Engineering Chemistry Lab Manual

Course Objectives:
The course consists of experiments related to the principles of Chemistry
required for engineering students. The student will learn

1. Estimation of Hardness and Chloride content in water to check its suitability for
drinking purpose.
2. To determine the rate constant of reactions from concentrations as a function of time.
3. The measurement of physical properties like adsorption and viscosity.
4. To synthesize the drug molecules and check the purity of Organic molecules by thin
layer Chromatographic (TLC) technique.

Course Outcomes:
The experiments will make the students gain skills on:

1. Determination of parameters like hardness and chloride content in water.

2. Estimation of rate constant of a reaction from concentration-time relationship.
3. Determination of physical properties like adsorption and viscosity.
4. Calculation of Rf values of Organic molecules by TLC technique.

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Chemistry Lab Do’s and Don’ts

The chemistry laboratory must be a safe place in which to work and learn about
chemistry. Most of these involve just using common sense.

1. Wear chemical splash goggles at all times while you are in the laboratory.
2. Wear a chemical-resistant apron.
3. Be familiar with your lab assignment before you come to lab. Follow all written and
verbal instructions carefully. Observe the safety alerts in the laboratory. If you do not
understand a direction or part of a procedure, ask the teacher before proceeding.
4. When entering the lab/classroom, do not touch any equipment, chemicals, or other
materials without being instructed to do so. Perform only those experiments
authorized by the instructor.
5. No student may work in the lab without an instructor present. Work only with your
lab partner(s). Do not venture to other lab stations for any reason.
6. Do not wear bulky or dangling clothing.
7. Never eat or drink in the laboratory.
8. Wash acid, base, or any chemical spill off of yourself immediately with large amounts
of water. Notify your teacher about the spill.
9. Clean up spills immediately. If you spill a very reactive substance such as an acid or
base, tell the people in the area and obtain assistance from your teacher. Acid spills
should be neutralized with baking soda, base spills with vinegar before cleaning them
up.
10. If chemical substances get in your eye, wash the eye out for 15 minutes with cold
water. Hold your eye open with your fingers while washing it.
11. If you take more of a chemical substance from a container than you need, you should
not return the excess to the container. This might cause contamination of the
substance remaining. Dispose of the excess as your teacher directs.
12. Never smell anything in the laboratory unless your teacher tells you it is safe. Do not
smell substance by putting your nose directly over the container and inhaling.
13. Do not directly touch any chemical with your hands. Never taste materials in the
laboratory.
14. If you burn yourself with a hot object, immediately put the burnt area under cold
water for 15 minutes. Inform your teacher.
15. Observe good housekeeping practices. Work areas should be kept clean and tidy at all
times. Only lab notebooks or lab handouts should be out on the table while
performing an Experiment. Books,bags should not be on the lab table. Passageways
need to be clear at all times.
16. Always replace lid of bottles and jars.
17. If your Bunsen burner goes out, turn off the gas immediately.
18. Always add acid to water and stir the solution while adding the acid. Never add water
to an acid.
19. Report all accidents to your teacher.
20. Absolutely no running, practical jokes, or horseplay is allowed in the Laboratory.
21. Thoroughly clean your laboratory work space at the end of the laboratory session,
Make sure that all equipment is clean, and returned to itsoriginalPlace.
22. Wash your hands before leaving the lab.

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Determination of total hardness of water by complexometric method using EDTA

Aim: - To Estimate the total hardness of water (i.e., calcium and magnesium ions) present in
the given sample of water by EDTA method.

Apparatus: -
 Conical flask (250ml) - 1
 Burette (50ml) - 1
 Measuring jar (20ml) - 1
 Beakers (250ml) - 2
 Pipette (20ml) – 1

Chemicals required: -
 Buffer solution (Ammonia-Ammonium chloride),
 Eriochrome black – T indicator (EBT – indicator),
 Standard EDTA solution (0.01M),
 Standard hard water 0.01M solution and
 Sample (tap) water.
Principle: - Hard water which contains calcium and magnesium ions form wine red coloured
unstable complex with EBT – indicator. This complex is titrated against EDTA solution, the
indicator is replaced by EDTA and a stable complex (colorless) is formed by releasing the
free indicator in the solution which is blue. In order to maintain pH 9-10 buffer solution is
added.

Equations

Ca2+ / Mg2+ + EBT (pH 9-10) [ ](wine red color Unstable complex)

[ ] + EDTA (pH 9-10) [ ] + EBT indicator blue color

(Colour less stable complex)

Structure OF EDTA Structure of disodium salt of EDTA

Structure of EBT Indicator:

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Procedure:

STEP I: Preparation of standard solution of CaCO3:-

Weigh 0.1gm of CaCO3 and transfer into 100 ml standard flask through funnel
add 2ml of concentrated HCl solution and add 40 to 50ml of distilled water. Shake the
flask well for uniform concentration. Make up the solution up to the mark with distilled
water and then calculate the molarity of CaCO3.

We know that
M.Wt. of CaCO3= 100gm
𝑤𝑡 𝑜𝑓 𝐶𝑎𝐶𝑂3 1000
Molarity (M) = × 100 (𝑚𝑙)
𝑀𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝐶𝑎𝐶𝑂3

0.1 1000
M= ×
100 100

Then M = 0.01M

Molarity of standard hard water (CaCO3 solution) = 0.01 M

STEP II: Standardization of EDTA solution

Pipette out 20 ml of standard solution of CaCO3 into a clean conical flask. Add
2 ml of buffer solution and 3 to 4 drops of EBT indicator, it gets wine red color solution.
Take EDTA solution in a burette and titrate with EDTA solution till wine red color
changes to blue color. Note the burette readings and repeat the titration to get concurrent
values.

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Tabular column:
Volume standard Burette reading
solution of CaCO3 in Volume of EDTA
S.NO Initial reading Final reading in
ml consumed in ml
in ml ml
1 20ml 0 ml

2 20ml

3 20ml

We know that M1V1=M2V2

M1= Molarity of CaCO3
M2=Molarity of EDTA
V1=Volume of CaCO3
V2=Volume of EDTA consumed

STEP-III:Estimation of Total hardness of water:

Pipette out 20 ml of tap water into a 250 ml clean conical flask add 2 ml of buffer solution and 3-
4 drops of EBT indicator, Titrate the wine red color solution with EDTA taken in burette,
till blue color end point is obtained. Repeat the titration to get concurrent values.

Tabular column:
Burette reading
S.NO Volume of Initial reading in Final reading in Volume of EDTA
sample water ml ml consumed in ml
taken in ml
1 20ml 0ml
2 20ml
3 20ml

Here M3V3 = M2V2

M3= Molarity of hard water
M2=Molarity of EDTA
V3=Volume of hard water
V2= Volume of EDTA consumed

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Totalhardness = M3×100×1000 = …………..ppm

RESULT:
1. Total hardness=………………ppm

Viva questions

1. What is the difference between hard water and soft water?

2. What are the salts responsible for the temporary and permanent hardness of water?

3. What is meant by softening of water?

4. What is ppm?
5. Why do we express hardness of water in terms of calcium carbonate equivalent?
6. What is degree of hardness of water?
7. Why PH 9 to 10 buffer solution is added during the determination of hardness of water?
8. Give the structures of EDTA and EBT.
9. What are the units for expression of hardness of water?
10. Give the relation between the hardness expression units.

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Determination of chloride content of water by argentometry

Aim: Estimation of chloride present in given water sample using AgNO 3.

Apparatus:

 Conical flask (250ml) - 1

 Burette (50ml) - 1
 Measuring jar (20ml) - 1
 Beakers (250ml) - 2
 Pipette (20ml) – 1
 Wash bottle.

Chemicals: Sample water, water sample, standard silver nitrate solution, Indicator potassium

chromate (K2CrO4) solution.

Principle:-

The amount of chloride in water can be simply determined by titrating the water sample with
silver nitrate solution by using potassium chromate indicator. The reaction is quantitative.
The AgNO3 reacts with chloride ion in a 1:1 ratio.

When silver nitrate solution is gradually added into the flask, then silver ions react
with chloride ions and forms silver chloride. It is precipitated in bottom of the flask. The
precipitation is white in color.

AgNO3(aq) + Cl–(aq) → AgCl(s) + NO3- (aq)

The end point of the titration takes place when all the chloride ions reacts and
precipitated. Then slightly extra silver ions react with the chromate ions and form a
brownish-red precipitate of silver chromate.

2AgNO3(aq) + K2CrO4(aq) → Ag2CrO4(s) + 2KNO3 (aq)

Preparation of standard solution of AgNO3 :-

Weigh 0.108 gm of AgNO3 and transfer into 100 ml standard flask through
funnel. Dissolve in minimum quantity of distilled water. Make up the solution up to the

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mark with distilled water and shake the flask well for uniform concentration then
calculate the molarity of AgNO3.
M.Wt. of AgNO3= 108gm
Molarity = Wt of AgNO3 *1000 / 108 * 100
0.108 1000
M= ×
108 100

Then molarity of AgNO3= 0.01 M

Procedure: Determination of chloride content of water

Take a 20 ml of water sample into a conical flask. Add 2-3 drops of potassium chromate

(K2CrO4) indicator to conical flask. The color of the water sample is turn into light yellow.

Take standard silver nitrate solution in to burette. Titrate the solution until the light yellow

color changes to permanent brownish-red color (brick-red color), precipitate with white color

precipitate.

Note the volume of silver nitrate added. Repeat the titration for concurrent values. Calculate
chloride ion concentration

Tabular column:
S. Volume of sample Burette reading Volume of
N0 water in ml Initial reading Final reading in AgNO3
in ml ml consumed in
ml
1 20 0 ml
2 20
3 20

Calculations:

M1V1=M2V2
M1= Molarity of AgNO3 M2=Molarity of Water sample
V1=Volume of AgNO3 Consumed. V2=Volume of Water sample

Molarity of (cl-) water sample M2 =V1 M1 /V2

Cl– present in the given water sample = M2 × 35.5 ×1000

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Cl– present in the given water sample = mg/liter

Result: -The amount of Chloride ion present in the given water sample is --------mg/lit

Viva questions
1. What is argentometry
2. What is the indicator used in this experiment
3. Give Cr oxidation number in K2CrO4
4. Why we get brick red color in the end point.
5. What is the indicator color?
6. Give the AgNO3 molar mass.
7.

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Estimation of an HCl by conductometric titrations.

Aim :- To determine the end point of strong acid against strong base by conductometric
titration.
Apparatus:-
 conductivity cell -1
 conductivity meter - 1
 beaker (100ml) - 1
 burette (50ml) -1
 glass rod - 1
Chemicals:-
 HCl (0.1M) solution – 40ml,
 NaOH solution (0.5M).

Principle:-Has the alkali is added from the burette into the cell containing acid, the
concentration of H+ ions change in the graphical manner which leads to a considerable
changes in the electrical conductance of the solution which is measured using a
conductivity meter. Then from the plot of conductance vs volume of alkali, the precise
neutralization point is determined.
Consider a titration of strong acid like HCl against NaOH i.e., strong base, the equation
will be
HCl + NaOH  NaCl + H2O.
When HCl is taken in a beaker as a titrate the initial conductivity is high, because strong
acid completely dissociates into H+ ions. The ionic conductivity of H+ ion is more. When
NaOH is added as a titrant the OH– ions of NaOH& H+ ions of HCl combine to produce
undissociated water and therefore the number of H+ ion decreases. There by the
conductivity gradually decreases after every addition of NaOH.
After the end point, H+ ions are neutralized by OH– ions & the addition of NaOH causes
the increase of number of OH– ions & hence the conductivity starts to increase again. Plot
a graph between conductivity vs volume of NaOH added give rise to two straight line
branches intersecting at the neutralization point like a ‘V’ shape.

Procedure:-

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Clean the burette and fill with standard NaOH solution.Take 40 ml of given HCl solution
in a 100 ml beaker and dip the conductivity cell in it and measure the conductance
initially. Now add NaOH solution from burette, drop wise i.e., 1 ml for each of the
addition, after each addition, stir the solution and note down the change in conductance
the measured conductance are recorded and tabulated in the table. Take the 20 readings.
Plot the graph between conductivity and volume of NaOH added. Where the
intersection of two straight lines gives the end point.Calculate the strength of given strong
acid using the NaOH solution

Tabular column:
S.NO Volume of NaOHin ml Observed conductance of HCl

Conductance
(ms)

Neutralization point

Volume of NaOH (ml)

Calculations and observations: - The end point of Titer value from graph is= -----ml.

The strength of acid is calculated by M 1V1 = M 2 V2

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M1= Molarity of NaOH = 0.5M M2 = Molarity of HClsoln =_____M

V1= Vol of NaOH consumed = ____ ml (graph)
V2 = Vol of HCl taken in beaker = ____ml

𝑀1𝑉1
M2 = 𝑉2

Result:- 1. The end point from the curve= -------------ml

2. The Molarity of HCl =--------M
3. The Strength of HCl = M× 36.5 =

Viva questions

1. What is specific conductance?

2. Mention the units of specific conductance?
3. What is the relationship between equivalent and molar conductance?
4. What is cell constant?
5. Explain the graph for the above experiment.
6. Give the units for conductance.
7. What is the difference between cell and electrode?
8. What are the products when acid reacts with base?
9. 1M HCl solution contains how many grams of HCl.

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Estimation of Acetic acid by conductometric titrations

Aim: To estimate the amount of Acetic acid present in the given solution by
conductometric titration.
Apparatus:-
 conductivity cell -1
 conductivity meter - 1
 beaker (100ml) - 1
 burette (50ml) -1
 glass rod – 1
Chemicals:-
 Acetic acid (0.1M) - 40ml
 NaOH solution (0.5M).

Principle:-
In this experiment, acetic acid is a weak acid. When it is titrated with a strong
base like NaOH, initially the conductance is low due to the feeble ionization of acetic
acid. On the addition of base, there is decrease in conductance not only due to the
replacement of H+ by Na+ but also suppresses the dissociation of acetic acid due to
common ion acetate. But very soon, the conductance increases on adding NaOH as NaOH
neutralizes the un-dissociated CH3COOH to CH3COONa which is the strong electrolyte.
This increase in conductance continues raise up to the equivalence point. The graph near
the equivalence point is curved due the hydrolysis of salt CH 3COONa. Beyond the
equivalence point, conductance increases more rapidly with the addition of NaOHdue to
the highly conducting OH− ions. You will get a titration curve which is shown below. The
point of intersection of the two lines gives the point of neutralization i.e. equivalence
point.
Procedure:-
Clean the burette and fill with standard NaOH solution. Take 40 ml of given CH 3COOH
solution in a 100 ml beaker and dip the conductivity cell in it and measure the
conductance initially. Now add NaOH solution from burette, drop wise i.e., 1 ml for each
of the addition, after each addition, stir the solution and note down the change in
conductance.The measured conductance are recorded and 20 readings are tabulated in the
table. Plot the graph between conductivity and volume of NaOH added. Where the

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intersection of two straight lines gives the end point.Calculate the strength of given
CH3COOH from unknown strength of NaOH solution

Tabular column:
S.NO Volume of NaOH in ml Observed conductance of CH3COOH
1 0
2 1
3 2
4 3

Graph:
Plot a graph by taking volume of NaOH on x-axis and conductance of the solution on
y-axis. Two straight lines intersecting at a point is obtained. The intersection point
corresponds to volume of NaOH required for the neutralization of weak acid.

Conductance
(ms)

Neutralization point

Volume of NaOH (ml)

M1= Molarity of NaOH = 0.5M M2 = Molarity of CH3COOH soln =_____M

V1= Vol of NaOH consumed = ____ ml (graph)
V2 = Vol of CH3COOH taken in beaker = ____ml
M1V1=M2V2

M2 = M1V1/V2

Result:- 1.The end point = -------------ml

2. The Molarity or Concentration of CH3COOH =-------M

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Estimation of HCl by Potentiometric titrations.

Aim:- To find the concentration of HCl by titrating it against standard NaOH solution
Potentiometrically.

Apparatus :-
 Potentiometer -1
 Pt electrode - 1
 Saturated calomel electrode-1
 100ml beaker - 1
 50ml Burette-1
 Glass rod

Chemicals: -
 Standard 0.5M NaOH solution,
 HCl solution – 40ml,
 Quinhydrone powder.

Principle:- A galvanic cell is a device which converts chemical energy to electrical

energy. It consists of 2 electrodes and the potential difference between 2 electrodes is
called emf of the cell. This can be measured by an instrument called potentiometer.
EMF of the given cell is given by
Ecell = Eoxi + Ered
The Nernst equation for the electrode potential of an electrode is given by
M Mn+ + ne–

=
[ Conc of [M] =1]
When E.M.F

= electrode potential of cell.

= standard electrode potential

n = Number of electrons involved in the reaction.
T= temperature in Kelvin

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R= gas constant.
F= Faraday current in coloumbs
In potentiometric titration an electrode whose potential depends on the
concentration of the ion being titrated is useful by measuring its potential by using
Quinhydrone electrode. The concentration of H+ ions is measured by Quinhydrone which
is an equimolar mixture of Quinone and hydroquinone.
Q + 2H+ +2e- QH2

Ecell= ESCE + log

Here n = 2, [QH2] = [Q] = 1 then

Ecell= ESCE + log [H+]

Here Q= Quinone, QH2= Hydroquinone.

This electrode is also called as Indicator electrode.
ESCE= 0.2422v.
Procedure:-
Take 40 ml of HCl solution in a 100 ml beaker. Add a pinch of Quinhydrone powder.Dip
the platinum electrode in the solution along with saturated calomel electrode. These are
connected to the potentiometer. Fill the burette with standard NaOH (0.5M) from the
burette into the beaker containing HCl and stir the reaction mixture. Note down the emf
values. Repeat the titration up to17-20 readings.

Tabular column:
S.No Volume of emf(Volts) ∆E ∆V ∆E/∆V
NaOH
1
2
3
4
5

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Graph

Plot a graph by taking cell EMF on y-axis and volume of NaOH on x- axis. A
curve showing inflexion at the equivalence point is obtained.The graph gives an inverted ‘S’
shaped curve.

Plot another graph by taking ΔE/ΔV on y-axis and volume of NaOH on x-

axisgives inverted ‘V’ shaped curve..

Neutralization point

EMF ∆E/∆V
(mv/mL)
Volume of NaOH (mL)

Volume of NaOH(mL)

Calculations and observations:-

The end point of titer value from graph is= -----ml.

The strength of acid is calculated M1V1 = M2V2

M1= Molarity of NaOH =0.5M M2 = Molarity of HClsoln =_____M

V1= Volume of NaOH consumed = __ ml(graph)
V2 = Volume of HCl taken in beaker = ____ml

M2 = M1V1/V2

Result:- End point of the reaction from the graph = --------ml

Molarity of HCl = ------M.
Strength of HCl = M×36.5

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Viva Questions

1. Define electrode potential?

2. What is emf?

3. Define a reference electrode?

4. Define reduction potential?

5. Why salt bridge is used in the construction of a cell?

6. Write the cell notation for the reference electrode (calomel)?

7. Write the cell notation of quinhydrone electrode?

8. Write the Nernst equation.

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Estimation of Ferrous ion (Fe2+) by Potentiometry using KMnO4

Aim: To estimate the amount of ferrous ion present in the given solution by
potentiometry
Apparatus:
 Potentiometer -1
 Platinum electrode-1
 Saturated calomel electrode-1
 100ml beaker-2
 50ml burette-1
 Glass rod-1
Chemicals:
 Standard KMnO4 solution
 Ferrous ion solution

Principle: The reduction potential of any redox system is given by

[Reduced sate]
E = E°+ RT/ nF log [Oxidised state]
Cell reaction:
MnO4- + 8H+ + 5e- Mn+2 + 4H2O
5Fe+2 5Fe+3 + 5e-
Therefore net reaction is
MnO4- + 5Fe+2 + 8H+ → Mn+2 + 5Fe+3 +4H2O
For a ferrous-ferric system, Fe2+ ⇋ Fe3+

Procedure:
The burette is filled with the given standard potassium permanganate solution.

Pippet out 40 ml of the ferrous ion solution into a clean 100 ml beaker. A platinum
electrode (indicator electrode) and a standard calomel electrode (reference electrode)
from the potentiometer are dipped in to the beaker.

The solution in the beaker is stirred using a stirrer and the initial EMF is noted. 0.5 ml
of potassium permanganate solution is added from the burette at regular intervals of time,
stirred well and the EMF is measured. Volume of the solution added and the
corresponding EMF readings are noted. At the end point, there is a sharp increase in EMF

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due to the complete oxidation of ferrous ion to ferric ion. Addition of potassium
permanganate solution is continued until the equivalent point is crossed by at least 5 ml.

Tabular column :
S.NO Volume of EMF(volts) ∆E ∆V ∆E/∆V
KMnO4
1
2
3
4
5
6

Using the equivalence point, concentration of ferrous solution is calculated using the equation

𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2

Graph:

From the observed values, ∆E = E 2 - E1, ∆V = V2 - V1 and ∆E/∆V is calculated and a graph is
drawn by plotting ∆E/∆V (y-axis) against volume of potassium dichromate added (x-axis). A
smooth curve is drawn by joining the points. The peak in the graph indicates the end point.
From the end point, the amount of the ferrous present in the given solution is calculated.

Equivalence point Equivalence

EMF ΔE/ΔV point

Volume of KMnO4 Volume of KMnO4

Calculations:

Volume of potassium permanganate (V1) =……….ml

Strength of potassium permanganate (M1) =……… M

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Volume of ferrous ion solution (V2) =………. ml

Strength of ferrous ion solution (M2) = ?
Number of moles of potassium permanganate (n1) = 1
Number of moles of Fe+2 (n2) = 5

Amount of ferrous ion present in the given solution = Strength of ferrous ion X
Equivalent weight of ferrous ion

Result:-Amount of ferrous ion present in the given solution = ……….. g / liter

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Determination of rate constant of acid catalysed hydrolysis of methyl acetate

Aim:- To Determine the rate constant of Hydrolysis of Methyl acetate

Apparatus:-:
 Conical flasks-1
 Burette (50ml)-1
 Pipette -5ml - 1
 Stopwatch-1
 water bath-1
 Ice
 Glass rod-1
Chemicals:
 Methyl acetate -5ml
 0.5 M of HCl
 Standard NaOH
 Phenolphthalein indicator

Principle:-
When esters such as methyl acetate react with water, it is converted to alcohol
and acid, and the reaction can be explained as;
H+
CH3COOCH3 + H2O CH3COOH + CH3OH
This is a reversible reaction, but with the presence of excess water, this reaction can be
considered as a complete reaction. Hydrolysis occurs slowly in pure water, acid acts as
catalyst.
If this reaction is conducted in a dilute solution with the presence of a known
concentration of strong acid, the rate and order of the reaction depends only on the
concentration of methyl acetate. This is thought to be due to the concentration of water
which is considered to be constant throughout the experiment and the concentration of
acid does not change. The rate of reaction, however, is proportional to the concentration
of acid.
The fact that this is a first order reaction is established by substituting the results in the
first order rate expression; K = 2.303/t log (a/a-x)
And verifying the constancy of the value of rate constant, K or in this case,
(a - x) = (V∞ - Vt) and a = (V∞ - Vo)

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𝟐.𝟑𝟎𝟑 𝑽∞ − 𝑽o
Then k1 = log
𝒕 𝑽∞ − 𝑽𝒕

Where,
Vo = initial titer value
V∞ = final titer value at the end of the experiment and
Vt = titer value at the various time intervals chosen as the hydrolysis proceeds, there will
be proportional increase in the concentration of acetic acid formed.
Procedure:-
Take 50 ml of 0.5 M HCl in a clean reagent bottle and place it in a water bath to attain
room temperature. Fill the burette with 0.5 M NaOH solution. Now add 5 ml of pure
methyl acetate to the reagent bottle containing HCl solution and shake the solution.
Immediately note the time and pipette out 5ml of the reaction mixture into a clean conical
flask containing 50 ml of ice cold water in order to quench the reaction. Now add two
drops of phenolphthalein indicator and titrate against 0.5M NaOH solution until a pale
pink colour just persists. Repeat the titration with 5 ml of the reaction mixture for every
10 minutes of time interval up to 50 minutes & tabulate the results.
.
Heat the remaining reaction mixture in a water bath at 60 oC for about 20 minutes.
Cool it to room temperature and pipette out 5 ml of the reaction mixture into a clean conical
flask containing 50 ml of distilled water and 2 drops of phenolphthalein indicator. Titrate this
against 0.5M NaOH solution and note the titer value as V∞.

Tabular column :

S Time in Volume of NaOH (V∞ - Vt) (V∞-V0) log

𝑉∞ − 𝑉o
𝑉∞ − 𝑉𝑡 𝟐.𝟑𝟎𝟑 𝑽∞ − 𝑽o
( V∞- Vt) k= log
No Minutes consumed (Vt) 𝒕 𝑽∞ − 𝑽𝒕

1 0
2 10
3 20
4 30
5 40
6 50
7 ∞

Graph:

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Plot a graph by taking log (V∞ - V0) / (V∞ - Vt) on Y-axis and time on X-axis.A
straight line passing through origin is obtained and its slope is equal to k/2.303.

𝑉∞ − 𝑉o
log 𝑉∞ − 𝑉𝑡
𝑑𝑦 𝐾1
Slope = 𝑑𝑥 = 2.303
Then K1 = slope (2.303) min-1

Time (min)

Result:

The average rate constant for the hydrolysis of methyl acetate using 1M HCl of
reaction is __________________ min-1.
The rate constant obtained from the plotis ________________ min -1.

Viva questions
1. What is pseudo first order reaction
2. Define order
3. Define molecularity
4. Why we were used phenolphthalein indicator in this experiment.
5. Give first order rate constant units.
6. Give the rate units.
7. Define the rate of the reaction.
8. What is the role of HCl in this experiment?
9. Why this is pseudo first order reaction.
10. Explain differences between molecularity and order.

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Synthesis of aspirin
Aim:- To prepare the aspirin from salicylic acid.
Apparatus:-
 Beaker(100ml) -1
 Conical flask (100ml) - 1
 wash bottle-1
 water bath
 glass rod-1
 Thermometer-1
 Measuring jar(10ml)-1
Chemicals:-
 Salicylic acid
 Acetic anhydride
 Ethanol,
 conc. H2SO4

Introduction:- The chemical name of Aspirin is acetyl Salicylic acid, Aspirin is extensively
used as antipyretic, analgesic and anti-inflammatory drug.
Principle:-Aspirin is an acetyl derivative of salicylic acid and prepared by Acetylation of
salicylic acid.
Acetylating with acetic anhydride in the presence of an acid.

Procedure :- Take 5 gm of salicylic acid in a 150ml conical flask and add 10 ml of acetic
anhydride. Shake the solution well and add 4 to 5 drops of conc. H 2SO4. The temperature of
the reaction mixture rises to 70-800C because of exothermic reaction. Maintain the

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temperature of the reaction at 70-800C for about 20 min by heating it on a water bath till the
solution is formed. Allow the solution to cool to room temperature and pour the solution into
100ml of ice water/cold water, into a 250ml beaker with stirring (addition of water is to
destroy excess of free reagent). Scratch the walls of the beaker with glass rod to induce
crystallisation and stir the solution till complete precipitation occurs. Filter the colourless
crystalline solid and wash it with cold water. Spread the solid aspirin on a filter paper and dry
it. Recrystallise the pure aspirin sample from a mixture of ethanol and water. Find the
melting point of sample.

Result: - Yield of compound is equal to ------------------ gm.

Viva questions

1. What is the chemical name of Aspirin?

2. Write the reaction involved in aspirin preparation?
3. What is the intermediate involved in the reaction?
4. Why the reaction is called O-acetylation?
5. What is the role of conc.H2SO4?
6. What are the medicinal uses of Aspirin?

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SYNTHESIS OF PARACETAMOL

Aim: - To prepare the organic compound paracetamol

Apparatus: - Beaker, conical flask, wash bottle, glass rod, thermometer & measuring jar.
Chemicals:
 4-aminophenol,
 Acetic anhydride,
 conc. H2SO4.

Principle:- Paracetamol is made by reacting 4-aminophenol with ethanoic anhydride

(more commonly called acetic anhydride). This reaction forms an amide bond and
ethanoic acid as a byproduct.
When the reaction is complete the paracetamol is then isolated and purified.
Paracetamol an analgesic and fever-reducing medicine similar in effect to aspirin.

4-aminophenol ethanoic
anhydride paracetamol ethanoic acid

Procedure: - Preparation of paracetamol

Weigh 2 g of 4-aminophenol and transfer in to a 100 ml thoroughly cleaned and dried
conical flask. Add to the flask 3 ml of acetic anhydride and 18ml of water. The contents of
the flask may be mixed thoroughly. Warm the mixture on a water bath previously
maintained at 120°C for about 20–25 minutes with constant stirring. After that cool it in
ice water where the sample mass get solidifies, filter it and take the weight of sample.

Result:- Yield of compound is equal to ------------------ gm.

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Thin layer Chromatography calculation of rf values of ortho and para nitro phenol

Aim: To determine the thin layer chromatography calculation of R f values of ortho and para
nitro phenol.
Apparatus:
 TLC plates,
 TLC chamber,
 Mobile phase,
 Filter paper.

Chemicals:
 o-nitrophenol
 p-nitrophenol
 Tolune

Procedure: Draw a pencil line 1 cm above the bottom of TLC plate and mark spots for each
p-nitrophenol and o-nitrophenol, equally spaced along line.
Use a capillary tube and add a tiny drop of each solution to a different spot and allow
the plate to dry.
Add the solvent tolune to a chamber or a large beaker with a tight lid so that the
solvent is not more than 1 cm depth.
Place the TLC plate in the chamber. Make sure that the level of solvent is below the pencil
line. Keep the lid when the solvent level reaches about 1 cm from the top of the plate, remove
the plate and mark the solvent level with pencil. Allow the plate to dry in a fume cupboard.
Place the plate under a u.v. lamp in order to see the spots.

Results

(Retardation factor) Rf = distance travelled by the compound/ distance travelled by the

solvent

Rf value of o-nitrophenol =

Rf value of p-nitrophenol =

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Determination of acid value of coconut oil

Aim: To estimate the acid value of given oil.

Apparatus: -
 Conical flask
 Burette
 Measuring jar
 Beakers
 Pipette
Chemicals required: -
 Ethanol,
 Diethyl ether,
 Coconut oil,
 0.1M KOH solution
 Phenolphthalein indicator

PRINCIPLE:
The given oil is treated against a strong base such as KOH. The fatty acids in the oil
react with base to form salts of fatty acids. From the volume of KOH consumed, acid value of
oils can be estimated. In this estimation phenolphthalein is used as indicator.

Procedure
Estimation of acid value:
About 10 g of oil is weighed & transferred into a conical flask.To this 50ml of solvent
mixture of ethanol and diethylether mixture is added & shaken well to dissolve the oil.To this
9-10 drops of phenolphthalein indicator is added & the solution is titrated against KOH
solution till the color changes to pink. The experiment is repeated to get two concurrent
readings.

Tabular column :

S.No Weight of oil (mg) Initial burette Final burette KOH

reading reading consumed(ml)

Estimation of acid value:

eq.wt of KOH × vol.of KOH (Burette reading) × Normality of KOH

Acid value of KOH = weight of oil

56 × vol.of KOH (Burette reading) × 0.1

Acid value of KOH = weight of oil

RESULT: The acid value of coconut oil is --------

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Verification of freundlich adsorption isotherm- adsorption of acetic acid on charcoal

Aim:To Study the adsorption of acetic acid from solution on activated charcoal
Apparatus:
 Reagent bottles (150 ml) -5
 Burette (50ml) -1
 Funnel
 wattmann paper no. 41
 pipette(10ml)-1
 Conical flask (250ml) -1

Chemicals:

 0.1N acetic acid solution

 0.1N NaOH solution,
 charcoal - 1gm
 phenolphthalein indicator

Principle:

Freundlich proposed a relation between the amount of solute adsorbed on a definite amount
adsorbent and the equilibrium concentration of the adsorbate in the solution. According to
which
x/m = kCe1/n
where x = amount of solute adsorbed
m= mass of the adsorbent
Ce= equilibrium concentration of adsorbate
k = constant.
n = no. of layers of acetic acid adsorbed to the surface layer of charcoal.
In general, 1/n is less than 1 and taking logarithm for the above equation, we get
log(x/m) = log k + 1/n log Ce

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Procedure:
Take 5 clean reagent bottles and number them from 1-5 and prepare the following
solution mixtures.

Bottle Volume of acetic Water

No. acid solution
1 50ml -
2 40ml 10ml
3 30ml 20ml
4 20ml 30ml
5 10ml 40ml

Now stopper each bottle after adding 1gm of charcoal and shake the bottles in a
rotatory motion and allow them to stand for at least 1 hour. In the mean time, fill the burette
with 0.1N NaOH solution. Pipette out 10ml of stock 0.1M acetic acid solution into a clean
conical flask and add 1 or 2 drops of phenolphthalein indicator and titrate it against sodium
hydroxide solution. The end point is noted when a faint pink colour is observed. After 1 hour
filter the contents of each bottle separately through a Wattmann filter paper no. 41. While
filtering, reject the first 5ml of the filtrate and collect the rest. Wait until the filtration is
complete and pipette out 10ml of the filtrate into a clean conical flask and titrate it against
with 0.1N NaOH by adding 1-2 drops of phenolphthalein indicator. The end point is noted
when a faint pink colour is observed.
Repeat the procedure with the filtrate of other bottles and tabulate the results.
Graph:

Plot a graph by taking log(x/m) on y-axis and log(Ce) on x-axis. A straight line cutting
y-axis is obtained. The slope of the straight line is equal to 1/n and the intercept is equal to
log(k).

log(x/m) Slope=1/n

log (k)

log(Ce)

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Tabular column :

Initial Vol of 𝑪𝒊 − 𝑪𝒆 𝒙 log𝒎

𝒙
log(Ce)
x=
Bottle concentration N/10 𝟏𝟎 𝒎
No. of acetic acid NaOH
(Ci) (Ce)
1
2
3
4
5

Result:
The Freundlich adsorption isotherm is verified for the adsorption of acetic acid on
charcoal. The value of n obtained from the graph of log(x/m) vs log (Ce) is
___________________

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Determination of viscosity of castor oil and groundnut oil by using Ostwald’s

Viscometer.
Aim: - To determine the viscosity of given liquid using Ostwald’s viscometer.
Apparatus: -
 Ostwald’s viscometer-1
 Stopwatch-1
 Beaker(100ml) -2
Chemicals: -
 Water,
 Test liquids (n-butanol,Castor oil, Groundnut oil)
Principle: - Viscosity is one of the properties of liquid and depends on temperature. It is
the resistance of the liquid to flow. Higher the viscosity, greater will be the resistance to
its flow. It opposes the relative motion of adjacent portion of two liquids and is regarded
as a kind of internal friction when a liquid is flowing through a narrow tube.
Which is measured in millipoise (mp) and the formula is
𝜂𝑎 𝑑
= 𝑑 𝑎 𝑡𝑎
𝜂𝑤 𝑤 𝑡𝑤

Where ηa = viscosity of test liquid

ηw = viscosity of water
da = density of test liquid.
ta= time taken for test liquid
dw= density of water (g/ml)
tw = time taken for water .

Procedure: - The Ostawald’s viscometer consists of a fine capillary tube with a bulb A at
its upper end, U-tube and a bulb B at the lower end. There are two marks x and y on the
tube above and below the bulb A. Clean the viscometer thoroughly with distilled water.
Set the viscometer vertically and introduce a measured volume of given organic liquid
into a large bulb B. Now suck the liquid up into the bulb A through a rubber tube attached
to the cup to a level higher than mark x. Now allow the liquid to flow freely through the
capillary. Start the stop-clock when the liquid reaches mark x and the time when it

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reaches mark y. Repeat the same procedure by taking exactly the same volume of distilled
water.
Tabular form:
S. No. Liquid Time in seconds Average Coefficient Literature
(t1+t2)/2 of viscosity Value
t1 t2 (η) (mPa.S)
1 Water 0.890
2 n-butanol 2.573
3 Stannol 1.074

Result:-
The viscosity of given liquid is found to be -----------------------millipoise

Viva questions
1. What are the dimensions of Viscosity?
2. What is the effect of temperature on Viscosity?
3. What are the Applications of Viscosity Measurement?
4. Discuss the factors on which Viscosity depends?
5. Define the Viscosity.

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Determination of partition coefficient of acetic acid between n-Butanol and water

Aim:- To determine the partition coefficient of Acetic acid between n-butanol and water
Chemicals:
 n-butanol,
 acetic acid,
 distilled water,
 NaOH Solution.

Apparatus:
 Burette,
 pipette,
 100 ml conical flask,
 250 ml Stoppered bottle,
 Wash bottle,
 Dropper

Principle: Nernst distribution law states that at constant temperature, when a solute is
allowed to distribute between two immiscible solvents in contact with each other, then at
equilibrium the ratio of the concentration of the solute in two solvent layers is constant. When
a solute is shaken in two immiscible liquids, then the solute is found to be distributed
between the liquids in a definite manner, if the solute is soluble in each of the
solvent.According to distribution law, the distribution co-efficient at a particular temperature
is given by
Kd = C1 / C2, where
C1 and C2 represent the concentrations of solute in solvent 1 and 2 respectively. When the
solute molecules in each solution phase are in same state of association.
(Or)
𝐶𝑜𝑟𝑔
KD = 𝐶
𝑎𝑞
Where KD = partition or distribution coefficient
Corg = Concentration of solute in organic (upper) layer
Caq =Concentration of solute in the aqueous (lower) layer.

Procedure:
Take a clean reagent bottle and take 20 ml of n-butanol, 25 ml distilled water and 5 ml of
acetic acid. Now cork the bottle and shake it well without spilling of the solution for about 10
minutes. Now open the cork and keep the bottle aside for 5 minutes without distributing so
that the two layers separate out. Fill the burette with 0.1M NaOH and clamp it to the stand.

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Now pipette out 5mL of the upper layer (org) layer into a clean conical flask and
add 2 to 3 drops of Phenolphthalein indicator and titrate against 0.1 M NaOH until the
solution turns to pale pink color. The solution must be shacked vigorously during the
titration, and note the titer value as VOrg. Now pipette out 5mLl of lower layer with
another pipette into a clean conical flask and add 2 to 3 drops of phenolphthalein and
titrate against 0.1 M NaOH. Note the end point as Vaq.

Now add 5mL of n-butanol and 5mL of distilled water to the reagent bottle and
shake it for about 5 min and allow it to settle. Repeat the above titration for both the
layers and note down another set of readings. Repeat the above procedure for three more
sets of readings. Calculate the distribution coefficient for each set of readings.

Tabular column :

S. Volume of NaOH Volume of NaOH for aqueous Corg Caq 𝐶𝑜𝑟𝑔

KD =
No for organic layer layer 𝐶𝑎𝑞

Graph:

Plot a graph by taking Caq on x-axis and COrg on Y-axis. A straight line passes through the
origin. Find the slope of the straight line which is equal to the KD.

Y Axis

Slope= KD
COrg

X Axis
Caq

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Result:

The average experimental distribution coefficient of the distribution of acetic acid between n-
butanol and water is ____________________________

The Distribution Coefficient obtained from the plot of COrg vs Caq is __________

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Determination of Surface tension of a given Liquid using Stalagmometer

Aim:-To determine the surface tension of the given liquids using Stalagmometer.
Apparatus:-
 Stalagmometer,
 small rubber tube,
 Beaker.
Chemicals:
 Distilled water,
 Test solution i.e., soap solution, aniline, acetophenone, n-butanol.

Principle:-All the molecules in a liquid are held together by force of attraction and this
causes the surface of the liquid to behave like a stretched skin. Surface tension is the result of
the force of attraction between the molecules present on the surface.
It is defined as the force of acting per unit length of the surface of the liquid.
The formation of drops depends on the surface tension of the liquid and all liquids will not
give same number of drops from same volume of liquid.
The surface tension of a given liquid can be evaluated by using the equation

2 = n1× d2
1 n2 × d1

Where 2 = is the surface tension of the given liquid.

1 = is the surface tension of water.
n1 = is the no. of drops for water.
n2 = is the no. drops for the given liquid.
d1 = is the density of water.
d2 = is the density of the given liquid.
Procedure:-
Description of stalagmometer:
It consists of a fine capillary tube with a bulb at the center. The upper end of the tube
is fitted with a rubber tube which is used to suck the liquid. The lower end of the tube
consists of a fine capillary bore. The upper and lower ends of the bulb contain two marks say
A and B.
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Clean the stalagmometer thoroughly with distilled water followed by chromic acid
and again with distilled water. Now suck the distilled water through the upper end slight
above the mark A and tighten the rubber tube with a pinch cock. Clamp the stalagmometer
and release the pinch cock. Count the number of drops till the liquid reaches the lower mark
B. Repeat the procedure and measures the no. of drops and the mean of the readings is taken
into account.
Now discard water and dry the tube by using dry air current or in the oven. Repeat the
procedure with the other given liquids and tabulate the results. Knowing the density values of
the respective liquids calculate the surface tension using the above given formula.

Tabular column :

Sl. Liquid No. of drops of liquid Average Surface Literature

No. (n1+n2)/2 tension () Value
n1 n2 (dynes/cm)
1 Water 71.99
2 n-butanol 24.6

Note:
Density of water = 1.00 gr/cm3
Density of butanol = 0.81gr/cm3

Result:-a) Surface tension of n-butanol is _______________ dynes/cm

b) The surface tension of given test liquid is -----------------------------dynes/cm

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Viva questions

1. Define surface tension.

2. Give the equation for the determination of surface tension.

3. Which method is involved in stalagmometer?

4. What is the value of surface tension of water?

5. Give the units for surface tension expression.

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