Na2CO3 solution into a clean conical flask. Add 2 drops
of methyl orange indicator. The solution becomes yellow. Titrate with the given HCl (taken in
the burette) to a initial light pink appears, this is the end point. Repeat the process of titration
till at least two concurrent values are obtained.

30
PART :C
DETERMINATION OF CARBONATE AND BI-CARBONATE ALKALINITY IN
WATER:
Volume of BURETTE READING Volume of HCl
Water consumed
sample Phenolphthalein Methyl Orange VP VM
Initial Final Initial Final
(ml) (ml) (ml) (ml)

CALCULATION:
- 2-
Phenolphthalein alkalinity (P): It is due to complete OH and ½ CO3 present in water

H2O Vs HCl,
NH2OVH2O = N HClVHCl
N H2O = N HCl VHCl
VH2O
N H2O = …….N
Phenolphthalein alkalinity (P): N H2O X 50 X 1000 =
(Where, 50= Equivalent weight of CaCO3)

Methyl orange alkalinity (M): It is due to all the ions present in water OH- & ½ CO32- , HCO3-
, hence methyl orange alkalinity is equal to total alkalinity of water)

NH2O VH2O = NHCl VHCl

N H2O = NHCl VHCl = ………..N
VH2O
Methyl orange (M)): N H2O X 50 X 1000 =

S.No Observations Alkalinity due to -

Hydroxide Carbonat CO3 2- ) Bicarbonate (HCO3 - )
(OH- )
1 P=0 M
2 P=M P or M
3 P=½M 2P
4 P>½M 2P-M 2(M-P)
5 P<½M 2P M-2P

31
PART C:
DETERMINATION OF 𝑪𝑶𝟑 2- & 𝑯𝑪𝑶𝟑− ALKALINITY IN TEST SOLUTION:
Make up the given test solution up to the mark by adding distilled water. Make the solution
homogeneous. Pipette 20 ml of test solution containing both 𝐶𝑂3−2 & 𝐻𝐶𝑂3− in a clean
conical flask.

i) Add 2 drops of phenolphthalein indicator, and titrate the sample with standard HCl. Until
the pink color just disappears-note the titre value as phenolphthalein end point [P].

ii) Add 2 drops of methyl orange indicator to the same solution and continue the titration until
color changes from yellow to red or pink. Note the titre value as [M] end point

RESULT:
Alkalinity of Carbonate in given water sample = ______ppm
Alkalinity of Bicarbonate in given water sample = ______ppm

32
EXPERIMENT: (5) ETERMINATION OF STRENGTH OF GIVEN HCL BY
CONDUCTOMETRIC TITRATION
PART A: Standardisation of NaOH
S.No Volume of HCl Burette Readings Volume of NaOH
Initial(ml) Final (ml)
1. 20
(ml) Consumed (ml)
2. 20
3. 20
As per volumetric analysis, N1V1 = N2V2
Normality of NaOH (N2) = ; Volume of NaOH consumed, (V2) = ……..ml
Normality of HCl (N1) = ………? Volume of HCl (V1) = 20 ml
𝑵𝟏 𝑽𝟏
N1V1 = N2V2 𝑵𝟐 = = …… N
𝑽𝟐

PART B: DETERMINATION OF HCl

CALCULATIONS & OBSERVATION
S.NO VOLUME OF NaOH CONDUCTANCE
1.

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

33
EXPERIMENT : (5)
Determination of strength of given HCl solution.
AIM: To determine the strength of hydrochloric acid solution by titrating against
standard sodium hydroxide solution by conductometrically.
APPARATUS: Conductivity meter, conductivity cell, burette, beaker, glass rod.
CHEMICALS: HCl & NaOH
PRINCIPLE: Conductometric titration is the volumetric analysis based upon the
measurement of the conductance during the course of titration. The number of free ions ,
charge on the free ions and mobility of the ions affects the
Conductance of an aqueous solution. When one electrolyte is added to another electrolyte
, the change in number of free ions cause a change in the conductance.
For example when a strong acid (HCl) is titrated against a strong base (NaOH),
before NaOH solution is added from the burette, the acid solution has high conductivity
due to the highly mobile H+ ions. When NaOH is added to the acid, the conductivity of
the acid solution decreases due to the neutralization of highly mobile H+ ions of the acid
-
with OH ions of the base.

HCl + NaOH → NaCl + H2O

Thus, the conductance of the solution continues to decrease until the equivalent point is
reached. Further addition of NaOH solution will increase the conductance by highly
mobile hydroxyl ions.
PROCEDURE:
PART: A-STANDARDISATION OF NaOH
Pipette out 20 ml of given 0.1N HCl solution in a clean conical flask, add phenolphthalein
indicator and titrate with NaOH taken in burette till light pink color appears. Repeat the
process till concurrent values are obtained.
PART: B - DETERMINATION OF HCl
1. Fill the burette with standard NaOH solution.
2. Take 20 ml of given HCl solution in 100 ml beaker and dip the conductivity cell in it
and measure the conductance initially.
3. Now add 1 ml NaOH from the burette drop wise.
4. After each addition, stir the solution gently by using glass rod and note down the
change in conductance.
5. Measured conductance values are recorded in the table.

34
 CALCULATION:
Normality of NaOH (N2) =
Volume of NaOH consumed, end point from graph (V2) = ……..ml
Normality of HCl (N3) = ………?
Volume of HCl (V3) = 20 ml
For Neutralization,
N2V2 = N3V3
𝑵𝟐 𝑽𝟐
𝑵𝟑 = = __________N
𝑽𝟑

Normality (strength) of HCl (N3) = …….N

The amount of HCl in the given solution = N3 X Eq. Wt of HCl

= N3 x 36.5 gms/ lt
= …………gms/lt.

35
 GRAPH:
Plot the graph between conductance against volume of base added, which consists of
2 straight lines. The intersection of 2 straight lines gives the end point as shown in the
graph below

Conductance

Volume of NaOH

RESULT:
1. The end point of the titration = …………ml
2. The strength (Normality) of given solution =………….N.
3. The amount of HCl present in the given solution = ………..gms/litre

36
37
EXPERIMENT-(6)

DETERMINATION OF HCl AND ACETIC ACID IN GIVEN MIXTURE BY

CONDUCTOMETRY:

PART A: STANDARDISATION OF NaOH:

S.No Volume of HCl Burette Readings Volume of NaOH

Initial (ml) Final (ml) Consumed (ml)
1. (ml)
20
2. 20
3. 20
As per neutralization formula
N1V1 = N2V2
Normality of NaOH (N2) = ; Volume of NaOH consumed, (V2) = ……..ml
Normality of HCl (N1) = ………? Volume of HCl (V1) = 20 ml

𝑵𝟏 𝑽𝟏
N1V1 = N2V2 𝑵𝟐 = = …… N
𝑽𝟐

PART B : DETERMINATION OF HCl AND ACETIC ACID

S.NO VOLUME OF NaOH CONDUCTANCE
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.

38
EXPERIMENT-(6)

DETERMINATION OF HCl AND ACETIC ACID IN GIVEN MIXTURE BY

CONDUCTOMETRY

AIM: To determine the end point of the titration of a mixture of acids with strong base by
conductometric method and DETERMINATION of the mixture of strong and weak acids.

APPRATUS: Burette, beaker, burette stand, glass rod, conductivity meter &conductivity cell

CHEMICALS: NaOH, HCl & CH3COOH

PRINCIPLE: Conductometric titration is the volumetric analysis based upon measurement of

the conductance during the course of titration.

When a mixture containing strong acid(HCl) and a weak acid(CH3COOH) is titrated

against a strong base(NaOH), strong acid will be neutralized first. The neutralization takes
place in the following way. First strong acid react with the strong base and then weak acid
reacts with strong base.

HCl + NaOH NaCl + H2O

CH3COOH + NaOH CH3COONa + H2O

(salt, strong electrolyte)

The conductance of the mixture falls on the addition of NaOH due to the neutralization of
highly mobile H+ ions with a base till the strong acid neutralized. Then the conductivity rises
due to the neutralization of the weak acid to the salt which is a strong electrolyte. Finally the
conductivity raised rapidly as the alkali is introduced in excess after the neutralization of the
weak acid. This is due to the presence of fast moving OH- ions.

PROCUDURE:

PART A: STANDARDISATION OF NaOH

Pipette out 20 ml of given 0.1N HCl solution in a clean conical flask, add phenolphthalein
indicator and titrate with NaOH taken in burette till light pink color appears. Repeat the
process till concurrent values are obtained.
PART B: DETERMINATION OF HCl AND ACETIC ACID
1. Fill the burette with standard 0.1N NaOH solution.
2. Pipette out 10ml of given HCl and 10ml of CH3COOH solution into clean 100ml
beaker.
3. Wash the conductivity cell with distilled water and dip it in a mixture of acids taken in
the beaker
4. Connect the conductivity cell to the conductivity meter and measure initial
conductance.

39
CALCULATIONS:
HCl vs NaOH:

Normality of NaOH (N2) =

Volume of NaOH consumed, end point from graph (V2) = ……..ml
Normality of HCl (N3) = ………?
Volume of HCl (V3) = 20 ml
For Neutralization,
N2V2 = N3V3
𝑵𝟐 𝑽𝟐
𝑵𝟑 = = __________N
𝑽𝟑

Normality (strength) of HCl (N3) = …….N

The amount of HCl in the given solution = N3 X Eq. Wt of HCl

= N3 x 36.5 gms/ lt
= …………gms/lt.

CH3COOH vs NaOH:

Normality of NaOH (N2) =

Volume of NaOH consumed 2nd end point from graph (q-p) (V2) =__________ml

Normality of CH3COOH (N4) = ________________ml

Volume of CH3COOH (V4) = _10ml

As per volumetric analysis

N4V4 = N2V2

𝑵𝟐 𝑽𝟐
𝑵𝟒 = = __________N
𝑽𝟒

N4 = _____N

Amount of CH3COOH in the given solution = N4 x Eq.Wt. of CH3COOH

= N4 x 60
= ________g/L

40
 5. Now add NaOH solution from the burette drop wise i.e. 1ml addition. After each
addition stir the solution by glass rod and note down the conductance.
6. The measured conductance values are tabulated in the table.

GRAPH: Plot the graph between conductance along Y-axis and volume of NaOH added
along X-axis. The conductometeric titration curve will be by two breaks. The first one
corresponds to the equivalent point of HCl and second to equivalent point of CH3COOH. The
graph obtained is shown below.

conductance

p q

volume of NaOH

Equivalent point of HCl = p

Equivalent point of CH3COOH = q - p

CALCULATIONS:

RESULTS:

1. The equivalent point HCl = ________________ml

2. The normality of HCl = _______N
3. The amount of strong acid(HCl) in given solution = __________g/l
4. The equivalent point of CH3COOH = ______ml
5. The normality of CH3COOH = ___________N
6. The amount of weak acid (CH3COOH) in the given solution = ________g/l

41
42
EXPERIMENT (7): DETERMINATION OF HCl BY POTENTIOMETRY
PART A: STANDARDISATION OF NaOH
S.No Volume of HCl (ml) Burette Readings Volume of NaOH Consumed (ml)

Initial (ml) Final (ml)

1. 20

2. 20

3. 20

As per neutralization formula

N1V1 = N2V2
Normality of NaOH (N2) = ; Volume of NaOH consumed, (V2)=Burette Reading= ml
Normality of HCl (N1) = …? Volume of HCl (V1) = 20 ml
𝑵𝟏 𝑽𝟏
N1V1 = N2V2 𝑵𝟐 = = …… N
𝑽𝟐

PART B : DETERMINATION Of HCl

S.NO Volume Of NaOH EMF ∆E ∆V ∆E/∆V

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

43
EXPERIMENT(7):
DETERMINATION OF HCl BY POTENTIOMETRY
AIM: To determine the strength of hydrochloric acid solution by titrating against standard
sodium hydroxide solution by using potentiometer.
APPARATUS: Potentiometer , platinum electrode, saturated calomel (reference ) electrode,
beaker, glass rod, burette and burette stand
CHEMICALS: HCl, NaOH & Quinhydrone.
PRINCEPLE: Potentiometric titration depend on measurement of emf between reference
electrode and an indicator electrode.
The quinhydrone electrode (indicator electrode) is prepared by taking
saturated solution of quinhydrone in a known quantity of strong acid whose concentration to
be determined. This electrode is combined with the calomel electrode to make the cell. The
cell representation is as shown below.
Pt, Hg,Hg2CL2/KCl (sat.)//H+ (unknown )/Q,QH2, pt
When the HCl is titrated against NaOH solution, the EMF is going on
decreasing as the H+ ion concentration decreases. After equivalent point is reached the EMF
-
values increases due to presence of OH .

The reaction between the HCl and NaOH is as shown below.

HCl + NaOH → NaCl + H2O
PROCEDURE:
PART- A: STANDARDISATION OF NaOH
Pipette out 20 ml of given 0.1N HCl solution in a clean conical flask, add phenolphthalein
indicator and titrate with NaOH taken in burette till light pink color appears. Repeat the
process till concurrent values are obtained.
PART -B: DETERMINATION OF HCl:
1. Fill the burette with standard sodium hydroxide solution(NaOH) after rinsing the
burette with NaOH upto zero mark.
2. Take 20 ml of given HCl solution into a clean beaker , and pinch of quinhydrone
power to the solution until get Saturated. Dip the platinum electrode into the
solution and combine it to saturated calomel electrode by using a salt bridge.
3. Connect the platinum electrode to the positive terminal and calomel electrode to the
negative terminal in the potentiometer.
4. Measure the EMF value initially.
5. Now add NaOH from the burette drop wise i. e., 1 ml for each addition. After each
addition, stir the solution by using a glass rod and note down the EMF values.
6. The measured EMF values are tabulated in the table.

44
CALCULATION:
Normality of NaOH (N2) =
Volume of NaOH consumed, end point from graph (V2) = ……….ml
Normality of HCl solution (N3) = ………?
Volume of HCl solution (V3) = 20 ml
As per neutralization formula
N3V3 = N2V2
𝑵𝟐 𝑽𝟐
𝑵𝟑 = = __________ = N
𝑽𝟑

Normality (strength ) of HCl solution (N3) = ……..N

The amount of HCl in the given solution = N3 x Eq. Wt of HCl

= N3 X 36.5 gms/lt. =
= ……………… gms lt.

45
GRAPH: Plot a graph between EMF against the volume of NaOH added and a curve is
obtained as shown below.

EMF

Volume of NaOH added

The point of inflexion (where the curve changes its curvature) in the curve gives the
equivalent point.
The accurate value can be obtained by plotting a graph between ∆E/∆V against the volume of
the NaOH added. The graph obtained is shown as below.

E/ V

Volume of NaOH added

RESULT:
1. The normality of HCl solution = …………N
2. The amount of HCl in the given solution = ……….gms/lt.

46
47
EXPERIMENT (8): Determination of Fe+2 by Potentiometry using KMnO4
Part A: Standardization of KMnO4
Titration of Std. F.A.S. Vs. KMnO4
S.No Volume of FAS Burette Readings Volume of KMnO4 Consumed
(ml) Initial (ml) Final (ml)
1. 20
2. 20
3. 20

As per neutralization formula

N1V1 = N2V2
Where, N1 = Normality of Std F.A.S ______ N V1 = Volume of Std F.A.S = 20 ml
N2 = Normality of KMnO4 _____ ? V2 = Volume of KMnO4 _____ Burette reading
N1V1 = N2V2
𝑵𝟏 𝑽𝟏
𝑵𝟐 = = __________ = N
𝑽𝟐

Normality of KMnO4 (N2) = ________N

PART B: DETERMINATION OF KMnO4
S.NO VOLUME OF EMF ∆E ∆𝐕 ∆𝐄/∆𝐕
KMnO4

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

48
EXPERIMENT (8):
Determination of Fe+2 by Potentiometry using KMnO4
Aim: To estimate the amount of ferrous ion present in the given solution by using
potentiometer
Apparatus: Potentiometer, platinum electrode, saturated calomel (reference ) electrode,
beaker, glass rod, burette and burette stand
Chemicals: KMnO4 , FAS(ferrous ammonium sulphate)
Principle:
Ferrous ion oxidizes to ferric ion whose concentration increases with progressive addition of
potassium permanganate and the observed EMF generally increases
5 Fe+2 → 5Fe+3+ 5e-
MnO-4 + 8H+ +8e_ → Mn+2 + 4 H2O

5 Fe+2 + MnO-4 → 5Fe+3 + Mn+2 + 4 H2O

The total reaction
2KMnO4+8H2SO4+10FeSO4→K2SO4+2MnSO4+5Fe2(SO4)3+8H2O
The cell is constructed as
Hg/HgCl2/saturated KCl/ Fe+2, Fe+3 /pt
Addition of potassium permanganate increases the observed EMF. At the end point , there is
sharp increases in EMF due to complete oxidation of ferrous ion to ferric ion
PROCEDURE:
PART A : STANDARDIZATION OF GIVEN KMnO4 SOLUTION
Pipette out 20 ml of the prepared std. Ferrous Amm. Sulphate solution into a clean conical
flask. Titrate with KMnO4 (taken in the burette) to a faint pink color which persists for at
least a minute. This is the end point. (Last addition of KMnO4 should be drop wise with
particular care to allow each drop to become decolorized before the next is added). Repeat the
process till at least two concurrent values are obtained
PART B: DETERMINATION OF Ferrous ions
• Fill the burette with standard potassium permanganate KMnO4 after rinsing the
burette with KMnO4 upto zero mark.
• Take 20 ml of given FAS solution into a clean beaker , and dip a platinum electrode
and combine it to saturated calomel electrode by using a salt bridge.
• Connect the platinum electrode to the positive terminal and calomel electrode to the
negative terminal in the potentiometer.
• Measure the EMF value initially.
• Now add from the burette KMnO4 drop wise i. e., 1 ml for each addition. After each
addition, stir the solution by using a glass rod and note down the EMF values.
• The measured EMF values are tabulated in the table.

49
CALUCLATION:
Normality of KMnO4 (N2) =
Volume of KMnO4 consumed, end point from graph (V2) = ……….ml
Normality of FAS solution (N3) = ………?
Volume of FAS solution (V3) = 20 ml
As per neutralization formula
N3V3 = N2V2
𝑁2 𝑉2
𝑵𝟑 = = __________ = N
𝑉3

Normality (strength) of FAS solution (N3) = ……..N

The amount of Fe+2 in the given solution = N3 x Eq. Wt of Fe+2

= N3 x gms/lt.
= ……………… gms lt.

50
GRAPH: Plot a graph between EMF against the volume of KMnO4 added and a curve is
obtained as shown below.

EMF

Volume of KMnO4 added

The point of inflexion (where the curve changes its curvature) in the curve gives the
equivalent point. The accurate value can be obtained by plotting a graph between ∆E/∆V
against the volume of theKMnO4 added. The graph obtained is shown as below.

E/ V

Volume of NaOH added

RESULT:
1. The normality of FAS solution = …………N
2.The amount of FAS in the given solution = ……….gms/lt.

51
52
EXPERIMENT:9
DETERMINATION OF KMnO4 BY COLORIMETRIC METHOD

Part A: Standardization of KMnO4

Titration of Std. F.A.S. Vs. KMnO4 :
S.No Volume of FAS (ml) Burette Readings Volume of KMnO4
Initial (ml) Final (ml) consumed

1. 20
2. 20
3. 20

As per neutralization formula , N1V1= N2V2

Where, N1 = Normality of Standard F.A.S =______ N
V1 = Volume of Standard F.A.S = 20 ml
N2 = Normality of KMnO4 =________?
V2 = Volume of KMnO4 = _____ (Burette reading)= ml
𝑵𝟏 𝑽𝟏
𝑵𝟐 = = __________ = N
𝑽𝟐

PART B : DETERMINATION OF MANGANESE IN KMnO4

S.No. Volume of Distilled Volume of Concentration Absorbance
water KMnO4 (or) OD Values
1.

2.

3.

4.

5.

6.

7.

8.

9.

10.

53
EXPERIMENT:9
DETERMINATION OF PERMANGANATE BY COLORIMETRIC METHOD

AIM: To Determine the amount of Permanganate present in KMnO4 Solution by

colorimetry method.

APPARTUS: Photo Colorimeter, beaker, glass rod, pipette, burette, test tubes and cuvettes.

CHEMICALS: KMnO4, Distilled water.

PRINCIPLE: Colorimeter is an instrument used to measure the intensity of light absorbed

by a substance. The relation between absorbance (A) and concentration of the solution(C) is
given by Beer-Lambert’s law.

Log Io/I = A = εCX

Where,

Io = Intensity of incident light

I = Intensity of transmitted light

ε = Molar absorption coefficient (formerly called molar extinction coefficient)

X = Thickness of cell

C = Concentration of the solution

From the equation, it is seen that, the absorbance (A) is directly proportional the molar
concentration and thickness of the cell.

PROCEDURE:
PART A:
STANDARDIZATION OF GIVEN KMnO4 SOLUTION:
Pipette out 20 ml of the prepared std. Ferrous Ammonium Sulphate solution into a clean
conical flask. Titrate with KMnO4 (taken in the burette) to a faint pink color which persists
for at least a minute. This is the end point. (Last addition of KMnO4 should be drop wise with
particular care to allow each drop to become decolorized before the next is added). Repeat the
process till at least two concurrent values are obtained.

PART B:
1. Preparation of various standard KMnO4 solutions
Now prepare a series of solutions of concentration 0.001N, 0.002N,
0.003N,0.004N,0.005N,0.006N,0.007N,0.008N and 0.009N by transferring 1ml, 2ml, 3ml,
4ml, 5ml ,6ml, 7ml, 8ml, 9ml, 10ml stock solution respectively into the test tubes and make
up to 10ml using distilled water.

54
2. Colorimetric method
• The transmittance of colorimeter is adjusted to 100% using distilled water i.e. set it
zero
• Check the absorbance of highest concentrated solution (0.1N) by using different
filters.
• Select the filter which is giving highest absorbance for the given solution and set it
to zero by using blank (distilled water).
• Now measure the absorbance of all the solutions
• In the similar way measure the absorbance of given unknown solution

Calibration graph
Plot a graph between the concentration along the X-axis and absorbance on the Y-axis to
obtain the straight line. From the graph the concentration of unknown solution is measured.

The graph which is obtained is shown a

RESULT:

The concentration of unknown sample is _______________

The Amount of Permanganate in given Solution__________________________

55
EXPERMINET – 10
PREPARATION OF ASPIRIN :
AIM : To prepare a pure sample of Aspirin
APPARATUS 1. Measuring jar 2. Beaker 3. Conical flask 4. Glass rod 5. Watch glass 6.
Funnel
CHEMICALS
1. Salicylic acid 2. Acetic anhydride 3. Conc. Sulphuric acid
BASIC PRINCIPLE:
Aspirin is an acetyl derivative of salicylic acid and prepared by the acetylation of salicylic
acid.
the acetylation of salicylic acid is carried out in two ways.
1. Acetylation with acetic anhydride in presence of an acid.
2. Acetylation in presence of acety1 chloride by using pyridine base.

Procedure:
Take 5 gms of salicylic acid in a 100 ml conical flask add about 10 ml of acetic anhydride: to
this mixture 1-2 ml of conc .sulphuric acid . Shake the solution well and the temperature of
the reaction mixture raises to 70° − 80 °C because of exothermic reaction. Maintain the
temperature of the reaction at 70° − 80 °C for about 20 minutes by heating it on water bath.
Allow the solution to cool to room temperature and pour the solution into 100 ml of cold
water taken in a 250 ml beaker with stirring (addition to water is to destroy excess of
reagent). Scratch the sides of the beaker with a glass rod to induce crystallisation and stir the
solution till complete precipitation. Filter the colourless, crystalline solid and wash it with
cold water. Spread the solid aspirin on a filter paper and dry.
Recrystallise the crude aspirin sample from a mixture of ethanol and water ( 1 : 1 ). Find the
melting point of the sample.

The melting point of aspirin reported is 130° − 135 ° C.

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Precautions:
1. Take acetyl chloride in excess as it can act as acetylating reagent and solvent.
2. Make sure that all salicylic acid is dissolved in acetylating mixture.
3. The presence of unreacted salicylic acid is checked by adding a drop of 1% ferric
chloride solution to the reaction mixture and observing the colour. Formation of
intense colour indicates the presence of unreacted salicylic acid in that case
recrystallisation is compulsory.

Pharmaceutical applications of Aspirin

RESULT:
Amount of aspirin obtained: _________gms

57
58
EXPERIMENT - 11
DETERMINATION OF RATE CONSTANT OF ACID CATALYSED HYDROLYSIS
OF METHYL ACETATE:

Observation
s.n Time Volu Burette Volume ( V∞ - log V∞ - 2.303 log
o (min me of reading of NaOH Vt) Vt V∞ −Vo
𝑣∝ −𝑣𝑡
) soluti Initi final consume
on al d (ml)
: (min-1)
taken (ml)

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EXPERIMENT - 11
DETERMINATION OF RATE CONSTANT OF ACID CATALYSED HYDROLYSIS
OF METHYL ACETATE :
Aim :
To determine the rate constant of the hydrolysis of ethyl acetate an acid as a catalyst.
Basic principle :
The hydrolysis of ester occurs according to the equation
CH3COOC2H5 + H2O→ CH3COOH + C2H5OH
The reaction follows pseudo first order kinetics
In the presence of an acid, this reaction should be of second order, since two molecules are
reacting. But, it is found to be first order. This may be explained in the following way :
The rate of the reaction is given by
dx / dt = k’ [CH3COOCH3] [ H2O ]
where k’ is the rate constant (or specific rate constant). Since water is present in large excess,
its active mass (molar concentration) virtually remains constant during the course of the
reaction. Therefore, its active mass gets included in the constant, and the above equation
reduces to :
dx / dt = k1 [CH3COOCH3]
Thus, the rate of the reaction is determined by one concentration term only (that is, by a
single power of the concentration term only). Hence, the reaction is first order.
Such reactions are also referred to as pseudo first order reactions. The progress of the reaction
(hydrolysis of ester) is followed by removing a definite volume of the reaction mixture, at
definite intervals of time, cooling it in ice, and titrating the acetic acid formed against alkali,
which has already been standardized. The amount of alkali used is equivalent to the total
amount of hydrochloric acid present originally and the amount of acetic acid formed in the
reaction. The amount of acetic acid formed (x), at definite intervals of time (t), can be
obtained. The amount of acetic acid formed, at the end of the reaction, is equivalent to the
initial concentration (a) of the ester. Suppose the volumes of the sodium hydroxide solution
(titre value) required for neutralization of 5 ml of the reaction mixture are :
(i) at the commencement of the reaction is Vo
(ii) (ii) after time (t) is Vt
(iii) (iii) at the end of the reaction is V∞
Then
x (amount of acetic acid formed after time ) is proportional to (Vt -Vo )
a (initial concentration of ester) is proportional to (V∞ -Vo )
[a – x] (concentration of ester present after time t) is proportional to

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 (V∞ -Vo ) - (Vt -Vo ) = ( V∞ -Vt )
The first order rate expression given by :
𝑎
k1 = 2.303 log 𝑎−𝑥would correspond to :
V∞ −Vo
k1 = 2.303 log 𝑣∝ −𝑣𝑡

Procedure:
DETERMINATION OF RATE CONSTANT (K1) FOR THE ACID-CATALYZED
HYDROLYSIS OF METHYL ACETATE.
1. 100 ml of given HCl (whose strength is determined in step II) solution is taken in a
stoppered reagent bottle.
2. 5 ml of methyl acetate solution is added to the HCl solution. Note the time when half of
the methyl acetate solution is added. The mixture is shaken well.
3. Pipette out 5 ml of the reaction mixture and discharge it into 50 ml of ice cold water
kept in a conical flask.
4. Titrate the reaction mixture against NaOH solution using phenolphthalein as indicator.
This titre value corresponds to Vo.
5. Steps 3 and 4 are repeated at intervals of 5, 10, 15, 20, 30, 45, 60 minutes. Each titre
value corresponds to Vt .
6. The remaining solution is taken in a stoppered conical flask and heated to 60o C, and
kept at this temperature for 5 minutes.
7. The solution is allowed to cool to room temperature.
8. Repeat Steps 3 and 4. This titre value corresponds to V∞ till concurrent values are
obtained.
9. Plot a graph of log (V∞ -Vt ) versus time (t) and determine the slope.
10. Report the theoretical and graphical value of rate constant (k1).
RESULT:
Rate Constant (k1) for the acid-catalyzed hydrolysis of methyl acetate (CH3COOCH3) at ….
o C = _____________________ (theoretical). = _____________________ (graphical).

61
 CHEMISTRY VIVA QUESTIONS

1. What is EDTA? Write the structure of EDTA.

ANS: Ethylene Diamine Tetra Acetic acid

2. What is EBT?
ANS: Eriochrome black-T, used as an indicator in EDTA experiment.
3.What is pH? Write the formula for it. What is its range?
Ans: pH is to find out whether the solution is acid or basic (or) neutral.
pH = -log10[H+] The pH range is 0 to 14.
4.What is a buffer solution? Give examples.
Ans: Buffer solution is the one which maintains the pH of a solution constant.
Ammonia buffer = Ammonia chloride and liquid ammonia.

5. What the pH range is to be maintained around 10 in EDTA titration?

Ans: In order to get the end point, steel blue colour. It is the colour of the indicator EBT.
6. On what principle the colour changes from wine red to steel blue?
Ans: Hard water + EBT Metal ion –indicator complex(wine red colour) Metal ion-indicator complex
+ EDTA Metal ion – EDTA complex + Indicator
7. What is alkalinity?
Ans: A measure of acid neutralizing ability of a substance
8. Which ions impart alkalinity to the natural water?
Ans : Carbonate, bicarbonate and hydroxide ions.
9. How many types of alkalinity are possible?
Ans:1. Carbonate alkalinity 2. Bicorbonate alkalinity and 3. Hydroxide alkalinity

10.What is a standard solution ?

Ans: A solution whose strength is known is called a standard solution.

11.What is a normal solution ?

Ans: A solution containing one gram-equivalent mass of the solute per litre of the solution is called a
normal solution.

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12.What is the equivalent mass of KMnO4 when it acts as oxidizing agent in acidic medium ?
Answer. KMnO4 loses 5 electrons per molecule, when it acts as oxidizing agent in the presence of
acids. Therefore, its equivalent mass is one-fifth of its molecular mass.

13.What is redox reaction?

Ans: A chemical reaction in which both oxidation and reduction reaction takes palce.

14.What is Oxidation?
Ans: Oxidation is
a) Loss of Electrons
b) Increase in Oxidation number
c) Gain of Oxygen
d) Loss of Hydrogen

15.What is Reduction?
Ans:-Reduction is
a) Gain of Electrons
b) Decrease in Oxidation number
c) Loss of Oxygen
d) Gain of Hydrogen

16. What is the indicator used in this reaction?

Ans: No indicator is used. KMnO4 acts as a self indicator.

17. What is the color change in this reaction?

Ans: Colorless to pale pink.

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ROUGH WORK

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