BS514CHE-E(DSEA) LM

B.Sc.
THIRD YEAR SEMESTER – 5

CHEMISTRY

GREEN CHEMISTRY & ENVIRONMENTAL CHEMISTY

Laboratory Manual and Record

“We may forgo material benefits of civilization, but we cannot forgo

our right and opportunity to reap the benefitsof the highest education
to the fullest extent as the education is the greatest material benefit”
-Dr. B. R. Ambedkar

Dr. B. R. AMBEDKAR OPEN UNIVERSITY

HYDERABAD
2020
 C O U R S E T EAM
Course Development Team
(CBCS Edition)

Editor
Dr. K. Prameela

Writers
Sri. D. Koteswara Rao

Cover Design
Venkata Swamy

First Edition : 2020

© 2020, Dr. B. R. Ambedkar Open University, Hyderabad, Telangana.

All rights reserved. No part of this book may be reproduced in any form without the permission
in writing from the University.

The text forms part of Dr. B. R. Ambedkar Open University Programme.

Further information on Dr. B. R. Ambedkar Open University courses may be obtained

from the Director (Academic), Dr. B. R. Ambedkar Open University, Road No. 46,
Prof. G. Ram Reddy Marg, Jubilee Hills, Hyderabad – 500033.

Web: www.braou.ac.in
E-mail: info@braou.ac.in

Printed on behalf of Dr. B. R. Ambedkar Open University, Hyderabad by the Registrar.

Lr. No. –

Printed at : ……………………………………………………………………….
 PREFACE
This Laboratory Mannual deals with topics included in B.Sc third year chemistry,
fifth semester practical course (pertaining to discriptive elective course - A), Green
chemistry and Environmental Chemistry by the Dr. B. R. Ambedkar Open University.

The Laboratory Mannual is covered in two blocks, each block comprising of four
units. Each unit contains aim of experiment , objectives, chemical and apparatus need for
the experiment.

The first block is deals with detailed discussion of procedures of synthesis of some
chemical compounds using green methods such as microwave assisted synthesis, ultrasonic
assisted sythesis and some solvent free general heating reactions.

In the second block, we included practical procedures related to water analysis

such as pH, conductivity, total dissolved substances, alkalinity and hardness.

This laboratory mannual is prepared in a self instructional pattern. The university

hopes that the student can successfully carryout the experiments and it serves both as an
instructor and as a record. So you keep the mannual as neat as possible and record your
observations in the space provided.
 CERTIFICATE
Certified that this is a bonafied record of the

Laboratory work carried out by Sri / Kum / Smt

............................................................................................................................

Admission No. ..................................................................

in the study centre of Dr. B. R. Ambedkar open uni-

versity during the year .............................

Signature of HOD Signature of the Counsellor

Date :
 CONTENTS

Block-1: Green Chemistry 1

Unit – 1: Preparation of Salicylic Acid (Aspirin)

by Microwave Assisted Method 3
Unit – 2: Preparation of Cu(II) Phthalocyanine Complex 7
Unit – 3: cis - Dihydroxylation of Styrene
by Ultrasonic Assisted Method 11
Unit – 4: Green Synthetic Process Alternative

to Conventional Process 16

Block-2: Environmental Chemistry 33

Unit – 5: Determination of Conductivity and

Total Dissolved Substances (TDS) of Water 35
Unit – 6: Determination of Ph of Water 41
Unit – 7: Determination of Hardness of Water 43

Unit – 8: Determination of Alkalinity of Water 53

Model question paper 58

 BLOCK-1

GREEN CHEMISTRY - 1
Organic compounds either obtained from natural sources or prepared
synthetically involve some of the importent reaction such as N - and O - acetylation,
condensation, alkylation, halogenation, nitration, oxidation, reduction, diazotization and
coupling etc...

It is therefore essential that students should know the principles, mechanism,

techniques involved in the preparation, purification methods, characterisation, establishing
the identity, and calculation of the percentage yield of the compounds.

Thus this block deals with the following units.

Unit – 1: Preparation of Acetyl Salicylic Acid (Aspirin) By Microwave

Assisted Method
Unit – 2: Preparation of Cu(II) Phthalocyanine Complex

Unit – 3: cis - Dihydroxylation reaction of Styrene by

Ultrasonic Assisted Method

Unit – 4: Green Synthetic Process Alternative To Conventional

Process

1
2
 UNIT - 1: PREPARATION OF ACETYL SALICYLIC ACID
(ASPIRIN) BY MICROWAVE ASSISTED METHOD

1.0. AIM

The aim of the experiment is to understand the application of microwave power in the
prepare a pure sample of aspirin by the o-acetylation of salicylic acid.

1.1. OBJECTIVE
After compleation of this experment you should be able to
• define the microwave power,
• selecting the suitable power for the preparation.
• handling of glassware and required chemical in the microwave assisted
synthesis.
• understanding the new synthetic path for the synthesis of Acetyl Salicyclic Acid.

1.2. APPARATUS
Microwave oven
Conical flask (200ml)
Measuring Jar (100ml)
Test tube
Glass rod

1.3. CHEMICALS
Salicylic acid (2.5 g)
Aceticanhydride 4.5 ml
Conc.Sulphuric acid (1 or 2 drops) (For convenstional synthesis)
Conc. Phosphoric acid (3-5 drops) (Microwave synthesis)

1.4. PRINCIPLE
A Microwave is a form of electromagnetic radiation it is in between IR and
radiofrequency. It falls in lower frequency of energy from the range 300 to 300000 MHz. the
microwave of within this region causes molecular rotation but not affected the molecular structure.

Microwave energy source can be successfully used in the synthesis of various chemical
compounds in the field of organic and inorganic chemistry. It is very efficient, economical and
eco friendly green synthetic methodology.

3
 In conventional heating synthetic methods apparatus, all materials used in the preparation
gets heated to same thermal energy and it takes longer time to complete, leads to lower yields,
by products are formed along with desired products and some time it leads to decomposition of
starting materials or products due to its harsh reaction conditions. In other hand, microwave
assisted synthetic methods easily handle selective heating and higher temperatures (superheating
and sealed vessels) of the reactions, considerably faster reaction in less time, pure products or
with minimum by products.

Most of the chemical laboratories used domestic microwave oven with multiple energy
ranges for the synthesis of chemical compounds. However, microwave technology developed
synthetic microwave work station with different capacities. Microwave oven reactors are
classified in two types. Multi mode synthetic microwave reactor and mono or single mode
synthetic microwave reactor.

In single mode microwave rectors are having small compact cavity to hold the single
vessel containing reaction mixture. This kind of reactors can handle one reaction vessel at a
time. which makes them an ideal tool for optimizing chemical reactions on a small scale.

Multimode reactors have larger cavities in which the microwave field is distributed in a
non sequential manner. In common multimode reactors the waves are reflected from the cavity
walls and multiple modes of the electromagnetic waves interact with the cavity load. Because
of their larger size, these instruments can host multiple reaction vessels.

O-Acetylation N-acetylation involves the replacement of hydrogen of hydroxyl group NH2 by

acetyl radical. Thus salicylic acid when heated with acetic anhydride undergoes o-acetylation
forming o-acetyl salicylic acid (aspirin). This reaction involves the following steps as illustrated
in O-acylation.

Reaction:
O
OH H3 C
O C CH3
C O
COOH
+ O COOH CH3 COOH
+
C O Acetic acid
H3C
2-acetoxybenzoic acid
Salicylic Acid Acetic anhydride or
Acetyl salicylic Acid
Mechanism
O O
CH3 H3C O
OH C C O C CH3
O C
COOH O O CH3 COOH
H
+ O
COOH
O C
-H +
CH3
CH3COOH

4
1.4. PROCEDURE
In conventional method

Place 2.5g of dry salicylic acid and 4.5ml of acetic anhydride in a dry 100ml conical flask,
add one or two drops of concentrated sulphuric acid and rotate the flask to secure through
mixing. Warm on a water bath to about 50-600C stirring with a glass rod for about 10 minutes.
Allow the mixture to cool occasionally stirring. Add 30ml of cold water, stir well when aspirin
separates out as a colourless solid. Filter at the pump. Wash it with a little cold water, allow it to
drain and recrystallise from hot 50% alcohol.

Microwave synthesis of aspirin

Take 2.5 grams of dry salicylic acid and 4.5 of acetic anhydride in 250 ml conical flask .
add carefully 3 to 5 drops of 85 % phosphoric acid to the solution and mix the contents thor-
oughly. Heat the mixture in Microwave oven in minimum power till all the salicylic acid was
dissolved. Later heat the reaction mixture at 350 to 400 watt microwave power for a minute.
After completion of the reaction cool the reaction mixture to room temparature, add 30 ml of
cold water to the mixture, and the solution was cooled on an ice bath until aspirin crystallized.
The crystals were filtered using a Buchner filter and wash the residue using chilled water. Dry
the resulted residue and determine its melting point

1.5. REPORT
Melting Point :
Yield :
% Yield :
Appearance :

Note: 1. Aspirin decomposes at its melting point. Report the melting point range.
2. Acetylation can also be performed using acetyl chloride in the presence of
pyridine.
3. Phenols usually form O-acyl solid derivaties which are readily
characterized.
4. Aspirin is used as an antipyretic and an analgesic.

5
 1.6. SELF ASSESSMENT ON REACTION AND REACTION
MECHANISM

6
UNIT - 2: PREPARATION OF Cu(II) PHTHALOCYANINE
COMPLEX

2.0. AIM
The aim of the experiment is to prepare a sample of Cu(II) - Phthalocyanine complex
by Microwave assisted synthesis.

2.1. OBJECTIVE
After compleation of this unit you should be able to

• formation of Cu - Complex.

• preparation of porpyrine structure.

• operation of Microwave oven for synthesis.

2.2. APPARATUS
1. 100ml Beaker .

2. Measuring jar and droppers.

3. Glass rod.

4. Funnel....etc

2.3. CHEMICALS
l. Phthalic anhydride (4 mol)

2. Anhydrous CuCl2 (1 mol)

3. Ammonium Molybdate. (1 mol)

4. Urea (4 mol)

2.4. PRINCIPLE
Cu (II) Phthalocyanine is formed through the cyclotetramerization of Pthalic anhydride
or phthalic acid. In this unit Cu- complex is prepared by Phthalic anhydride with urea and
anhydrous CuCl2. This reaction is catalysed by the ammonium molybdate. These are used as
dyes, pigments , synthesis of nanomaterials, photo voltaic cells , photosenisitizes for treating non
vasive cancers and Biosensors.

7
 Reaction:
O
O

+ 4 +
4 O CuCl 2
H 2N NH 2
copper(II) chloride
Urea
O
Phthalic anhydride

(NH4)6Mo7O 24

N N
N

N Cu N

N
N N

Cu (II) Phthalocyanine Complex

2.5. PROCEDURE
Preparation of Anhydrous CuCl2

Take 2 g of CuCl2.2H2O into a dry china dish, heat it to melt on flame to liquid and continue
heating untill vapour disappears. Allow it to solidify and grind it fine powder. It is called anhy-
drous CuCl2.

8
Take accurate 0.5g of anhydrous CuCl2 , that is to be intimately combined with excess urea (5.5
g, 92 mmol), phthalic anhydride (3.2g, 20 mmol), and ammonium molybdate (61 mg, 0.05 mmol)
using a mortar and pestle. Grind these contents until a homogeneous mixture is formed, and
then place it in a beaker that is covered with a watch glass. Place this beaker in a petri dish
containing silica gel (silica jacket) and irradiate in a laboratory microwave oven for 6 min. After
each interval of 1 min, stop microwave radiations for 5 sec. There is no need to stir the reaction
mixture after each interval. The presence of a white layer on the complex is observed, which
may be due to the formation of ammonium carbonate during the reaction. Cool the reaction
mixture to room temperature, grind it and wash with 5% caustic soda, water, 2% hydrochloric
acid and again with water respectively. The dried phthalocyanine thus obtained is weighed for
the calculation of yield. Take Dry complex and prepare the 10-3 to 10-4 stand solution of Cu (II)
Phthalocyanine by dissolving it in N-methyl-2-pyrolidinone and record the UV-vis spectrum to
characterize. Determine its melting point and yield.

2.6. REPORT

Melting Point :

Yield :

% Yield :

Appearance :

Note: 1. Concentrated Sulphuric acid drop is to be added only when benzylidene aniline does
not separate in the usual process.

2. All aromatic aldehydes readily condense with primary aromatic amines to yield
characteric solid schiff's bases.

Ref:

9
 1. Solventless and One-Pot Synthesis of Cu(II) Phthalocyanine Complex: A Green
Chemistry Experiment- R. K. Sharma, Chetna Sharma, and Indu Tucker Sidhwani
(doi. 10.1021/ed100473u)

2. Synthesis and Characterization of Water Soluble Cu(II) Phthalocyanine Complexes

B. Wang &H. Zh. Ma. doi.org/10.1081/SIM-120037523

2.7. SELF ASSESSMENT ON REACTION AND REACTION

MECHANISM

10
 UNIT - 3: cis - DIHYDROXYLATION OF STYRENE BY
ULTRASONIC ASSISTED METHOD

3.0. AIM

The aim of the experiment is to understand the application of Ultra sonicator in the
dihydroxylation reaction of styrene by KMnO4.

3.1. OBJECTIVE
After compleation of this experment you should be able to
• define the Ultra sonication,
• selecting the suitable temperature and ultrasonic power for the preparation.
• handling of glassware and required chemical in the ultrasonic assisted
synthesis.
• understanding the new synthetic path for the oxydation of styrene by KMnO4.

3.2. APPARATUS
Ultrasonicator
Boiling tube
Measuring Jar
Beaker tube
Gass rod

3.3. CHEMICALS
Styrene (2.5 g)
KMnO4 Solid
t-Butyl alcohol
Conc. Phosphoric acid (3-5 drops) (Microwave synthesis)

3.4. PRINCIPLE
sound in Chemical activation:
Sound waves are broadly classified into three categories
1. 10 Hz - 18 Hz Human hearing region.
2. 20 KHz - 100 KHz Power ultra sound (used in cleaning and sonochemistry)
100 KHz - 1 MHz Extended Range
3. 1 MHz - 10 MHz Used in medical diagnosis and analysis.

11
 Ultra sound is sound waves having frequencies higher than those which human ears
can respond. It is transmitted through any substance - solid, liquid or gas which possesses
elastic properties.

The use of ultrasound in chemical reactions in solution provides specific activation

based on a physical phenomenon: acoustic cavitation. Cavitation is a process in which mechanical
activation destroys the attractive forces of molecules in the liquid phase. Applying ultrasound,
compression of the liquid is followed by rarefaction (expansion), in which a sudden pressure
drop forms small, oscillating bubbles of gaseous substances. These bubbles expand with each
cycle of the applied ultrasonic energy until they reach an unstable size; they can then collide
and/or violently collapse.

There are two types of effects mediated by ultrasound, chemical and physical. When
the quantity of bubbles is low - using standard laboratory equipment - it is mainly physical rate
acceleration that plays a role. For example, a specific effect is the asymmetric collapse near a
solid surface, which forms microjets. This effect is the reason why ultrasound is very effective
in cleaning, and is also responsible for rate acceleration in multiphasic reactions, since surface
cleaning and erosion lead to improved mass transport.

12
 Reaction:

Olefin undergoes oxidation with aqueous KMnO4 and OsO4 to produce cis dihydroxy
product. styrene also undergoes oxidation with KMnO4 it produces 1-phenylethane-1,2-diol.

H OH
OH

KMnO 4
t-BuOH
H
H2O
H
)))))), 20 min
styrene RT
1-phenylethane-1,2-diol

Mechanism:

In the above reaction cis diols are obtained. The hydroxylation of alkene with KMnO4
involves the cyclic intermediate of manganate ester. The intermediate breaks down in water to
give cis-1,2-diols.The manganate ion is converted to MnO2 as precipitation.

O O
Mn O
O
O O Mn
O O HO OH
H
H
H
H

H
H2O H
+ MnO2

3.4. PROCEDURE
Ultrasonic synthesis of aspirin

Take 208 mg of styrene and 474 mg of KMnO4 in to a clean and dry conical flask.
Dissolve the mixture in 2 ml of t-butyl alcohol and 20 ml water. Keep the flak in Ultrasonicator.
Subject the mixture on ultrasonication at room temperature for about 20 minutes. Check the
reaction progress with thin layer chromatography (hexane; Ethyl acetate, 4:1 v/v). After
completion of the reaction then extract the resulted product with dichloromethane (alternatively

13
 dichloroethane or chloroform) three times with 10 ml portion. Combine all extractions of
organic solvents, dry it with sodium sulfate and evaporate the solvent we get the desired product.
Determine its yield and boiling point.

3.5. REPORT
Melting Point :
Yield :
% Yield :
Appearance :

Note: 1. For frequencies between 20 and 30 KHz, it is recommended to use

hearing protections. The ultrasonic frequency is not audible; it is in fact
the vibration modes of the tank structure that you can hear. Over 40
KHz, the noise level is lower and not much annoying..

14
3.6. SELF ASSESSMENT ON REACTION AND REACTION
MECHANISM

15
 UNIT - 4: GREEN SYNTHETIC PROCESS ALTERNATIVE
TO CONVENTIONAL PROCESS
In this unit we going to learns some importent green reactions and green processes
which are alternative to highly expensive, time consuming and hazardous conventional reactions
and preocesses.

4A: ACETYLATION OF PRIMARY AMINE (PREPARATION

OF ACETANILIDE)

4A.0. AIM

To prepare the acetanilide from acylation reaction by adopting green process with
generation of less hazardous materials.

4A.1. OBJECTIVE
After compleation of this experment you should be to

 Identification of alternative green processes and materials.

 Usage of acetic acid alternative to acetic anhydride (banned by excise and

pollution control departments).

4A.2. APPARATUS
250 ml Round bottomed flask
Measuring Jar
Beaker
Funnel

4A.3. CHEMICALS
Aniline - 10 ml (10.2 g)

Glacial acetic acid - 30 ml

Zinc dust - 0.5 g

4A.4. PRINCIPLE
Conventionally acetanilide is prepared from the aniline, acetic anhydride in presence
of pyridine, dichloromethane. Usage of Pyridine and dichlromethane is not ecofriendly and
acetic anhydride is banned due to its misuse in the production of norcotic drugs and toxixity.

16
 Alternatively acetaniline is prepared boiling of aniline, acetic acid and Zn dust. In this
reaction acetic acid reacts with Zn dust produces diacetoxy zinc, it reacts with aninline by
electrophilic substition on amine group leads to acetanilide.
Reaction:
O

NH2
HN CH3

CH3COOH

Zn
Boiling
Mechanism:

O O O
Zn
Zn
Boiling
H3C OH H3C O O CH3

NH2

C
H3C NH
O H

H3C C N H

+ + + ZnO
H3C O
CH3COOH

17
 4A.5. PROCEDURE
A mixture of aniline (10 ml) and zinc dust (0.5 g) in acetic acid (30 ml) in a 100 ml round
bottom flask was heated over a gentle flame using water condenser. Heating was continued for
about 2 hrs. The reaction mixture was then carefully poured in cold water (100 ml) in a 250 ml
beaker with cooling and vigorous stirring. The shining crystals of acetanilide were separated
slowly. After 15 min. the acetanilide crystals were collected by filtration. The solid crystals
were washed over the Buchner funnel with water and the product was dried (yield, 10 gm). It
was crystallized in boiling water. Determine its yield and melting point.

4A.6. REPORT
Melting Point :
Yield :
% Yield :
Appearance :

Green Context:

Avoids use of acetic anhydride (usage banned in some states, due to its usage in
narcotic business and its toxic nature.

Minimizes waste by-products

Avoids hazardous solvent

Ref:
1. Monograph on Green Chemistry Laboratory Experiments, Green Chemistry Task Force
Committee, DST.

18
4A.7. SELF ASSESSMENT ON REACTION AND REACTION
MECHANISM

19
 4B: BASE CATALYZED ALDOL CONDENSATION
(SYNTHESIS OF DIBENZALPROPANONE)

4B.0. AIM

To prepare the dibenzalpropanone from Benzaldehyde and acetophenone by adopting

green aldol condensation.

4B.1. OBJECTIVE

After compleation of this experment you should be able to

 Identification of alternative green processes and materials.

 Understanding the mechanism of aldol condensation.

4B.2. APPARATUS
Conical Flask with cork

Boiling tube

Measuring Jar

Beaker

Glass rod

4B.3. CHEMICALS
Acetone –1 ml (0.83 g)

Benzaldehyde – 3.8 ml (3.9 g)

NaOH – 30 ml of 10 % soln

4B.4. PRINCIPLE

Carbonyl compound with  - hydrogen atom undergoes a reversible self addition in

presence of dilute alkali to give condensation product called - hydroxy carbonyl compound or
aldol known as aldol condensation.

Acetone is the carbonyl compound with six hydrogens containing possition to the
carbon positions undergo conensation reaction with two moles of benzaldehyde produces di
hydroxy carbonyl compound which is on dehydrogenation produces dibenzalpropanone by the
removal of two water molecules.
20
Reaction:
CHO O
O
Aq NaOH
2 +
H 3C CH 3 C2H5OH

Mechanism:
H O
C
O
O
OH
H2 O
-H2O H3C CH2
H3C C H
H2

O H OH
O H OH
C
H 2C C OH
H2 H3 C C
-H2 O H2
H O
C

H2O

HO H O H OH

C C
H2 H2

-2H2 O

1,5-diphenylpenta-1,4-dien-3-one

21
 4B.5. PROCEDURE
Measure 1 ml of Benzaldehyde and 3.8 ml of Acetone in a clean and dry conical flask.
Dissolve the reaction contents present in the conical flask in 15 ml alcohol mix it thoroughly for
2 minutes. Add 30 ml of 10% sodium hydroxide solution and then shake the reaction contents
vigorously by keeping cork for 20 min. simultaneously release the pressure generated in the
flask. Cool the reaction mixture on ice bath, a pale yellow crystals are separated out. Filter it
wash with cold water and recrystallize with hot water. Determine its yield and melting point

4B.6. REPORT
Melting Point :
Yield :
% Yield :
Appearance :

Green context:

Hazardous organic solvents are avoided

Reagents are non-toxic

22
4B.7. SELF ASSESSMENT ON REACTION AND REACTION
MECHANISM

23
 4C: DIELS-ALDER REACTION BETWEEN FURAN AND
MALEIC ACID ([4+2] CYCLOADDITION REACTION)

4C.0. AIM

To prepare the Diel’s alder adduct from Furan and maleic acid by 4+2 cycloaddition
reaction.

4C.1. OBJECTIVE

After compleation of this experment you should be to

 Identification of alternative green processes and materials.

 Understanding the mechanism of cycloaddition reaction.

4C.2. APPARATUS
Conical Flask with cork

Boiling tube

Measuring Jar

Beaker

Funnel and glass rod

4C.3. CHEMICALS
Furan –1 g

Maleic acid – 2 g

4C.4. PRINCIPLE

Conjugate addition of two are more olefins and dienes like   systems to produce
cyclic adduct called cycloaddition reaction.

Diene undergo cycloaddition with dienophine under thermal reaction condition to pro-
duce a cyclic adduct called Diel’s Alder reation.

In this reaction Furan act as diene and Maleic acid act as dienophile are undergoes
conjugate addtion to produce furan-maleic acid adduct. These are molecular reactions. No in-
termediates are formed and solvent will not influence the reaction.

24
Reaction:

O
HOOC
H2O COOH
+

HOOC O

COOH

Mechanism:

O
HOOC COOH

HOOC O
COOH

Transition state

COOH

COOH
7-oxabicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid

or Furan-Maleic acid adduct

25
 4C.5. PROCEDURE
Take 1g of furan and 2g of Maleic acid into a clean round bottomed flask it containing
10 ml distilled water. Stir or shake the mixture vigorously for about 2-3 hrs at room temperature
( continuous and constant stirring or mixing of reaction mixture required to progress of the
reaction). After completion of the reaction time, cool the reaction mixture, an adduct of product
is obtained. Filter it and recrystallize using aqueous ethanol. Determine its yield and melting
point.

4C.6. REPORT
Melting Point :
Yield :
% Yield :
Appearance :

Green context:

Reaction carried out in aqueous medium avoiding benzene

Efficient at room temperature itself

100% atom efficient

26
4C.7. SELF ASSESSMENT ON REACTION AND REACTION
MECHANISM

27
 4D: TRANS ESTERIFICATION OF VEGITABLE OIL TO
CRUDE BIO-DIESEL

4C.0. AIM

To understand the reaction and mechanism of transesterification of vegetable oil to

produce bio diesel fuel from vegetable oil and the process of transforming one type of ester into

another type of ester.

4D.1. OBJECTIVE

After compleation of this experment you should be able to

 define the trans esterification.

 study the production of bio diesel from vegetable oil.

 understand the mechanism of transesterification.

4D.2. APPARATUS
Conical Flask with cork

Boiling tube

Measuring Jar

Beaker

Separating Funnel and glass rod

4D.3. CHEMICALS
Vegetable oil – 100 ml

Methanol – 20 ml

NaOH or KOH - 3 pellets

4D.4. PRINCIPLE

Biodiesel is a cleaner burning renewable alternative to diesel fuel that is made from
biological sources namely vegetable oil or animal fats (triglycerides). It is mixable with diesel,
stable in mixture, and can be burned in an unmodified diesel engine at any concentration.

28
 Biodiesel is made through a transesterification reaction. Transesterification is the
chemical process through which one ester (a chemical having the general structure R’-COOR’’)
is changed into another. When the original ester is reacted with an alcohol, the process is called
alcoholysis. Vegetable oil (an ester compound) and methanol (an alcohol) reacting in presence
of a catalyst to give biodiesel. Vegetable oil is a triglyceride (or triacylglycerol), which is essentially
a glycerin (or glycerol) molecule connected via ester bonds to three fatty acid molecules. Vegetable
oils and animal fats are composed of triglycerides. During the reaction, the fatty acids of the
triglyceride molecule are cleaved and attach to the methyl group of the methanol to form fatty
acid alkyl esters which are biodiesel. In order to get the transesterification of vegetable oil going
a base catalyst is potassium hydroxide (KOH). This reaction is represented as follows.

Reaction:

OR O
O
3 CH3
O O RO O
Methyl ester of f aty acid
H2C OR
+
CH3OH
CH O OH
Aq KOH
H2C H2C

O CH OH
O H2C

OR OH
Triglycerides of vegitable oil glycerin (or glycerol)

The transesterification reaction produces crude biodiesel. The product is considered

crude because it is contaminated with methanol, basic salts, and glycerin. All of these contaminants
are water soluble. Therefore, we need to remove them using a water wash. After washing
biodiesel with water, it decreases the quality of biodiesels due to presence of water content.
Bubble the dry air through wet biodiesel to dry it. This process forces the evaporation or settling
of water molecules remaining in the fuel and leaves to generate finished biodiesel fuel.

29
 OR

O O O
H2 H2
O O C C
H
RO O C O OR
H 2C OR
CH3OH
CH O ONa
Aq KOH +
H 2C O

O CH 3
RO O
O
Methyl ester of f aty acid
OR

CH3OH Aq KOH

H2 H2 O
C H C H2 H2
NaO C ONa C H C
RO O C ONa
ONa CH 3OH
+ ONa
+
O Aq KOH
O
CH 3
RO O CH 3
Methyl ester of f aty acid RO O
Methyl ester of f aty acid

4D.5. PROCEDURE

Preparation of sodium or potassium methoxide solution:

Take 20 ml of pure methanol into a 250 ml conical flask and then add 3 pellets of
Sodium or Potassium hydroxide. Stirr the mixture till sodium or potassium hydroxide pallets.

Preparation of Biodiesel:

The pure vegetable oil (100 ml) was warmed to about 40 oC in a 250 ml beaker. The warmed up
oil was poured into the methoxide solution with continuous stirring. At first the mixture would
become cloudy, but should soon two layers would separate. This was stirred for 15-20 minutes.
The contents of the flask were transferred into a 250 ml separatory funnel. The mixture will
separate into two different layers. The glycerol will fall to the bottom, and the methyl ester
(biodiesel) will float to the top. Allow the experiment to sit for an hour. The stopcock of the
separatory funnel was opened and the glycerol was allowed to drain into a small beaker.
30
 Top most layer in the separating funnel is methyl ester of facty acid, it is crude bio
diesel. it requires purification for futher its application.

4D.6. REPORT
Melting Point :
Yield :
% Yield :
Appearance :

Green Context:

This lab experiment demonstrates three key green principles: the use of renewable
feedstock, catalysis and design for degradation. Vegetable oil is a renewable starting material
as it is derived from growing plants, rather than irreplaceable material like the earth’s petroleum
and natural gas supplies. The reaction is catalyzed by NaOH making this process economically
viable for the industrial scale production of biodiesel. Biodiesel is an excellent product as it is
environmentally friendly.

Safety:

 Methanol: Flammable and poisonous. Dispose excess by allowing it to evaporate in

the fume hood.

 NaOH: Very corrosive. Causes severe burns. May cause permanent eye damage.
Very harmful by ingestion.

Clean Up

 Clean all glassware and bench space.

 Biodiesel can be used in candles or tiki torches (not suitable for use in an engine)

 Glycerin contains excess methanol. This can be boiled off under a fume hood
(not a student activity) and the methanol-free glycerin can be used to make soap.

 Wash water can be sent down the drain

31
 4D.7. SELF ASSESSMENT ON REACTION AND REACTION
MECHANISM

32
 BLOCK - 2

ENVIRONMENTAL CHEMISTRY
This block deals with the principles, mechanism, techniques involved in the
preparation, purification methods for characterisation and establishing the identity and
calculation of the percentage yield of the some more organic compounds.

Unit – 5 : Determination of Conductivity And Total Dissolved Substances

(TDS) of Water

Unit – 6 : Determination of Ph of Water

Unit – 7 : Determination of Hardness of Water

Unit – 8 : Determination of Alkalinity of Water

33
34
 UNIT - 5: DETERMINATION OF CONDUCTIVITY AND
TOTAL DISSOLVED SUBSTANCES (TDS) OF WATER
5.0. AIM
The aim of the experiment is to determine the physical parameters of water such as
total dissolves substances and conductivit.

5.1. OBJECTIVE
After compleation of the unit you should be able to
define the terms total dissolved substances (TDS) and conductivity.
experimental determination of TDS and conductivity of water.

5.2. DETERMINATION OF CONDUCTIVITY AND TOTAL

DISSOLVED SUBSTANCES (TDS) OF WATER SAMPLE
5.2.1.Determination of Conductivity of water sample.
Principle- Specific conductance is determined by using a Wheatstone bridge in which a variable
resistance is adjusted so that it is equal to the resistance of the unknown solution between
platinized electrodes of a standard conductivity cell. The cell constant is determined by the
following relationship:

Specific conductance = Conductance × Cell constant, or

Cell constant
Specific conductance 
Resistance
The cell constant is determined experimentally with a standard solution of known conductance.
Apparatus:
a. Conductivity Meter
b. Conductivity Cells
Cells of at least two different cell constants, for measurement of wide range of con ductivities.
Specific conductance ranges and corresponding values of cell constants are given below
SPECIFIC CONDUCTANCE CELL CONSTANT
μS/cm at 25 0C
20 – 1000 0.2
40 - 2000 0.5
100 - 4000 1.0
200 - 10000 2.0
400 - 20000 5.0
10000 - 40000 10.0

35
 Chemicals required:

Standard Potassium Chloride Solution- Dissolve 0.5232gm potassium chloride (dried at

1800C for 1hr) in demineralized water and dilute to 1000 mL. The distilled water used for
preparing standard solutions should have a very low conductivity. The specific conductance of
this solution at 250C is 1000μs/cm and the concentration of this solution is 0.00702 N. Alternatively,
dissolve 0.7456 gm of anhydrous potassium chloride, (dried at 180:C for 1hour) in distilled water
and make up to 1000 mL at 250C . The specific conductance of this solution at 250C is 1408 μs/

cm and the concentration of this solution is 0.01N.

Procedure:

Set the instrument according to manufacturer’s instruction. Determine conductivity of

0.00702 N potassium chloride or 0.01 N. Potassium chloride solutions by use of instrument in
accordance with manufacturer’s instructions. Measure the temperature of the solution before
and after the test and take the mean value (t0C). Take 100 ml beaker and rinse it with double
distilled water twice. Measure 50 ml of water sample into previously cleaned beaker. Deter-
mine the conductivity of the water sample by keeping conductivity cell.

Calculation:
Calculate specific conductance as follows:
Specific conductance at 250C, s/cm = CKf
Where
C= conductivity in s/cm;
K = Cell Constant (in general it is 1.000) and
f = factor for converting specific conductance value to that at 250C

Where f = at 250C it is 1.000, at 270C it is 0.960 , at 300C it is 0.907 and at 35 0C it is

0.829

36
37
 5.2.2. Determination of Total Dissolved Substances (TDS) of water sample.
a. Conducometric method:
The ability of a solution to conduct an electric current is the functioning of the concentration
and charge of ions in the solution and also depends on ionic mobility. Ionic mobility decreases
with increase in number of ions per unit volume of solution due to interionic effect and other
factors. Broadly, the relationship between conductivity and dissolved solids and conductivity
and soluble cations is given by the following equations:

A Cobs = S and,

Cobs = 100 C

Where

A = multiplication factor for converting conductivity values to total dissolved solids;

Cobs = conductivity in s/cm,

S = total dissolved solids in mg/L, and

C = total soluble cations in meq/L.

Note - 1: the value of A varies from 0.54 to 0.96 depending on the nature of ion present in
water, and is usually taken as 0.65.

Note - 2: The relationship given above is approximate and is used for broad checking only and
should not be used for accurate calculations. Types of ions present in solution effect these
relationships. A pure solution of sodium bicarbonate with total dissolved solids 980 mg/L will
have a conductivity of 1000μs/cm and a solution of sodium chloride with total dissolved solids
500 mg/L will have the same conductivity. Presence of relatively low conductivity particles or
molecules like silicic acid and the presence of H+ and OH¯ ions affect the ratio between

conductivity and total dissolved solids.

38
Gravimetric Method

Principle – The sample is filtered and the filtrate evaporated in a china dish on steam bath.
The residue after evaporation is dried to constant mass at 103-105°C or 179-181°C

Apparatus

1. Gooch crucible-30mL capacity with 2.1 or 2.4 cm diameter glass fibre filter disc
(Whatman or equivalent paper>
2. Analytical Balance 200gm capacity and capable of weighing to nearest 0.1 mg..
3. Drying oven with thermostatic control for maintaining temperature up to 180 ±2°C.
4. Filtering assembly depending upon the type of filter selected.
5. China dish.
Procedure

Heat the clean evaporating China dish to 180°C for 1 hr. Cool in the desiccators, Weigh
and store in the desiccators until ready for use. Filter a portion of the water sample through
given Gooch crucible. Select volume of the sample which has residue between 25 and 250mg
preferably between 100 to 200mg. This volume may be estimated from values of specific
conductance to obtain a measurable residue, successive aliquots of filtered sample may be
added to the sample dish.

Stir volume of sample with a magnetic stirrer or shake it vigorously. Pipette this volume
to a weighed evaporating dish placed on a steam bath. Evaporation may also be performed in a
drying oven. The temperature of drying oven shall be lowered to approximately 98°C to prevent
boiling and splattering of the sample. After complete evaporation of water from the residue,
transfer this dish to an oven at 103-105°C or 179-181°C and dry to constant mass i.e. till the
difference in the successive weighing is less than 0.5 mg. Drying for a long duration (usually 1-
2 hr) is done to eliminate necessity of checking for constant mass. The time for drying to
constant mass with a given type of sample when a number of samples of nearly same type are
to be analyzed has to be determined by trial.

Weigh the China dish as soon as it has cooled avoiding residue to stay for long time as
some residues are hygroscopic and may absorb water form desiccant that is not absolutely dry.

Calculation:
Total dissolved Substance (TDS) mg/L = weight of dry china dish after evaporation
– initial empty weight of dry china dish

39
 5.5. REPORT
physical parameters of water sample are noted as
a. conductance of water sample:
b. Total dissolved substance (TDS) of water sample:

40
 UNIT - 6: DETERMINATION OF pH OF WATER
6.0. AIM
The aim of the experiment is to determine the physical parameters of water such as
total dissolves substances, pH and conductivity.

6.1. OBJECTIVE
After compleation of the unit you should be able to
• define the terms total dissolved substances (TDS), pH and conductivity.
• experimental determination of TDS, pH and conductivity of water.

6.2. APPARATUS
1. pH Meter with glass and reference electrode (saturated calomel) preferably with
temperature compensation.

2. Magnetic stirrer with polytetrafluoroethylene coated stirring bar.

3. Thermometer with least count of 0.5°C.

6.3. CHEMICALS
standared Buffer tablets

6.4. PRINCIPLE

pH value is the logarithm of reciprocal of hydrogen ion activity in moles per liter. In
water solution, variations in pH value from 7 are mainly due to hydrolysis of salts of strong
bases and weak acids or vice versa. Dissolved gases such as carbon dioxide, hydrogen sulphide
and ammonia also affect pH value of water. The overall pH value range of natural water is
generally between 6 and 8. In case of alkaline thermal spring waters pH value may be more
than 9 while for acidic thermal spring waters, the pH may be 4 or even less than 4. Industrial
wastes may be strongly acidic or basic and their effect on pH value of receiving water depends
on the buffering capacity of water. The pH value of water obtained in the laboratory may not be
the same as that the time of collection of water samples, due to loss or absorption of gases,
reactions with sediments, hydrolysis and oxidation or reduction taking place within the same
sample bottle. pH value should preferably be determined at the time of collection of sample.

The pH value is determined by measurement of the electromotive force of a

cell consisting of an indicator electrode immersed into the test solution and a reference electrode.
Contact between the test solution and the reference electrode is usually achieved by means of
a liquid junction which forms part of the reference electrode. The electromotive force is measured
with a pH meter i.e. a high impedance voltameter calibrated in terms of pH.

41
 Several types of electrodes have been suggested for electrometric determination of
pH value. Although the hydrogen gas electrode is recognized as primary standard, the glass
electrode in combination with calomel electrode is generally used with reference potential
provided by saturated calomel electrode. The glass electrode system is based on the fact that a
change of 1 pH unit produces an electrical change of 59.1 mV at 25°C. The active element of
glass electrode is membrane of a special glass. The membrane forms a partition between two
liquids of differing hydrogen ion concentration and a potential is produced between the two
sides of the membrane which is proportional to the difference in pH between the liquids.

6.5. DETERMINATION OF pH OF WATER SAMPLE

Follow the manufacturer’s instructions for operation of pH meter. Fix the glass electrode
and turn on the instrument. After required warm-up period. calibrate the instrument by using
standared buffer tablet solution. Then measure the pH of the water samples and note down the
results.

Caculation:
Note down the pH values as instrument moniter shown and respective temperature.

6.6. REPORT

pH of given water sample is ______________ and temparature at which. is ______

42
 UNIT - 7: DETERMINATION OF HARDNESS OF WATER
7.0. AIM
The aim of the experiment is to estmate the hardness of water by titrimetry method.

7.1. OBJECTIVE
After you complete this unit you should be able to
• define hardness of water.
• determine quantitatively the hardness of water

7.2. WHAT IS HARDNESS OF WATER

A sample of water which does not give lather or foam with soap but gives precipitate is
called Hard water. Hardness of water is due to the presence of bicarbonates, chlorides and
sulphates of calcium and Magnesium in dissolved state.
Ca+2 + 2C17H35COONa  Ca (C17H35COO)2  + 2Na+
Soap Ppt
(Sodium Stearate)
If the hardness of water is removed by boiling, it is called temporary or Carbonate
hardness. It is due to the presence of bicarbonates of Calcium & Magnesium.


Ca(HCO3)2 CaCO3 + CO2 + H2O


Mg(HCO3)2 MgCO3 + CO2 + H2O
If the hardness of water is not removed by boiling, it is called permanent or non carbon-
ate hardness. It is due to the presence of chlorides and sulphates of a Ca & Mg i.e. CaCl2,
CaSO4, MgCl2, MgSO4.
Samples of hard water collected from different sources contain varying amounts of
dissolved salts. It is expressed in Degree of hardness. The number of parts of CaCO3 equivalent
present in given amount of water is called degree of hardness.
Degree of hardness is expressed by the following units.
1. Parts per million (Ppm)
2. Milligrams per litres mg/L
3. Clarks degree of hardness clarks
4. French degree of hardness "French’’
Here only first two units which are generally used will be described.
Parts Per Million (Ppm): The number of parts of CaCO3 equivalent present in Imillion parts of

43
 H2O is called Ppm.
Milligrams per litre (mg/L): The number of milligrams of CaCO3 equivalent present in 1 lire of
water is called of mg/L. 1 Ppm = 1 mg/L.

7.3. APPARATUS
1. 50ml burette

2. Burette stand

3. Porcelain tile

4. 250ml conical flasks

5. 20ml pipette

7.4. CHEMICALS
1. Standard solution of calcium

2. EDTA solution

3. Ammonia - Ammonium chloride buffer solution (PH-10)

4. Eriochrome black-T- indicator.

7.5. PRINCIPLES
For estimation of hardness of water (Temporary and Permanent), EDTA is used which
forms a stable complex with Ca2+ & Mg2+ ions present in hard water at pH = 10 using a buffer
of (NH4OH + NH4CI) and Eriochrome black-T indicator.
EBT also forms a less stable complex with Ca2+ & Mg2+ ions as it acts as ligand. The
colour of solution becomes wine red. On titration against EDTA, wine red colour changes to
blue colour which gives the end point.
A disodium salt of EDTA is preferable as it is stable and gives a stable complex at pH-
10 with Ca2+ & Mg2+ ions.
Ca2+ + H2Y2-  CaY2- + 2H+ 78
H2Y2- = Bivalent anion EDTA

Ca+2 Ca - EBT Ca - EDTA

+ EBT + EDTA + EBT
Mg - EBT Mg - EDTA
Mg+2 Blue
colour Blue
Compex
colour
Wine red colour

44
7.6. PROCEDURE
Estimation of Temporary, permanent and total hardness of water consists of following three
parts.

1. Preparation of standard solution of hard water

Dissolve 1.0 gram of pure and dry (A.R) CaCO3 in minimum amount of dilute (3M)
HCI to convert it into CaCl2. Make the solution upto 1 litre with distilled water. Its degree of
hardness is Igm/litre or 1000 PPM. (I PPM- 1mg/L).

2. Standardization of EDTA solution

Pipette out 20ml of standard Hard water into a clean conical flask. Add 5 ml (1/4th test
tube) of buffer solution and few drops of EBT indicator. The contents of the flask attain wine
red colour.

Titrate the solution against EDTA from burette till the solution changes to blue colour. It
gives the end point. Note down the volume of EDTA required for titration. Repeat the experi-
ment to get 2 or 3 constant values. Let the volume of EDTA required for titration be V1ml.

Table: Standardisation of EDTA with Standard Hard Water

Volume of Burette Reading Vol. of EDTA

S.NO Standard Hard
Initial Final Required (V1)
Water
1. 20 ml

2. 20 ml

3. 20 ml

4. 20 ml

5. 20 ml

Pipette out 20ml of hard water sample into a cican cunical flask. Add 5 ml (1/4th test
tube) of buffer solution and few drops Eriochrome black -T indicator. The solution attains wine
red colour. Titrate this solution against EDTA from burette till the colour changes from wine red
to blue colour. Note down the volume of EDTA required for titration. Let this volume be V2ml.

45
 Table: Estimation of Total hardness of water

Volume of Burette Reading Vol. of EDTA

S.NO Sample Hard
Initial Final Required (V2)
Water
1. 20 ml

2. 20 ml

3. 20 ml

4. 20 ml

5. 20 ml

b) Estimation of permanent hardness

Take about 100ml of hard water sample. Boil it to remove hardness to about 1/4th of
volume. Bicarbonates of Ca+2 and Mg+2 decompose to form carbonates which settle down as
precipitate.


Ca(HCO3)2 CaCO3 + CO2 + H2O


Mg(HCO3)2 MgCO3 + CO2 + H2O

Filter it through what man filter paper 42 to remove insoluble CaCO3 and MgCO3. Now
temporary hardness is removed.

Make the solution upto original volume of 100ml with distilled water. Shake the solution
to make it homogenous. Pipette out 20ml of this solution into a clean conical flask and add 5 ml
(1/4 test tube) buffer solution and few drops of Eriochrome black T indicator. Titrate the solution
against EDTA from burette till the solution changes from wine red to blue colour.

Note down the volume of EDTA required for titration. Let this volume be V3 ml. Calcu-
late the total; temporary and permanent hardness.

46
 Table: Estimation of Permanent Hardness of water

Volume of Burette Reading Vol. Of EDTA

S.NO Sample Hard
Initial Final Required (V3)
Water
1. 20 ml

2. 20 ml

3. 20 ml

4. 20 ml

5. 20 ml

7.7. CALCULATIONS
Standard Hard Water:

1 mg CaCO3 in 1 1litre = 1 PPM.

1 mg CaCO3 in 1 litre = 1000 PPM

1000 ml standard Hard water contains 1000mg CaCO3

1000  20
20ml standand Hard water contains   20 mg CaCO3
1000

V1 ml EDTA = 20 mg CaCO3

1 ml EDTA = 20/V1 mg CaCO3

Total hardness of Water

20
1 ml EDTA =
V1 CaCO3

20V2
V2 ml EDTA =
V1 mg CaCO3

47
 20V2
20 ml hard water contains
V1 mg CaCO3

20V2 1000 1000V2

1000 ml Hard water contains =   PPM
V1 20 V1

Permanent hardness:

20
1 ml EDTA = mg CaCO3
V1

V3 ml EDTA = 20V3 mg CaCO3

V1

20 ml hard water contains = 20V3 mg CaCO3

V1

20V3 1000 1000V3

1000 ml hard water contains =   PPM
V1 20 V1

Temporary hardness = V2  V3  1000 P.P.M.

V1

(difference)

Simplified Calculations

V2
Total hardness of water =  1000 P.P.N
V1

V3
Permanent hardness of water =  1000 P.P.M.
V1

V2  V3
Temporary hardness of water =  1000 P.P.M.
V1

48
7.8. REPORT
1. a) Source (Sample of hard water collected)
b) Odour
c) Taste
2. Depth (approx. if known) -
3. Locality (From where sample collected) =
4. total hardness=
5. Permanent hardness =
6- Temporary hardness =
7- P of sample water =

49
 7.8. PRECAUTIONS
1. The titration should be carried out in buffer solutions of pH- 10
2. No other alkaline Earth metals should be present in the solution except Mg +2 and Ca+2
because they interfere in the titration.
3. The colour change near the end point is very slow, so the titration should be done slowly.
4. Over titration is to be avoided.

7.9. SELF ASSESSMENT QUESTIONS (SAQs)

1. Why Sodium salts of EDTA are used in titration?
2. What is the colour of Ca-EBT complex?
3. What is the function of buffer solution in the titration?
4. Write the structure of EDTA and disodium salt of EDTA?
5. How would you differentiate between hard and soft water?
6. What are the salts causing temporary and permanent hardness of water?
7. What happens when soap is rubbed with Hard water?
8. Write the units to express degree of hardness of water?
9. Define Ppm and mg/L
10.How do complexometric titrations differ from Redox titrations?

ANSWERS TO SAQS

50
51
52
 UNIT - 8: DETERMINATION OF ALKALINITY OF WATER

8.0. AIM
The aim of the experiment is to determine the phenolphthalein and methyl orange alka-
linity in the given water samples

8.1. OBJECTIVE
After you complete this unit you should be able to
• define alkalinity of water.
• determine quantitatively the alkalinity of water

8.2. APPARATUS
1. 50ml burette

2. Burette stand

3. Porcelain tile

4. 250ml conical flasks

5. 20ml pipette

8.3. CHEMICALS
Distilled Water – Distilled water used should have pH not less than 6.0. If the water has pH
less than 6.0, it shall be freshly boiled for 15 minutes and cooled to room temperature. Deionized
water may be used provided that it has a conductance of less than 2 μs/cm and a pH more than
6.0.

Standard solution of sulphuric acid - 0.02N

Phenolphthalein indicator - Dissolve 0.5 gm of phenolphthalein in 100mL, 1:1 (v/v) alcohol

water mixture.

Mixed indicator solution: Dissolve 0.02gm methyl red and 0.01gm bromocresol green in
100mL, 95 percent, ethyl or isopropyl alcohol.

8.4 PRINCIPLE

Pure water is neutral in nature with pH 7. Due to the presence of dissolved minerals in
rain water, the pH increases and becomes alkaline. Alkalinity in water is due to the presence of
hydroxide (OH–), carbonate (CO32–) and bicarbonate (HCO3–) ions. The various alkalinities

53
 are estimated by titrating the water sample against a standard acid using phenolphthalein and
methyl orange indicators successively. Hydroxide ions is completely neutralized to water using
phenolphthalein indicator (single step neutralisation)

OH– + H–  H2O
Carbonate ions is neutralized to bicarbonate ions using phenolphthalein indicator in the
first step. in the second step, these bicarbonate ions is completely neutralized to water and
carbon dioxide using methyl orange indicator (double step neutralisation).

CO32– + H+  HCO3–

HCO3– + H+  H2O + CO2

Bicarbonate ions are completely neutralized to water and carbon dioxide using methyl
orange indicator (single step neutralisation).

HCO3– + H+  H2O + CO2

8.5 PROCEDURE:
The burette is filled with standard sulphuric acid to the zero level, following
usual precautions. 20 ml of the given water sample is pipetted out into a conical flask. Two
drops of phenolphthalein indicator is added and titrated against the standard sulphuric acid. The
end point is the disappearance of pink colour. The titre value is noted as P. A drop of methyl
orange indicator is added to the same solution after the phenolphthalein end point and the titra-
tion is continued until the solution becomes orange. The total titre value is noted as M. The
titration is repeated to get concordant value and the titre values are noted in the Table.

54
 Volume of Sulphuric
Burette Reading
Volume acid consumed (ml)
S.No of water Phenolphthalein Methyl orange
sample Initial neutralization Neutralization P M
(P) (M)
1.

2.

3.

4.

5.

8.6. CALCULATIONS
Follow the below table to calculate the alkalinity of the water sample.

P=M OH- only

P=0 HCO3‒

P = ½M CO32‒

P > ½M both OH- and CO32‒ are present

P < ½M both CO32‒ and HCO3‒ are present

Phenolphthalein alkalinity

Volume of sulphuric acid (phenolphthalein end point) = ……….. ml

Strength of sulphuric acid = ………… N

Volume of water sample = …………. ml (Concordant Value)

Vacid  N acid  50 1000

Phenolphthalein alkalinity  VWatersample 55

= ppm
 8.6 REPORT
The given water sample contains

Phenolphthalein alkalinity = ppm

Methyl orange alkalinity = ppm

Note:

Interferences: Free available residual chlorine markedly affects the indicator color
response. The addition of minimal volume of sodium thiosulphate eliminates this inter-
ference. Substances such as salt of weak organic or inorganic acids present in large
amount may interfere.

Sample Preparation: The sample aliquot used for analysis should be either free from
turbidity or should be allowed to settle prior to analysis.

56
57
 DR B R AMBEDKAR OPEN UNIVERSITY
BSc 3 year 5 Semester Practical Examinations
Chemistry - 6 : Green Chemistry and Environmental Chemistry

Time: 3 hrs.] [Max. Marks: 20

--------------------------------------------------------------------------------------------------------------

1. Write the brief principle involved in the determination of toal alkalinity of

water. [5]

2. Prepare a sample of acetyl salicylic acid by microwave assisted synthesis.

Report its boiling point. [10]

3. Record [3]

4. Viva [2]

58
59