33

PRACTICAL MANUAL FOR CHEMISTRY LABORATORY

Part-1

Faculty:
Prof. Nirendra Misra (HOD) Dr. Rajib Bandyopadhyay
Dr. Anirban Das Dr. Manoj Pandey
0
 TABLE OF CONTENTS

Sr. Category Aim Page

No. No.
I General Instruction for Chemistry Laboratory 2
II Safety Instruction for Chemistry Laboratory: 4
III Safety measures in accidental case 6
1 External Indicator To determine the strength of given solution of ferrous 9
ammonium sulphate by titrating against standard N/40
K2Cr2O7 using potassium ferricyanide as an external
indicator
2 Iodometric Titration To determine the strength of given copper sulphate solution 13
by titrating against N/40 sodium thiosulphate (hypo) solution.
3 Iodimetric Titration To determine the purity of given ascorbic acid (Vitamin-C) by 16
titrating against standard N/10 iodine solution.
4 Complexometric To determine the total, permanent and temporary hardness of 19
Titration: Estimation given water by complexometric titration using standard 0.01M
of Hardness of Water EDTA solution.
5 pH-Metric Titration To determine the strength of given HCl solution using a 23
standard NaOH solution by performing a pH-metric titration
6 Conductometric To determine the strength of given HCl solution using a 26
Titration standard NaOH solution by performing a conductometric
titration.
7 Potentiometric To determine the strength of given HCl solution 30
Titration potentiometrically
8 Chemical Kinetics To study the kinetics of decomposition of sodium thiosulphate 35
by a mineral acid.
9 Estimation of Chloride To determine amount of Chloride in the given Water sample 37
in Water Sample by the Mohr Method.
10 Polymerization To prepare a polymer (Nylon 6,10) and identify the functional 39
groups by FT-IR
11 Meting Point To determine melting point of given organic compound. 43
Determination
12 Viscometer Determination of Viscosity of the Given Liquid by Ostwald 46
Viscometer

1
 I. General Instruction for
Chemistry Laboratory:
Laboratory note book:

 The one essential tool for any laboratory worker in any field is the
laboratory notebook.

 Its main purpose is to record observations, variations in procedures,

experimental results, conclusions and supplementary information from
texts, handbooks, and other printed sources.

 Laboratory records must be kept in ink.

 Never attempt to remove pages from the notebook nor to erase any
entries. Simply cross out neatly any entry you wish to delete and give the
page reference for the correction or type in the correction.

 Label the notebook on the outside and inside the front cover with your
name, roll number, batch number.

 Leave the first one or two pages blank for a Table of Contents which you
must keep up to date each week.

 Always read the upcoming experiments carefully and thoroughly, being

sure to understand all of the directions before entering the lab.

 It is essential that you come to the laboratory with a schedule of

operations planned in advance, and with all tables, equations, etc.
completed. Tables for the recording of observations should be clearly and
neatly set-up in advance.

 Take data during lab. Not after lab, on the assumption that it will be
neater. Put data directly in your lab book rather than transcribing from
another source (e.g., notebook or lab partner).

Laboratory apron:

 Laboratory aprons must be donned at all times. In the event of a spill,

these aprons are chemical and flame resistant, and could save you from
scar tissue.

2
Journal:

 One has to report experiment in reasonably neat manner in journal. A

report format for journal is given below.

 Left hand page:

o Observation

o Observation table

o Calculation

o Results

 Right hand page:

o Experiment No.

o Date & title

o General discussion

o Theory

o Reactions

o Procedure

o Precautions

3
II. Safety Instruction for
Chemistry Laboratory:
 All the laboratory apparatus should be handled properly.

 Never use the pipette with the help of mouth.

 While working with chemicals don't deviate from the instructions. One
should give attention while mixing chemicals. Don't mix them randomly
otherwise it could result in serious consequences.

 No unauthorized experiments are to be performed.

 There are different methods of disposal for different chemicals. All

chemicals shouldn't be washed down the drain. You must wash away the
chemicals in the sink.

 Never eat or drink anything in lab.

 Don’t sniff or taste chemicals. Even sniffing of some hazardous chemicals

can harm you.

 Never directly smell the source of any vapour or gas; instead by means of
your cupped hand, waft a small sample to your nose. Do not inhale these
vapours but take in only enough to detect an odour if one exists. For
many chemicals, if you can smell them then you are exposing yourself to a
dose that can harm you!

 Wash your hands frequently during lab, and definitely wash your hands
twice at the end of the lab, once in the lab itself, and again outside of lab,
especially before eating.

 Clean up all broken glassware immediately and dispose of the broken

glass properly.

 Beware of hot glass--it looks exactly like cold glass.

 Never pick up broken glassware with your bare hands, regardless of the
size of the pieces.

 Never put broken glass in a regular garbage can. A container is provided

that is especially for broken glassware.

 Never use reagents from an unmarked bottle.

4
 If a fire should occur in a beaker or some other container, cover it with a
glass dish or other flame-retardant item.

 Never move any object that is burning.

 Never use water to extinguish a chemical fire.

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

 Notify the instructor immediately in case of an accident.

5
 III. Safety measures in accidental
case:
Eye accidents:

 Flood your eyes immediately with water.

 For an acid, use dilute Sodium bicarbonate solution; for an alkali, use
dilute boric acid solution.

Burns:

 Acid burns: wash immediately with large quantities of water, then with
dilute (8%) sodium bicarbonate solution. If burn is severe, wash again with
water and apply the acriflavine.

 Alkali burns: wash immediately with water and 1% acetic acid solution.

 Bromine burns: wash immediately with ample supply of petrol, when the
bromine will be completely removed from skin.

 Organic substances: wash immediately with soap and warm water.

Cuts:

 Wash the wound with sterile gauze, soap and water. Disinfect with an
antiseptic and apply a bandage.

Reagents in mouth:

 If the reagents is in the mouth and not swallowed then spit out at once,
and wash the mouth out repeatedly with water.

 If the substance like acid or alkali is swallowed, dilute by drinking much

water. Then for acids follow by drinking much lime water. Milk may be
given but no emetics.

 For salts of heavy metals give milk or white of egg.

 For arsenic or mercury compounds give emetic without any delay.

Gas poisoning:

 Remove patient to fresh air and loosen clothing at neck. If breathing has
stopped, give artificial respiration until the doctor arrives.

6
Proper Handling of Chemicals and Equipment:

 Consider all chemicals to be hazardous unless you are instructed

otherwise.

 Know what chemicals you are using. Carefully read the label twice before
taking anything from a bottle.

 Never take excess of reagents than required.

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

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

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

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

 Never point a test tube or any vessel that you are heating at yourself or
your neighbor--it may erupt like a geyser.

 Dispose of chemicals properly. Unless you are explicitly told otherwise,

assume that only water may be put in the lab sinks. Some chemicals can
be washed down the drain, while others require a different method of
disposal. If a chemical can go in the sink, be sure to wash it away rather
than risk an unexpected reaction between chemical 'leftovers' later.

 Report all chemical spills immediately to your lab supervisor.

 Small spills on bench or floor must be cleaned up immediately. Neutralize

all acids and alkaline spills before cleaning.

 Be especially careful of spills around the balances.

 Before using burner, be sure nobody else on the bench has any organic
solvents.

 Before getting any organic solvents, be sure nobody on your entire lab
bench has an open flame.

7
 Never leave burners unattended. Turn them off whenever you leave your
workstation. Be sure that the gas is shut off at the bench rack when you
leave the lab.

 Never look down while opening of any container, including beakers, flasks,
and test tubes.

 Do not use graduated cylinder for any purpose other than to measure a
volume of liquid. Graduated cylinders should not be used to get reagent
for an experiment or to run reactions.

 Never put a dropper into a reagent bottle. Instead, put the reagent in a
beaker so you can bring it back to your desk and use dropper there.

8
1. EXTERNAL INDICATOR
Aim: To determine the strength of given solution of ferrous ammonium sulphate
by titrating against standard N/40 K2Cr2O7 using potassium ferricyanide as an
external indicator.

Principle:

Acidic K2Cr207 is a strong oxidizing agent. When it is added to ferrous ammonium

sulphate solution containing dilute H2SO4, only FeSO4 is oxidized and (NH4)2SO4
remains unchanged hence not shown in the equation. The reactions taking place
are as follows:

K2Cr2O7 + 4H2SO4  K2SO4 + Cr2(SO4)3 + 4H2O + 3O

6FeSO4 + 3H2SO4 + 3O  3Fe2(SO4)3 + 3H2O

The complete reaction is:

K2Cr2O7 + 6FeSO4 + 7 H2SO4  3Fe2(SO4)3 + K2SO4 + Cr2(SO4)3 + 7H2O

Or

Ionically, (Cr2O7)-2 + 14H+ + 6Fe2+  6 Fe3+ + 2Cr3+ + 7H2O

The end point on potassium dichromate titration is usually determined by using

two types of indicator. External indicator was once employed when no internal
indicator was available. Here the indicator cannot be added to the solution to be
titrated, but is placed in the depressions of a white glazed groove tile. About
0.1% solution of potassium ferricyanide acts as external indicator. Freshly
prepared pot. Ferricyanide indicator is used because the old solution of it
becomes contaminated with potassium ferrocyanide. The use of potassium
ferricyanide as an external indicator is the best known example in the titration of
iron with dichromate. As long as ferrous ion is present in the titration mixture, the
indicator will turn blue on the transfer of solution. The appearance of blue colour
is due to the formation of ferroferricyanide (Turnbull’s blue) according to flowing
reaction.

9
2K3Fe(CN)6 + 3FeSo4  Fe3[Fe(CN)6]2 + 3 K2SO4

Ferrous ferricyanide

Dark blue complex

Usually at the end point (all Fe+2 ions are oxidized to Fe+3) the colour of the
indicators drop becomes light brownish yellow due to reaction of indicator with
Fe+3 ions to produce brown coloured ferric ferricyanide complex.

Fe2(SO4)3 + 2K3[Fe(CN)6]  3K2SO4 + 2Fe[Fe(CN)6]

Yellowish brown

Thus, at the end point, the indicator fails to produce blue colour when treated
with a drop of titration mixture.

Regents:

0.1% solution of potassium ferricyanide, standard N/40 K2Cr2O7 potassium

dichromate, ferrous ammonium sulphate, dilute sulphuric acid.

Apparatus:

Pipettes, burette, conical flask, glass rod, test tubes, white glazed tile.

10
Procedure:

1. Rinse and fill burette with standard N/40 K2Cr2O7 solution.

2. Pipette out 10ml of given ferrous ammonium sulphate solution in a clean

conical flask and add to it about equal volume of dilute H2SO4.

3. Put a series of drops of indicator (potassium ferricyanide solution) with the

help of glass rod, on a white tile/ plate.

4. Titrate the ferrous ammonium sulphate with standard solution of K 2Cr2O7 from
the burette.

5. Near end point, take a drop of titration mixture and put it on one of these drops
on time and see the colour.

6. A strong blue colour will be produced. Continue the titrations and repeat the
process at different intervals and when the colour of indicator drop does not give
blue colour, the end point is reached. Note the reading of the burette. Repeat the
titration to get the exact end point.

Observations:

Burette: standard N/40 K2Cr2O7 solution

Pipette: 10 ml of ferrous ammonium sulphate solution

Indicator: 0.1% solution of potassium ferricyanide (freshly prepared)

Colour change: Prussian blue to yellowish brown

Observation Table:

Burette Reading K2Cr2O7

used (ml) Vol of K2Cr207
Sr. No Vol. of FAS used
used (ml)
Initial Final

1. 10ml 0.0ml ………. ……ml

2. 10ml 0.0ml ………. ……ml

3. 10ml 0.0ml ………. ……ml

11
Calculation:

Volume of unknown ferrous ammonium sulphate X normality of unknown ferrous

ammonium sulphate = Volume of standard K2Cr2O7 X normality

10 X N1 = V2 (Burette reading) X 0.025

N1= 0.025 X Burette reading

10

= ------------ N

Strength = Normality of ferrous ammonium sulphate X Eq. weight of ferrous

ammonium sulphate

=..................................g./L

Result:

The strength of given unknown ferrous ammonium sulphate is ..................... g./L

12
2. IODOMETRIC TITRATION

Aim: To determine the strength of given copper sulphate solution by titrating

against N/40 sodium thiosulphate (hypo) solution.

Principle:

Iodometric titrations are defined as those iodine titration in which some oxidizing
agent liberates iodine from iodide solution and then liberated iodine is titrated
with a standard solution of a reducing agent added from burette. In such titration,
a neutral or an acidic solution of oxidizing agent is employed. The amount of
liberated iodine from an iodide (i.e. KI) is equivalent to the quantity of the
oxidizing agent present. Iodometric titrations are used for the determination of
CuSO4, k2Cr2O7, KMnO4, ferric ions, antimonite ions, H2O2, MnO2, Bromine and
Chlorine etc.

The strength of copper sulphate is determined by Iodometric method. When KI is

added to a solution of copper sulphate a white cuprous iodide, Cu 2I2 is precipitate
and an equivalent amount of iodine is liberated. The free iodine is titrated with
standard solution of hypo, using starch an indicator. As soon as all the liberated
iodine has been reduced to iodide (NaI), the blue color of iodo-starch complex
will disappear and the colour of precipitate in conical flask will be white that is of
cuprous iodide. This indicates the endpoint.

The chemical reactions taking place are:

2CuSO4 + 4KI → Cu2I2↓ + 2K2SO4 + I2

White ppt.

2Na2S2O3 + I2 → Na2S4O6 + 2NaI

Sodium tetrathionate

13
Reagents:

Copper sulphate (penta hydrate) solution, Standard N/40 sodium thiosulphate

solution (hypo), starch Solution, KI crystals

Apparatus:

Pipette, burette, conical flask, weighing machine, paper to cover flask

Procedure:

1. Clean the burette and fill with hypo solution and note the initial reading.
Pipette out 10 ml of copper sulphate solution in a clean conical flask.

2. Now add 0.5 gm solid KI, mix well and cover the mouth of conical flask by
watch glass or paper and allow the mixture to stand for 2-5 minutes in the dark.

3. The solution becomes brown in colour due to liberated iodine. Now titrate the
liberated iodine with the hypo solution added from burette.

4. The brown colour of iodine fades slowly and when only a very faint yellow
colour (light straw colour) remains, adds 1 ml of starch solution.

This immediately forms a deep blue iodo-starch complex. Now, add further hypo
solution drop by drop, shaking well in whirling motion and titrate till the blue
colour just disappears. If the colour does not return within 10 seconds, this will
indicate end point. Note this burette reading. Repeat the titration until two
concordant readings are obtained.

Observation:

Burette: N/40 sodium thiosulphate (hypo) solution

Pipette: 10 ml of copper sulphate solution

Indicator: Starch solution (freshly prepared)

Color change: Blue to colorless (white ppts.)

14
Observation table:

S. No. Volume of Burette reading (ml) Vol. Of hypo

copper solution used
sulphate Initial final (ml)
taken

1. 10 ml

2. 10 ml

3. 10 ml

Calculation:

Volume of unknown copper sulphate solution X normality of unknown copper

sulphate solution= Volume of hypo solution X normality of hypo solution

10 X N1 = V2 (Burette reading) X N2

N1= 0.025 X Burette reading

10

Strength = Normality of copper sulphate X Eq. weight of copper sulphate

=..................................g/L

Result:

The strength of given unknown copper sulphate is .....................g/L.

15
3. IODIMETRIC TITRATION

Aim: To determine the purity of given ascorbic acid (Vitamin-C) by titrating

against standard N/10 iodine solution.

Principle:

Iodimetric titrations are defined as those iodine titrations in which a standard

iodine solution is used as an oxidant and iodine is directly titrated against a
reducing agent. Iodimetric procedures are used for the determination of reducing
agents like thiosulphate, sulphate, arsenates and stannous chloride etc. by
titrating against standard solution of iodine taken in a burette.

The titration of a reducing agent such as ascorbic acid with iodine (I 2, generally
present as I3- , triiodide ion) to produce iodide ion (I -) is referred to as an
Iodimetric titration.

C6 H8 O6 + 2 H2O + I2  C6 H6 O6 + 2 I - + 2 H3O +

Ascorbic acid ( vit – C) excess

Reagents:

Standard N/10 Iodine, Ascorbic acid, dilute H2SO4, freshly prepared 1% starch
solution

Apparatus:

Burette, conical flask, measuring cylinder, weighing balance etc.

Procedure:

16
1. Clean the burette and fill with standard N/10 Iodine solution and note the initial
reading.

2. Take 0.100 g. (100 mg) of given ascorbic acid powder in a clean conical flask
and dissolve it in 50 ml. of Distilled water (CO2 free distilled water)

3. Then add 10 ml of dilute H2SO4 solution and 1 ml. of freshly prepared 1%

starch solution.

4. Mix well and titrate with N/10 iodine solution, swirling the titration flask after
each addition of iodine until a permanent blue color is just obtained.

This is the end point. Note the burette reading and repeat the titration until two
concordant values are obtained.

Observation:

Burette: N/10 standard Iodine solution

Conical flask: 0.1 g. Ascorbic acid sample + 50 ml. distilled water + 10 ml. dilute
H2SO4 + 10 drops of 1% starch solution

Indicator: 1% Starch solution (freshly prepared)

Color change: Colorless to permanent blue color

Observation table:

Sr. Weight of Ascorbic Volume of N/10 % Purity of the

No. Acid (in gram) Iodine solution (in sample
ml)

1.

2.

3.

Calculation:

1 ml of 0.1 N I2 solution ≡ 0.008805 gm of ascorbic acid

Then,
17
Weight of ascorbic acid in 0.1 g. sample = 0.008805 X Burette Reading (in ml.)

=…………………g. of ascorbic acid in

0.1g.sample.

% Purity of Ascorbic acid = g. of Ascorbic acid X 100

________________________

Weight of sample taken (in g.)

Result:

Purity of given Ascorbic acid (Vitamin-C) sample is _________ %

18
4. COMPLEXOMETRIC TITRATION:
ESTIMATION OF HARDNESS
Aim: To determine the total, permanent and temporary hardness of given water
by complexometric titration using standard 0.01M EDTA solution.

Principle:

Hard water is due to metal ions (minerals) that are dissolved in the ground water.
Generally water contaminated with Ca or Mg salts is called hard water. When
impurities are in form of bi carbonate salts, they are easily removed by boiling as
boiling decomposes bi carbonates to insoluble carbonates. It is said to be
temporary hardness. When they are in in form of chlorides or nitrates etc. it is
called permanent hardness.

A complex is a molecule or ion formed by the reaction of two or more ions or

molecules capable of independent existence. A metal atom can usually form a
bond with one or more donor atoms which have at least one unshared pair of
electrons. The number of donor atoms which bond with a given atom depends
on the number of electron pairs that the metal ion can accept, in other words, the
coordination number of the metal ion. Complexing agents, or ligands, which can
provide more than one pair of electrons (multidentate ligands), are also called
chelating agents.

Many metals forms complexes with such reagents as contain appropriate

ligands. The most important chelating agent in analytical chemistry is ethelyene
diamine tetra acetic acid (EDTA). The tetra basic form of this acid forms
complexes with virtually all metal ions. EDTA is a hexadentate ligand; each of
the acid oxygen and each of the amine nitrogen can donate one electron
pair. The metal ion is usually held in a one-to-one complex with EDTA. The
complexes have four or five 5-membered rings, contributing significantly to their
stability. Dissociation constant values indicate that EDTA behaves like a
dicarboxylic acid. That is two of its carboxyl groups are strongly acidic and other
two hydrogen are released during formation of complex. In forms of its disodium
salt, it is used to estimate Ca++ and Mg++ ions.

It is important to realize that the electron pairs of the carboxylic acid groups of
EDTA are only available to the metal ion when the acid is dissociated. This
means that the effectiveness of the complexing agent is strongly affected by
pH. At low pH EDTA will be in the acid form and will not be an effective
complexing agent. Additionally, many metal ions form complexes with hydroxide

19
ions. Hydroxide ions compete with the chelating agent for coordination sites in
the metal ion. Therefore, the effectiveness of the complexing agent will also be
reduced at high pH. For a given chelating agent and metal ion, there will be an
optimum pH for the titration which will depend on the pK a values for the chelating
agent and the formation constants for the metal-hydroxide complexes. Therefore
suitable buffer solution is added to keep pH of the solution nearly constant and
pH sensitive indicators are used. In the estimation of hardness with EDTA, an
azo dye called Eriochrome Black-T is used as an indicator. This forms a metal
indicator complex, the stability of which is lower than that of the metal EDTA
complex. The solution is initially red due to metal ion indicator complex. As the
titration proceeds, the metal ions forms more stable complex with EDTA, hence
the indicator anion goes in to solution. As the indicator accumulates the colour
changes from red to blue at the end point.

Reagents:

Given sample of hard water, standard EDTA solution, buffer solution (pH=10),
solution of Eriochrome Black-T

Apparatus:

Pipettes, burette, conical flasks, hot plate.

Procedure:

Total hardness:

Clean the burette and fill with standard EDTA solution and note the initial
reading.

Pipette out 25 ml of given hard water in a clean conical flask.

Add 5 ml of buffer solution (pH=10) and 4-5 drops of indicator.

Titrate it against standard EDTA solution.

At the end point colour changes from red to blue.

Repeat it for two concordant readings.

Permanent hardness:

Take another 25 ml sample of same water and boil it for aout 15-20 minutes. This
will make temparory hardness to precipitate.

Filter it off and titrate the filtrate as described above.

Observation:

Burette: standard EDTA solution

20
Pipette: 25 ml of given water sample + 5 ml of buffer solution (pH=10)

Indicator: Eriochrome Black-T

Colour change: red to blue

Observation table:

Total hardness:

S. No. Volume of Burette reading (ml) Vol. Of EDTA

water sample solution used
taken Initial final (ml)

1. 25 ml .........ml

2. 25 ml .........ml

3. 25 ml .........ml

V2=.........ml

Permanent hardness:

S. No. Volume of Burette reading (ml) Vol. Of EDTA

water sample solution used
taken Initial final (ml)

1. 25 ml .........ml

2. 25 ml .........ml

3. 25 ml .........ml

V2=.........ml

Calculation:

Total hardness:

Total hardness (mg/L as CaCO3) =

Burette reading X M EDTA X MW of CaCO3 X1000

Volume of sample

21
Permanent hardness (mg/L as CaCO3) =

Burette reading X M EDTA X MW of CaCO3 X1000

Volume of sample

Subtract value of permanent hardness from total harness to get value of

temporary hardness

Result:

Total hardness (mg/L as CaCO3) =………………………

Permanent hardness (mg/L as CaCO3) =………………..

Temporary hardness (mg/L as CaCO3) = …………………

22
5. pH-METRIC TITRATION:
Aim: To determine the strength of given HCl solution using a standard NaOH
solution by performing a pH-metric titration

Principle:

In this experiment, the pH of a solution is utilized as an indicator for determining

the end-point of a strong acid-strong base titration. The base solution is standard
while the concentration of acid is unknown.

A fixed quantity of solution of strong acid is taken in a beaker and its’ initial
pH is recorded. To this, if we start adding a strong base solution, we find that the
pH of the reaction mixture follows a graph of the following type:

Volume of base added

Apparatus Required:

1. pH-meter
2. Burette (50 ml)
3. Measuring cylinder 10 ml.
4. Beaker (100 ml)
5. Measuring Cylinder (100 mL)
6. Volumetric Flask (100 ml)

Reagents Required:

1. ‘X’ N HCl solution

2. NaOH Solution (1N)

23
Procedure:

Preparation of 0.1 N NaOH solution:

Take 10 ml of the given 1N NaOH solution by using 10ml.measuring cylinder and

transfer it to a 100 ml. volumetric flask. Dilute it up to the mark with distilled
water.

Performing the Titration:

1. Wash the burette with distilled water and mount it on the stand.
2. Fill the 0.1 N NaOH solution (prepared earlier) into the burette.
3. Using a pipette, take out 30 mL of given HCl solution into a 100 mL
beaker.
4. Dip the pH electrode into the beaker and turn the pH-meter on. Measure
the initial pH of the acid solution.
5. From the burette, start adding the NaOH solution in 1 ml. increment. Note
down the pH after each increment.
6. Continue with the previous step till about the pH 12 and then empty the
burette into a waste container.
7. Plot a graph between the observed pH value and the volume of NaOH
solution added. Locate the end point as the point of maximum slope on
the graph (see figure in theory).
8. Calculate the strength using the data obtained.

Observation Table:

Sr. No. Volume of 0.1 N NaOH pH

added
1 0.0 ml.
2 1.0 ml.
3 .
4 .
5 12

24
Calculations:

N1V1 = N2V2

N1= Concentration of acid,

N2= Concentration of NaOH (0.1)
V1= volume of acid taken = 10 mL, and
V2= volume of base required for complete neutralisation (read from the graph)

Once the normality of HCl is calculated, its strength in g/L can be calculated by
multiplying the Normality with the molecular weight:
Strength (in g/L) = N1 X Molecular weight of HCl

Result:

The strength of HCl solution is -------------- g/L.

Precautions:

Electrode is very costly as well as delicate. Handle electrode with care.

Do not keep electrode outside in open air. Always dip electrode in distilled water.
This is very important part of this experiment.

25
6. CONDUCTOMETRIC TITRATION
Aim: To determine the strength of given NaOH solution using a standard 1N HCl
solution by performing a conductometric titration

Apparatus Required:

1. Conductometer
2. Burette (50 ml)
3. Measuring Cylinder (100 mL)

Reagents:

1. 1N HCl
2. xN NaOH

Theory:

The specific electrical conductivity and the electrical conductance are a measure
of the ability of a solution, a metal or a gas – in brief all materials – to conduct an
electrical current. In solutions, the current is carried by cations and anions
whereas in metals it is carried by electrons. If a substance has a high electrical
conductance G, the electrical or ohmic resistance R is low. The electrical
conductance G is the reciprocal of the resistance R:

The unit of R is the Ohm and the unit of G is the Siemens.

To measure the electrical conductance, a voltage is applied to the electrode pairs

and the current that flows is measured. During this process, the cations migrate
to the negative electrode, the anions to the positive electrode and the solution
acts as an electrical conductor.

A conductor is defined by its length and cross-section. The smaller the electrode
gap l and the larger the electrode area A, the larger the measurable current at
the same electrolyte concentration and same voltage. The electrical conductance
G is given by the equation:

26
Where A is the electrode area, l the electrode gap, γ is the specific conductivity
and ρ the specific resistance. γ and ρ are material constants with the units S/m
and Wm. This equation also illustrates the relation between the specific
conductivity γ and the conductance G.

The quotient of the length and area is the cell constant K(resulting in the unit m-
1
):

In this experiment, the conductivity of a solution is utilized as an indicator for

determining the end-point of a strong acid-strong base titration. The base
solution is standard while the concentration of acid is unknown.

A fixed quantity of the solution of strong acid is taken in a beaker and its’ initial
conductivity is recorded. Being a strong electrolyte, the conductivity value will be
large. To this, if we start adding a strong base solution, we find that the
conductivity falls slightly in the beginning. This is because the added strong
electrolyte is consumed completely in the neutralization reaction, and hence the
ionic concentration doesn’t appreciate much. On the other hand, dilution of the
existing ions due to increase in volume causes the conductivity to decrease.
However, as soon as the equivalence point is reached, the added ions of the
strong base remain free in solution, and hence beyond this point, further addition
of base leads to a sharp rise in the conductivity of the solution.

To determine the end point, the observed conductivity of the solution is plotted
against the volume added. Conductivity values follow two distinct linear trends
before and after the equivalence point, as can be seen in the following schematic
diagram:

27
Procedure:

Performing the Titration:

1. Wash the burette with distilled water and mount it on the stand.
2. Fill the 1N HCl solution (prepared earlier) into the burette.
3. Using a 100 mL measuring cylinder, take out 200 mL of x N NaOH
solution into a 250 ml beaker.
4. Dip the conductivity cell into the beaker and turn the conductometer on.
Note down initial conductance in ms.
5. From the burette, start adding 1N HCL solution with 1 ml increment. Note
down the conductivity after each increment.
6. Plot a graph between the observed conductivity (ms) value and the
volume of 1N HCL added. Locate the end point as the intersection of the
two lines (see figure in theory).
7. Calculate the strength using the data obtained from graph.

Observation Table:

Sr. No Volume of 1N HCl Conductance(ms)

added(ml)
1. 0.0(initial)
2. 1.0
3. 2.0
. .
. .
41. 40.0

Calculations:

1) Normality of HCl :

N1V1 = N2V2

Here,

N1= Concentration of base = x N,

28
V1= volume of base 200 ml and
V2= volume of acid (read from graph)
N2= Concentration of acid 1N.

Once the normality of NaOH is calculated, its strength in g/L can be calculated by
multiplying the normality with the molecular weight/ equivalent weight.

Strength (in g/L) = N1X 36.5

Result:
The strength of NaOH solution is g/ml.

Precautions:
 Electrode is very costly as well as delicate. Handle electrode with care.
 Do not keep electrode outside in open air. Always dip electrode in given
KCl solution. This is very important part of this experiment.

29
7. POTENTIOMETRIC TITRATION
Aim: To Determine the Normality of Acetic Acid Potentiometrically.

Requirements:

Sodium Hydroxide Solution (NaOH), Standard Hydrochloric Acid Solution (HCl),

Quinhydrone, Calomel Electrode, Platinum Electrode, Potentiometer, Burette,
Pipette.

Principle:

Many Acid-Base titrations are difficult to accomplish using a visual indicator for
one of several reasons. Perhaps the analyst is colour-blind to a particular
indicator color change; there may not be a suitable colour change available for a
particular type of titration or the solutions themselves may be coloured, opaque
or turbid. It may be desired to automate a series of replicate determinations. In
such situations, potentiometric titration, using a glass hydronium ion selective
electrode, a suitable reference electrode and a sensitive potentiometer (a pH
meter) may be advantageous.

Any acid-base titration may be conducted potentiometrically. Two electrodes,

after calibration [to relate potential in millivolts (mV) to a pH value] are immersed
in a solution of the analyte. One is an indicator electrode, selective for H3O+ and
the other a stable reference electrode. The potential difference, which after
calibration is pH, is measured after the successive addition of known increments
of acid or base titrant.

When a potentiometric titration is being performed, interest is focused upon

changes in the EMF of an electrolytic cell as a titrant of known concentration is
added to a solution of unknown. The method can be applied to all titrimetric
reactions provided that the concentration of at least one of the substances
involved can be followed by means of a suitable indicator electrode.

30
The critical problem in a titration is to recognize the point at which the quantities
of reacting species are present in equivalent amounts. The titration curve can be
followed point by point, plotting as ordinate, successive values of the cell EMF
(pH) vs. the corresponding volume of titrant added.

Procedure:

Take 10mL of HCl in a 250ml beaker. Add about 100mL of distilled water. Add a
pinch of quinhydrone to saturate the solution. Dip calomel and platinum
electrodes in the solution and connect them to potentiometer. Now, from the
burette add 1mL of NaOH, stir and then note the value of EMF in potentiometer.
Continue to take reading after every addition of 1mL of NaOH. The emf goes
decreases continuously. At a certain point, the polarity is reversed. After
reversing of the polarity, take at least 5 more readings. From the preliminary
titration, find out approximate end point.

Repeat the titration by again preparing the same set and adding 0.2mL of NaOH
near the end point. Subsequent addition can be in 1mL. Repeat the same
procedure with acetic acid solution.

31
Observation:

Volume of
Sr. Emf (E) E
alkali (V) ∆E ∆V
No. observed (mV) V
added (mL)

32
 Volume of
Sr. Emf (E) E
alkali (V) ∆E ∆V
No. observed (mV) V
added (mL)

33
Calculation:

Plot (i) Emf vs Volume of alkali and

E
(ii) vs Volume of alkali.
V

From the graph, evaluate the exact volume of alkali required to neutralize the
given acid and calculate the normality using.

N1 V1 = N2V2

Result:

Normality of Acetic Acid is _____________N.

34
8. CHEMICAL KINETICS

Aim: To study the kinetics of decomposition of sodium thiosulphate by a mineral

acid and also find concentration of unknown given sample.

Principle:
The decomposition of sodium thiosulphate in hydrochloric acid takes place
according to the following equation:
Na2S2O3 + HCl → 2 NaCl + H2O+ SO2↑+ S↓

The precipitation of sulphur is marked by turbidity in solution and this indicates

the progress of the reaction. The acid is taken in large excess to keep its
concentration more or less constant and solutions of various concentrations of
sodium thiosulphate are used to study the kinetics.

Reagents:
Sodium thiosulphate, N/2 hydrochloric acid
Apparatus:
Measuring cylinder, 5-6 beakers of 250 ml, stop watch, thermometer.

Procedure:
1. Weigh accurately 0.2, 0.4, 0.6, 0.8, and 1.0,a and X gm of sodium thiosulphate
and transfer it to a 5 beakers. Make their solutions in small amount of water and
make each up to 100ml and label them.
2. Add 20 ml of N/2 HCl in first beaker and run the stop watch.

3. Make a big cross mark on a white paper and put beaker on it. View the cross
from above through the solution.

4. The moment the cross mark becomes invisible, stop the stop watch and note
the time taken.

5. Repeat the same experiment with remaining four beakers.

6. Plot the graph, taking amount of sodium thiosulphate per 100 ml of solution on
y axis and reciprocal of time required to bring turbidity on x-axis. It gives a linear
pattern.

35
Observation:
Experimental temperature: …………………………..°C

Observation table:

Amount of sodium Time required for Reciprocal o time

thiosulphate taken Volume of N/2 turbidity ‘t’ 1/t
in gm per 100ml HCl
added (in ml)

0.2 20
0.4 20
0.6 20
0.8 20
1.0 20
X 20

The data tell that the reaction is of first order with respect to sodium thiosulphate
as reciprocal of time required for turbidity is proportional to initial concentration of
thiosulphate.

Result:
Since the graph is linear (straight line), the decomposition of thiosulphate by
mineral acid is a first order reaction.

From the graph, the unknown concentration can be determined by extrapolating

the 1/t value of the same in the X-axis to the straight line and then further to the
Y axis

36
9. ESTIMATION OF CHLORIDE IN
WATER SAMPLE
Aim: To determine amount of Chloride in the given Water sample by the Mohr
Method.

Principle:

The Mohr method uses chromate ions as an indicator in the titration of chloride
ions with a silver nitrate standard solution. On gradual addition of AgNO 3 solution
AgCl, precipitates at first. After all the chloride has been precipitated as white
silver chloride, the first excess of titrant results in the formation of a brick -red
coloured precipitate of silver chromate, which signals the end point. This is a
precipitation titration. Precipitation titrations are based upon reactions that yield
ionic compounds of limited solubility. The most important precipitating reagent is
silver nitrate. Titrimetric methods based upon silver nitrate are sometimes termed
argentometric methods.

The reactions are:

AgNO3 + NaCl →AgCl↓+ NaNO3

2AgNO3 + K2CrO4 → Ag2CrO4↓ + 2KNO3

Or ionically,

Ag+ + Cl- → AgCl(s) ↓

2Ag+ + CrO42- → Ag2CrO4 (s)↓

By knowing the stoichiometry and moles consumed at the end point, the amount
of
chloride in an unknown sample can be determined.

Reagents:

Given water sample, standard N/10 AgNO3 Solution, 5% aquous solution of

K2CrO4

Apparatus:

Pipettes, burette, conical flasks

Procedure:

Clean the burette and fill with standard AgNO3 solution and note the initial
reading.

37
Take 25 ml of given water sample in conical flask.

Add 1 ml of 5% aqueous solution of K2CrO4.

The mixture is titrated keeping flask against white background with standard
AgNO3 with constant shaking so that red colour produced by adding of each drop
gradually disappears.

When the red colour begins to disappear very slowly, AgNO 3 solution is added
dropwise until a pale brown colour persists after swirling the liquid.

The titration is repeated for concordat readings.

Observation:

Burette: standard N/10 AgNO3 Solutions.

Pipette: 25 ml. of water sample (chloride sample)

Indicator: 1 ml of 5% aqueous solution of K2CrO4

Color Change: yellow to brick red.

Observation table:

Sr. No. Volume of Burette reading (ml) Vol. Of N/10

water Initial Burette Final Burette AgNO3 used
sample Reading Reading (ml)
taken (ml)
1. 25 ml .........ml
2. 25 ml .........ml
3. 25 ml .........ml

Calculation:

Chloride (mg/L) = Burette reading X N of AgNO3 X 35 X 1000

Volume of sample

Results: The chloride in the given water sample = mg/L.

38
10. POLYMERIZATION
Aim: To prepare a polymer (Nylon 6, 10) and identify the functional groups by
FT-IR

Principle:

Synthesis of an Amide:
By using a carboxylic acid chloride, a more reactive carboxylic acid
derivative, the rate of reaction can be increased. In this reaction, HCl is
the by-product.
H O H O

R N + C R R N C R+ HCl

H Cl

amine Acid chloride amide

Synthesis of Nylon 6, 10 :
In order to make a polyamide, such as Nylon 6, 10, the amine molecule
must have a –NH2 group at each end, and the acid chloride must have a
–COCl group at each end.
The diamine and the diacid chloride bond together, end-on-end, to form
very long chains.
Nylon 6,10 is made from hexamethylene diamine (the diamine) and
sebacoyl chloride (the diacid chloride).

39
Mechanism:

Reagents: sebacyl chloride, hexane, 1,6-hexanediamine, 3% sodium hydroxide.

Reagent Preparation (mix in hood):

1. Dissolve 1 mL of the sebacyl chloride in 50 mL of hexane. Label Solution
SC
2. Dissolve 2.5 mL of 1,6-hexanediamine in 25 mL of 3% sodium hydroxide.
Label solution diamine.

40
Apparatus:

glass rods, beakers

Procedure:

1. Take 10 mL of the diamine solution and place in a beaker (50mL,

200mL or 400mL)
2. Carefully and gently pour 20 mL of the SC solution over the diamine
solution so as to form two layers. This can be accomplished either by
pouring down the side of the beaker or by using a funnel held just above
the surface of the other solution.
3. Reach to the interface with tweezers, grasp the polymeric film, and
SLOWLY withdraw it from the beaker. Using a glass stir rod or a large
test tube, WIND the nylon rope until one of the reagents is exhausted.
SLOW pulling will help to avoid incorporating of the solutions into the
nylon rope. You can overlap the rope on the glass rod.

4. Using a squirt bottle, wash the product first with water and then with
Acetone to speed the drying as well as to remove more of the reagents.
5. Measure the rope when you are done (you may want to go out into the
hallway).
6. How many meters of nylon rope did you get from your 30 mL of reagent?

Mass:
1. Pour 5 mL of the diamine solution into a beaker (50mL, 200mL or 400mL)
2. Slowly pour 10 mL of the SC solution into the beaker containing the
diamine solution. A white film should form at the interface of the two
layers.
3. Reach into the beaker with forceps and grasp the film in the center of the
beaker. Slowly pull straight up. Be careful not to let the thread of nylon
touch the sides of the beaker. Pull the nylon from the beaker and wrap the
thread around a large test tube.
4. Rotate the tube, counting revolutions, until no more nylon can be
obtained.
5. Record the number of revolutions of the nylon, along with the
circumference and diameter of the test tube used in the data section of
your laboratory notebook.
6. Wash the nylon with water and then with acetone to hasten the drying
41
 process. Press the washed nylon between paper towels until no more
water can be removed.
7. Finally, calculate the length of the nylon string produced in your
experiment using the following formula:
Nylon produced (meters) = Diameter of test tube * π * # test tube
revolutions (Where π = 3.14)
8. After thoroughly drying your nylon, obtain its mass (weight it on the
balance) and calculate your final % yield.

Observation:

Calculation:

Calculate the length of the nylon string produced in your experiment using the
following formula:

Nylon produced (meters) = Diameter of test tube * π * # test tube

revolutions (Where π = 3.14)

Results:

42
11. MELTING POINT DETERMINATION

Aim: To determine melting point of given organic compound.

Principle:

The melting point (mp) of a substance is one of the physical properties that
chemists use to identify a substance. The melting point is the temperature at
which a substance changes from a solid to a liquid state. A pure crystalline
organic compound usually has a sharp and characteristic melting point range
of 0.5 to 1 °C. The melting point range is determined by recording the temp at
which melting first begins and the temp at which melting is complete.
Impurities often depress the melting (freezing) point of a substance. They
also increase the range of melting. When a sample melts at a lower than
expected temperature over an extended range, this is a sign that the sample
was not pure. Consequently, the melting point of a compound is also a
criterion for purity and well as for identification.

A technique known as a "mixed melting point" may be used as additional

evidence in identifying a given compound. First, a melting point is taken of the
unknown and a tentative identification is made using literature data. Then the
unknown sample is mixed with some authentic sample of the suspected
compound and the melting point is taken of the mixture. If the mixture shows
no depression in the melting point, the two compounds almost certainly were
the same and the identification of the unknown is confirmed. If the mixture
shows a depression of melting point, the two compounds were not identical.

Often solid substances undergo some unusual behavior prior to actual

melting. Compounds may decolorize, decompose, soften, or shrink. It is
normal for compounds to appear to shrink immediately before melting. Actual
melting begins when the first drop of liquid becomes visible.

The apparatus most commonly used in the student laboratory for melting
point determinations is the Thiele tube. It is a glass vessel filled with oil and
so designed that the oil is efficiently circulated by convection currents when
the vessel is heated at the point shown in the figure- 1. Heating is generally
done with the small flame from a micro-burner.

The thermometer is held in the place indicated by a split stopper. The stopper
has a ‘V’ shaped groove cut in the side to allow for air and oil expansion when
the vessel is heated and also to expose that portion of the thermometer scale
which would otherwise be covered by the stopper. The capillary tube is held
43
in place by a rubber band cut from a small piece of rubber tubing. The bottom
of the capillary containing the sample is placed as close to the centre of the
thermometer bulb as possible. The bath oil is a stable, high boiling liquid. It
should not be heated much above 200°C.

Figure-1 Melting point apparatus

Reagents:

Given unknown organic compound

Apparatus:

Melting point apparatus, capillary tubes,

44
Procedure:

The compound whose melting point to be determined, is powdered

thoroughly on a plate with help of a spatula.

A capillary tube is sealed at one end by heating in a Bunsen flame.

It is then filled up to about 1cm length with the powdered substance.

The capillary is then attached to the lower end of the thermometer as shown
in figure.

The thermometer is placed in a Thiele’s tube filled with paraffin oil or

concentrated sulphuric acid such that liquid covers atleast filled length of the
capillary.

Since the oil expands considerably when heated, be certain to keep the
rubber band (if used) and the open end of the capillary tube well above the oil
level. Also be sure that the bottom of the capillary is effectively sealed.

Cork used is split one to allow for expansion of air.

The tube is gently heated and rise in temperature is observed carefully. The
temperature at which the substance begins to liquefy is noted. The
temperature at which the solid has completely changed into liquid is also
noted.

The range of temperature is recorded as melting point range of the

substance.

Observation:

Temperature when the first drop of liquid become visible: …………………°C

Temperature when the solid has completely changed into liquid:

…………………°C

Results:

Report result as melting point and melting point range for given compound.

45
12. Determination of Viscosity of the
Given Liquid by Ostwald Viscometer

Aim: Determination of viscosity of the given liquid by Ostwald viscometer.

Principle:

Due to internal friction when a fluid passes through one another, it

experiences a resistance to its flow, which is known as viscosity. The co-
efficient of viscosity is a measure of this resistance and defined as the
tangential force per unit area required to maintain unit difference of viscosity
between two layers unit distance apart. Its unit in C.G.S. system is dyne/cm 2.

When a homogeneous fluid of volume ‘v’ flows through a capillary tube of

length ‘l’, radius ‘r’, in time ‘t’, under a driving force ‘p’, the co-efficient of
viscosity is given according to Poiseuille’s formula by

 Pr 4 t
η=
8lv

The experimental determination of viscosity is rather different. If η1 and η2

are the viscosity of two different fluids of density ρ1 and ρ2 respectively which
are successively allowed to fall through the same length ‘h’ of capillary e.g.
between the marks of an Ostwald Viscometer, the pressures are given by h
ρ1g and h ρ2g and thus η1 and η2 are given by

r 4 t1 (h1 g ) r 4 t 2 (h 2 g )
1 = and  2 =
8lv 8lv

1 t 1t1
= 1 1 , or, 1 =  2  
 2  2t 2  2t 2

Reagents:

1. Supplied sugar solution

46
Apparatus:

1. Viscometer (Ostwald)
2. Stop Watch
3. Burette
4. Burette stand with clamp
5. pipette
6. beaker
7. Weighing/ Specific gravity bottle

Procedure:

I. Weigh out 30gms of sucrose in a 250 cc. volumetric flask.

II. Add water to the mark and make the sol. exactly 12% by proper
quantitative dilution.
III. From it prepare 3%, 6%, 9% solutions by taking appropriate
quantity of 12% sol.
IV. Find the densities of the above sol.
V. Wash the viscometer and rinse repeatedly with distilled water by
sucking it in, releasing and throwing away the washings.
VI. Suck in fresh distilled water kept in a beaker, release and start the
stop watch as the meniscus touches the upper graduation and stop
it when the meniscus touches the lower graduation.
VII. Note the time.
VIII. Repeat the process thrice and take the mean of the three readings.
IX. Again repeat the process with 4 sugar sol. starting with the least
concentrated one.
t
We know, 1 =  2  1 1  Here, 1 = viscosity of
 2t 2
sugar , 2 = viscosity of water,
1 = density of sugar sol.,  2 =
density of water, t1= time flow of
sugar sol., t2 = time flow of water.

Observation:

Room temp.----------------------------

Density of water--------------------------

Viscosity of water----------------------------

47
Table- 1 Determination of time of flow:

Material Time of flow Average Viscosity (C.P.)

(sec.) Time(sec.)s

0% sugar
solution

3% sugar
solution

6% sugar
solution

9% sugar
solution

12% sugar
solution

Precautions:

1) The viscometer must be clean & rinsed.

2) Viscometer should be clamped in a vertical position & it’s height must
remain constant each time when it is clamped.
3) Exactly same volume of the two liquid should be used.
48
 4) The viscometer should not be disturbed during the measurement of
time of flow

Discussion:

1. The method used to determine the unknown percentage of sugar sol.

Is known as relative viscosity because the viscosity of the unknown
sugar sol. Is found out by comparing it with viscosity of water.
2. we get the unknown percentage composition of sugar sol. From the
plotted graph (% age composition of sugar sol vs viscosity).
3. Temperature affects the viscosity of the sugar sol because temp. is
inversely proportional to density and hence inversely related with
viscosity is directly proportional to density. The temp. is maintained
around 250 – 300C.
4. The viscosity also increases with increase in concentration.

Result: The unknown percentage composition of sugar sol. is-----------

49