Department of Electrical Engineering

B. P. Poddar Institute of Management & Technology

Laboratory Report on
Chemistry 1 (BS-CH191)

Name of Student : ……………………………………………………..

Roll Number : ……………………………………………………..

Year : ……………… Semester ……………………….

Section : …………………Group .…………………………

Session : …………………………………………………….
 GENERAL INFORMATION

Chemistry-I Laboratory Semester Odd

Course Name
1st year, EE
Course Code BS-CH-191 Stream

Session 2019-2020 Section & Group

Faculty
Class Hours
Instructor/s

Technical Laboratory Chemistry Lab

Assistant/s Block-A-102 & 103

Analyse components from mixtures by separation and adsorption methods as well as

measure the viscosity of fluids.

COURSE Estimate some parameters that affect water quality by volumetric and electrochemical
OBJECTIVES titrations/experiments.

Gain practical knowledge to determine the rate constant of pseudo-unimolecular reaction

and partition coefficient.

COs COURSE OUTCOMES Cognitive Level

Analysis of acids by using adsorption on charcoal and thin layer

CO1 chromatographic methods Analyze

CO2 Determination of concentration of acids/alkali, redox potential and cell-

emf by using electrochemical cells Analyze

CO3 Determination of partition co-efficient of an acid in a mixture of two

immiscible phases. Analyze
Estimation of dissolved oxygen and chloride ion present in test water
CO4
sample Apply
Determination of the composition of the given solution using Ostwald’s
CO5
viscometer Apply

CO6 Determination of rate constant of ester hydrolysis Apply

I
 CO-PO-PSO MAPPING

COs PO PO2 PO3 PO4 PO5 PO6 PO7 PO8 PO9 PO10 PO11 PO12 PSO1 PSO2
1
CO1 1 2 - - - - 2 2 2 - - - -

CO2 1 2 - - - - 2 2 2 - 1 - 1

CO3 1 2 - - - - - 2 2 2 - - -

CO4 1 2 - - - - 2 2 2 2 - - - 1

CO5 1 2 - - - - - 2 2 2 - - - -

CO6 1 2 - - - - - 2 2 2 - - - -

- - 1
BS 1 2 - - 2 2 2 2 - 1 -
CH191

GENERAL SAFETY

 All the work areas and the surrounding environment should be kept clean andtidy

 A lab coat/Apron at all times should be worn while performing laboratoryexperiments.

 Do not ever try to smell or taste thechemicals.

 Removal of chemicals or other materials from the laboratory area is strictlyprohibited.

 Don’t casually dispose of chemicals anywhere in thelab.

 Broken glass should always be disposed in the specific glass disposalcontainer.

 Perform only those experiments that are asked by theinstructor.

 Do not perform any unauthorizedexperiments.

HANDLING ACCIDENTS AND INJURIES

 In case of any accident report it in the concerned authority immediately. Whether it is a spill,
breakage or injury in the form of cut, burn, etc. Do not spreadpanic.

 In case of chemical splash in eye(s) or skin, rush to the water tap and flush with running water
for a minimum of 20 minutes. Call the teacher or staff and seek medicalattention.

II
 COURSE POLICIES

1. Attendance

Attendance is compulsory. Please be respectful to your classmates by being on time. Cell phones should
be turned off and kept in thebag

2. Calculatorpolicy

You may need a pencil, eraser, calculator, 12 inch scale, cm graph sheet.

3. Plagiarism

Collaboration on performing the experiments and taking measurements is strongly encouraged; however,
the lab report you hand in must be solely your own. Sharing written work beforehand is considered as
academic dishonesty.

4. DisabilitySupport

If you have a disabling condition which may interfere with your ability to successfully complete this module,
please contact Faculty incharge.

5. Make-upExperiment

Make-up for a missing experiment will not be offered, normally. The only exceptions to that are illness or
emergency (e.g., death in family, a traffic accident, etc.), in which case you may contact your faculty in
charge.

6. Experiment in virtuallaboratory

As per policy you have to perform at least one virtual experiment.

7. Experiments beyond curriculum &Microproject

As per policy you have to perform at least one from each of the experiments mentioned above

Recommended books:

1. Engineering Chemistry (Theory and Practicals), N. Acharjee &P. Dhar; U.N. Dhur & Sons Pvt. Ltd.,Kolkata

2. Experiments in Applied Chemistry, Dr. Sunita Rattan; S. K. Kataria & Sons, NewDelhi

3. Laboratory Manual on Engineering Chemistry, S.K. Bhasin & Sudha Rani; Dhanpat Rai Publishing
Company, NewDelhi.

III
 COURSE ASSESSMENT PROCESS

Internal Assessment (40 Marks): To be marked out of 100 and then scaled down to40

1. CONTINUOUS ASSESSMENT: [80%]

Lab report [15marks]

Assignment number, Objective, theory, methodology/algorithm/data structure, results/output, discussion
and conclusion

Lab Performance & Attendance [50 marks]

Assessment based on methodology/algorithm/data structure and how to implement these to solve the
problems of the experiment / micro project provided in the lab.

Viva Voce [15 marks]

Viva-voce on each Lab experiment during every laboratory class will be conducted.

2. LABORATORY INTERNAL EXAMINATION: [20%]

Assessment During End Semester Examination: (60 marks)

Answer Script [20 marks]

Experiments are allotted to a student randomly on lottery basis. Answer scripts will be evaluated based on
the problem assigned to the student and his/her level of understanding, analyzing and designing a solution.

Performance [20 marks]

Overall performance skills and discipline of the student during Laboratory examination which they have to
complete in stipulated time will be evaluated.

Viva Voce [20 marks]

There is a viva-voce during examination.

Grading Scale

Grade Percent Score

O 90-100%

E 80-89%

A 70-79%

B 60-69%

C 50-59%

D 40-49%

F <40%

IV
 List of Experiments

Expt. Page Date of

Name of Experiment COs Signature Grade
No. No. Expt.

Determination of Dissolved Oxygen

1 CO4
Present in a Given Water Sample

Conductometric titration for

2 determination of the strength of a CO2
given HCL solution

Determination of Partition Co-efficient

3 of Acetic Acid between Water and CO3
n-Butanol

Adsorption of Acetic Acid on Activated

4 CO1
Charcoal

Determination of percentage
5 composition of sugar solution by CO5
OSWALD’S Viscometer

pH-metric titration for determination of

6 CO2
strength of a given HCl solution

To determine Chloride ion in a given

7 watersampleby Argentometric CO4
method

Determination of rate constant for the

8 hydrolysis of ethyl acetate catalyzed CO6
by HCl

Analysis of components of given

9 CO1
mixture by thin layer chromatography

10 Determination of Redox Potentials and CO2

cell emf by potentiometric method.

Additional Experiment
11

V
 ExperimentNumber…1 Date………………....

Objective: Determination of Dissolved Oxygen Present in a Given WaterSample

Theory

Determination of Dissolved Oxygen (D.O) is important for industrial purposes. D.O is needed for living
organism to maintain their biological processes. It is important in precipitation and dissolution of inorganic
substances in water. It is also an important factor in corrosion. D.O tests are used to control the amount of
oxygen in boiler feed water by mechanical, physical and chemical methods. This test helps to assess raw
water quality and to keep a check on stream pollution.
The principle involved is based on the oxidation of potassium iodide by dissolved oxygen present in
water. The liberated iodine is titrated against a standard sodium thiosulphate solution using starch as final
indicator. However, dissolved molecular oxygen in water is not capable of reacting with KI, so an oxygen-
carrier (such as manganese hydroxide) is used to bring about the reaction between KI and oxygen.
Manganese hydroxide is produced by the following reaction:

2NaOH + MnSO4 → Mn(OH)2 +Na2SO4

2Mn(OH)2+ O2 →2MnO(OH)2
(oxygencarrier) (Basic manganicoxide)

MnO(OH)2 + H2SO4 → MnSO4 + 2H2O + [O]

(Nascent oxygen)
2KI+ H2SO4+[O] → K2SO4 + H2O +I2

2Na2S2O3 + I2 → 2NaI +Na2S4O6

Starch + I2 → Starch-iodine complex (bluecoloured)

Sometimes, water contains substances like nitrites, sulphites, etc. and determination of dissolved
oxygen in their presence will give wrong results, since these ions also liberate iodine from KI. So, azide
(usually sodium azide) is used in alkaline iodide solution to take care of any nitrite, if present in water, does
not liberate iodine from KI. Sodium azide reacts with nitrite to decompose it asfollows:

2NaN3 + H2SO4 → 2HN3 + Na2SO4

HNO3+HN3 → N2O↑ + N2 +H2O

Procedure

(i) Standardization of Sodium Thiosulphatesolution:

25 ml of standard K2Cr2O7 was pipetted out into a conical flask. To this 10 ml of 1:1 H2SO4 and 10 ml
of 5% Potassium Iodide solutions were added. This solution was titrated against sodiumthiosulphate
1
 solution taken in a burette. When the solution becomes straw yellow colour, starch indicator was added and
then titration was continued. The end point was the colour change from blue to light green colour. The
titration was repeated to get concordant value.

(ii) Estimation of Dissolved Oxygen in Test Watersample:

250 ml of the supplied test water sample was taken in a stoppered bottle. To this 2 ml of alkaline
iodide (NaOH & KI) solution and 2 ml of manganous sulphate solution are added by dipping the end of the
pipette well-below the water surface and stoppered. The stoppered bottle was shaken thoroughly. The
formed precipitate was allowed to settle half-way and was mixed again. The process of shaking and settling
was repeated for at least three times. Then a 10 ml of conc.H2SO4 solution were added to get a clear yellow
solution due to iodine liberation. 100 ml of this solution was measured in a measuring cylinder (calibrated)
and transferred to a conical flask. This solution was titrated against sodium thiosulphate taken in the
burette. When the solution became straw yellow colour, starch indicator was added and continued the
titration till disappearance of blue colour. Titre value wasnoted.

Observation

(i) Table 1: Standardization of Sodium Thiosulphatesolution

Volume of Volume of Mean Volume of

Burette Reading (ml)
No. Standard Sodium Sodium
of K2Cr2O7 solution thiosulphate thiosulphate
Initial Final
Titration (ml) Solution(ml) Solution(ml)

V1

(ii) Table 2: Estimation of Dissolved Oxygen in Test Watersample

Volume of Mean Volume of

Volume of Burette Reading (ml)
No. Sodium Sodium
Test Water
of thiosulphate thiosulphate
Sample (ml) Initial Final
Titration Solution(ml) Solution(ml)

V2

2
 Calculation

(i) Standardization of Sodium Thiosulphatesolution:

(ii) Estimation of Dissolved Oxygen in Test Watersample:

Conclusion

The amount of D.O. present in the supplied Test Water sample =

3
Questions:

Teacher’s
signature……………….…………………..

4
ExperimentNumber…2 Date…………………

Objective: Conductometric Titration for Determination of Strength ofthe

Given HCl Solution

Theory

The principle of conductometric titration is based on the fact that the conductance of the solution depends on
following factors.

a. Mobility or ion conductance, no. ofions

b. Dilution. (It is avoided by taking titrant 10 times than the titratingagent)

During the titration i) When one ion is replaced by the other, due to difference in ion, conductivity of the
solution varies and ii) as the number of ions changes in solution during titration, the conductance also
changes. These changes are linear in nature. Hence two lines are obtained before and after the equivalence
point in a graphical plot of conductance C vs. Volume of titrant added. Intersection of these two straight lines
gives the end point from which the unknown strength can be calculated.

When Hydrochloric acid is titrated with Sodium Hydroxide the highly mobile hydrogen ions [λ0(H+) ≈ 350 ohm-
1
cm-1] are progressively replaced by slower moving Sodium ions [λ0(Na+) ≈ 50 ohm-1 cm-1] and so
conductance value decreases. After the neutralization point the conductance value rises sharply due to
excess of hydroxide ions [λ0(OH-) ≈ 198 ohm-1 cm-1].

The strength of the unknown acid can be calculated from the equation,

V1 x S1 = V2 x S2

Procedure

(i) At first, the electrodes are calibrated using distilled water and 0.1(N) KClsolution.

(ii) Standardization of the NaOHsolution

At first NaOH solution is taken in a burette. Now 25 ml of the standard oxalic acid solution (0.1N) is
pipetted out in a conical flask, 25 ml distilled water and 1-2 drops of Phenolphthalein indicator is added to it.
Then the solution is titrated with the NaOH solution until a light pink colour appeared. The titration is
repeated to get concordantvalues.

(iii) Measurement of ConductanceValues

1. 25 ml HCl solution is pipetted out in a 100 ml beaker and 25 ml distilled water is added to it. The electrode
is dipped into the solution and the conductivity reading (mho) is notedfirst.

5
2. Then NaOH solution is added gradually 2 ml at a time from the burette, mixed well and conductance value
is noted down after everyaddition.

3. After getting a minimum conductance the above process is continued till at least four increasing values of
conductance weretaken.

4. A graph is plotted taking ‘conductance’ in Y axis and ‘volume of NaOH’ in X axis. The point of intersection
of two lines gives the neutralizationpoint.

Observation

Temperature of thesolution= C

Table 1: Standardization of NaOH solution

Volume of Burette Reading (ml)

No. Volume of NaOH Mean Volume
Standard Oxalic
of Solution of NaOH
Acid solution Initial Final
Titration (ml) Solution (ml)
(ml)

Calculation

(i) Standardization of NaOHsolution:

6
Table 2: Measurement of conductivity of unknown HCl solution

Volume of NaOH Solution Conductivity

SI. No.
(ml) (m mho)

7
Paste Graph

8
Calculation

(ii) Determination of strength of unknown HClsolution:

Conclusion The strength of unknown HCl solution=

Questions:

Teacher’s
signature……………….…………………..

9
ExperimentNumber…3 Date…………………

Objective: Determination of Partition Co-efficient of Acetic Acidbetween

Water and n-Butanol

Theory
The Nernst distribution law states that at constant temperature when different quantities of a solute are
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 solution which is soluble in each of two immiscible liquids is shaken with a mixture of two such
solvents, it will distribute itself in the two solvents in such a way that at equilibrium, the ratio of the
concentration of the solute in the two liquids is constant at that temperature provided there is neither
association nor dissociation of the solute in solvents.

Consider a liquid-liquid system, say water and n-butanol (two immiscible solvents), to which little quantity of
acetic acid added. Acetic acid will dissolve partly in water and partly in n-butanol . According to distribution law,
the distribution co-efficient at a particular temperature is given by K=C1/C2 where C1 and C2 represents the
concentration of solute in solvent 1 and 2 respectively. The constant K is known as Distribution or Partition
Coefficient.

Thus the distribution coefficient of Acetic Acid in water and n-Butanol be K= Cw/Cb, where Cw =
Concentration of Acetic Acid in water and Cb= Concentration of Acetic Acid in n-butanol.

Procedure

The following mixtures were prepared in 250 ml leak proof, stoppered glass bottle:

Volume of solution of Volume of

Bottle Volume of Total Volume
Acetic Acidin Pure
No. water (ml) (ml)
n-Butanol(ml) n-Butanol (ml)
1 20 30 50 100

2 30 20 50 100

3 40 10 50 100

The bottles were shaken well for about 30 minutes in a shaker and then allowed to stand undisturbed for
about 10 minutes so that the two layers were separated distinctly.

5 ml of organic layer was pipette out from first bottle in a 100 ml conical flask. 20 ml of distilled water
and 1 drop of phenolphthalein indicator were added to it. The mixture was shaken vigorously for a
10
few second and then it was titrated with (N)/10 NaOH solution taken in a burette until pink end point
was reached. The titration was repeated. Same procedure was done with other two bottles.

5 ml of aqeous layer was pipette out from first bottle in a 100 ml conical flask. 20 ml of distilled water and 1
drop of phenolphthalein indicator were added to it. The mixture was shaken vigorously for a few second and
then it was titrated with (N)/10 NaOH solution taken in a burette until pink end point was reached. The
process was repeated. Same procedure was done with other two bottles.
The room temperature was noted down.

Observation

Table 1: Titration of organic layer

Volume (Vb) Mean volume (V1)

Bottle No. of Volume of N/10 NaOH
of aliquot from of NaOH solution Cb
No. Titration solution (ml)
organic layer (ml) (M)
(ml)
Initial Final
1

1. 2

2. 2

1
3.
2

Table 2: Titration of aqueous layer

Volume (Vw) of Volume of N/10

Bottle No. of aliquot from NaOH solution Mean volume (V2) of Cw
No. Titration aqueous layer (ml) NaOH solution (ml) (M)
(ml)
Initial Final
1

1. 2

11
 3

2. 2

1
3.
2

Calculation

(i) Titration of organiclayer

Vb × Cb = V1 × SNaOH

V  SNaOH
Cb  1
Vb

(ii) Titration of aqueouslayer

Vw × Cw = V2 ×SNaOH

V SNaOH
C w  2
Vw

12
 Final Calculation of K

Cw Mean Cw = K
No. of Bottles Cb (N) Cw (N) Cb
Cb

Conclusion
The distribution co-efficient of acetic acid between water and n-Butanol =

Questions:

Teacher’s
signature……………….…………………..

13
 ExperimentNumber…4 Date…………………

Objective: Adsorption of Acetic Acid on ActivatedCharcoal

Theory

Surface of any solid or liquid is in a state of strain due to unsaturated force. To lower this strain they try to
adsorb foreign particles on the surface. Extent of adsorption depends on (a) nature of adsorbent and
adsorbate, (b) nature of surface, (c) temperature and (d) concentration of adsorbate. For a given pair of
adsorbent and adsorbate and at a given temperature relation between extent of adsorption and
x
concentration is called adsorption isotherm. Freundlich's empirical equation is KC n 1
m
Here 'x' is the amount of adsorbate adsorbed by `m g of adsorbent; 'C' is the concentration of adsorbate
and 'K' and 'n' are constants with .Taking logarithm of both sides-
x 1
log  log K  log C
m n
Hence, plot of log x/m against log C will be a straight line.

Procedure

A) Standardization of the NaOHsolution

At first NaOH solution is taken in a burette. Now 25 ml of the standard Oxalic Acid solution (0.1N) is
pipetted out in a conical flask, 25 ml distilled water and 1-2 drops of Phenolphthalein indicator is added to it.
Then the solution is titrated with the NaOH solution until a light pink colour appeared. The titration is repeated
to get concordantvalues.

B) Adsorptionof Acetic Acid on ActivatedCharcoal

i. 3 stoppered bottles are taken and clean and drythem.

ii. In those 3 labelled stoppered bottles, the following mixture are prepared (as given below) so as to make
total volume in each bottle as60ml.

Bottle number 1 2 3
60 50 40
Volume of 0.6 M CH3COOH(ml)
0 10 20
Volume of distilled water(ml)

14
iii. 2 grams of powdered charcoal are added to each bottle, stoppered, shaken well and let them stand for
45min with intermittentshaking.
iv. The content of bottle 1 is filtered into a conical flask. Then 10ml of the filtrate is taken into a 100ml
conical flask and titrated this against N/10(approx.) NaOH solution using phenolphthalein as indicator.
At the end point, the solution will turn pink. It was repeated to get concordantvalue.
v. The above process was repeated with contents of otherbottles.

Observation

o
Roomtemp= C

Table 1: Standardization of NaOH solution

No. Burette Reading
Volume of Volume of Mean Volume of
of (ml)
Standard Oxalic NaOH Solution NaOH Solution
Titration
Acid solution(ml) Initial Final (ml) VNaOH (ml)

Table 2: Titration of Acetic acid

Weight of activated charcoal in each bottle= 2g

Volume of acetic acid solutions for each titration= 5ml

Bottle Burette reading Volume of standard Mean value

number Initial Final NaOH Solution used(ml) (ml)

1 V1

2 V2

3 V3

15
Table 3: Adsorption of Acetic Acid by charcoal

Initial Concentration
Amount of Weight of
Bottle conc of of acetic acid Log
acetic acid the adsorbent x/m log C
no acetic acid after (x/m)
adsorbed (x) (m)
Ci adsorption(C)
1 0.6 M1 x1 2

2 0.5 M2 x2 2

3 0.4 M3 x3 2

Calculation

i) Standardization of NaOHsolution:

ii) Adsorption of Acetic Acid 0n Activated Charcoal:

Bottle no1:

16
ii) Bottle no2:

ii) Bottle no3:

17
Paste graph

18
Conclusion

Then a graph is plotted taking ‘log x/m’ in Y axis and ‘log C’ in X axis. A straight line is found that
prove the validity of the Frenudlich isotherm. From the Y intercept ‘log K’ is found and from the
slope of the line the value of ‘n’ is determined.
Thus, logK= andn=

Questions:

Teacher’s
signature……………….…………………..

20
ExperimentNumber…5 Date…………………

Objective: Determination of Percentage Composition of a Given Sugar Solution

using Oswald’s Viscometer

Theory

Whenever a liquid flow, each portion of it experience a resistance to flow while flowing across another
position. The co-efficient of viscosity is a measure of this resistance to flow. It is defined as tangential force
required maintaining a unit velocity gradient between two parallel layers of liquid of unit area and it can be
expressed asfollows:

Tangential force

area X velocity gradient

Its unit is poise and is given by dyne second/square cm.

In Ostwald Viscometer the force driving a liquid of viscosity (1) through capillary depends on the difference
in liquid level (h), the density (d1), and the acceleration due to gravity (g). So it is given by the expression
hgd1.

If exactly the same volume of liquid of viscosity 2, is introduced into the same tube, the driving force is equal
to hgd2, where d2 is the density of the second liquid.

Therefore for a given apparatus and the same volume of liquid, is proportional to the driving force and to the
time of outflow.

Hence, 2 hd 2 g t2

1 hd1g t1

2 d 2 t 2

1 d1t1

This expression gives the viscosity of the second liquid relative to that of the first.

21
Procedure

1. The Ostwald Viscometer tube is filled up first with distilled water of particular volume (as instructed during
lab class) and the time is noted with the help of stopwatch for distilled water to pass from one mark to
another mark in the viscometer. It is repeatedtwice.

2. Different sugar solutions (same volume) of known concentration (such as 2%, 5% and 10%) are taken
and the corresponding flow time in viscometer are noted using the above procedure. The above
procedure are repeated again for the supplied sample solution of unknownconcentration.

3. Thedensityof each solution areprovided.

Observation

Room temperature at the time of theexperiment= C

Table: Determination of time of flow

Types of Percentage
Sl. No. Density (gm/cc) Time of Flow (sec) Mean time (sec)
Solution of sugar

Ist reading
1. Water
2nd reading
1st sugar Ist reading
2.
solution 2nd reading

2nd sugar Ist reading

3.
solution 2nd reading

3rd sugar Ist reading

4.
solution 2nd reading
Ist reading
Given sugar
5. Z%
solution 2nd reading

22
Paste graph

23
Calculation
1. The viscosity of water at noted temperature was found out from literature given below waterat
C=
2. Relative viscosity of each solution was calculated from therelation:
d t
2  d 2 t2 water
1 1

Then a graph is plotted taking ‘coefficient of viscosity’ 2 in Y axis and percentage concentration of sugar
solutions in X axis. A straight line is found and the concentration of unknown sugar solution (Z%) is found out
by drawing perpendicular from the straight line from the point of coefficient of viscosity of unknown solution
on the Xaxis.
24
Conclusion

The percentage concentration of the unknown sugar solution =

---------------------------------------------------------------------------------------------------------------------
Viscosity Coefficient of water at different temperature (obtained from Literature)

Temperature Viscosity Co-efficient

(o C) (Centipoise)
20 1.005
25 0.8937
30 0.8007
40 0.6560
50 0.5494

Questions:

Teacher’s
signature……………….…………………..

25
 ExperimentNumber…6 Date…………………

Objective: pH-Metric Titration for Determination of Strength of a Given

HCl Solution

Theory

Most of the chemical and biochemical processes are profoundly affected by the acidity or alkalinity of media
in which they take place. Acidity of the solution depends not only upon the molarity of the acid but upon the
concentration of the hydrogen ions, produced by the acids. Due to some practical difficulties, the acidity or
alkalinity of a solution is not expressed in terms of hydrogen ion concentration. Sorensen suggested the use
ofpH(puissanced’hydrogen)scale.Onthesescale,pHofany solutionisdefinedas:pH=-log10[H+]

The pH of a solution can be accurately measured with the help of a pH meter, whereas the approximate
value of pH are determined using a multiple range indicatorsolution.

Measurement of pH can be employed to monitor the course of acid-base titrations. The pH values of the
solution at different stages of acid-base neutralization are determined and are plotted against the volumes of
the acid/alkali added. On adding a base to an acid, the pH rises slowly in the initial stages, then it changes
rapidly at the end point. Then it flattens out. The end point of the titration can be detected where the pH
changes more rapidly. However, the shape of the inflexion point (i.e. where the pH changes abruptly) and
symmetry of the curve on its two sides depends upon the ionisibility of the acid and the base used and on the
basicity of the acid and the acidity of the base.

Procedure

I. At first, the electrodes are calibrated using buffer solutions of pH = 4 and pH =7.

II. Standardization of NaOHsolution:

At first NaOH solution is taken in the burette. Now 25 ml of standard Oxalic Acid solution is taken out by
pipette into a conical flask and 25 ml distilled water is added to it. 1-2 drops of phenolphthalein indicator is
added to the solution and titrated with the NaOH solution until a pink coloured solution appeared. The
titration is repeated to get concordant value.

III. Measurement of pH of unknown HClsolution:

25 ml of given HCl solution is taken out by pipette into a 100 ml beaker and 25 ml of distilled water is
added to it. The temperature of the solution is measured and the electrode is dipped into the solution. The
reading shown is the pH value of the solution at the initial stage. Now NaOH solution is added to the
unknown HCl solution gradually from the burette (2 ml at a time) and mixed well. The corresponding pH
value of the solution is noted from the pH meter. Near the end point a very small amount (0.2 ml) ofNaOH

26
 solution is added because change in pH very much appreciable. This is because when the acid was
neutralized, further addition of such a small amount 0.01 ml raises the pH to about 9 or 10. A graph is
plotted between pH and volume of NaOH added. From the graph the volume of NaOH required for the
complete neutralization of unknown HCl solution is determined.

Observation:
Temperature of thesolution= C

Table 1: Standardization of NaOH solution

Volume of Burette Reading
No. Volume of Mean Volume of
Standard (ml)
of NaOH Solution NaOH Solution
Oxalic Acid solution
Titration Initial Final (ml) (ml)
(ml)
V

Table 2: Measurement of pH of unknown HCl solution (with NaOH solution)

Volume of NaOH Solution

SI. No. pH
(ml)

27
Calculation

(i) Standardization of NaOHsolution:

(ii) Determination of strength of unknown HClsolution:

28
Paste Graph

30
Conclusion

The strength of unknown HCl solution =

Questions:

Teacher’s
signature……………….…………………..

31
ExperimentNumber…7 Date…………………

Objective: Determination of Chloride Ion in a Given Water Sample by

Argentometric Method

Theory

Chlorides are present in water usually as NaCl, MgCl2 and CaCl2. Although chlorides are not harmful as such,
their concentrations over 250 ppm impart a peculiar taste to the water thus rendering the water unacceptable
for drinking purposes. Further, existence of unusually high concentrations of chloride in a water sample
indicates pollution from domestic sewage or from industrial waste waters. The HCl acid generated from the
hydrolysis of salts like MgCl2 in the boiler at high temperature and pressure causes corrosion in boiler parts.
Moreover, chlorides in the form of MgCl2 and CaCl2 cause permanent hardness.

By argentometric method chloride ions in water sample, which is neutral or slightly alkaline, can be
determined by titrating it against standard AgNO3 solution using potassium chromate as an indicator. The pH
should be in between 7-8. As at higher pH AgNO3 get precipitated as AgOH and at lower pH K2CrO4 indicator
is converted to K2Cr2O7 asfollows.

Ag+ + OH- ↔ AgOH

2K2CrO4 + 2HCl ↔ 2HCrO4 + K2Cr2O7 + H2O+2KCl

Ag+ reacts with Cl- and CrO 42- when AgNO 3solution is released from the burette to the sample solution which
has Cl-.

Ag+ + Cl- ↔ AgCl↓ (White ppt)

2Ag+ + CrO42- ↔ Ag2CrO4↓ (Red ppt)

Red colour formed because of formation of Ag2CrO4. This colour may disappear if the solution contains high
concentration of Cl- ion.

Ag2CrO4 + 2Cl- ↔ 2AgCl↓ + CrO 42-

When the concentration of Cl- ions has decreased, the red colour starts disappearing slowly and slowly on
shaking and a stage is reached when all the Cl- ions have formed AgCl. One extra drop of AgNO3 at this
point reacts with K2CrO4 and reddish coloured Ag2CrO4 is formedagain.

Procedure

(i) Standardization of AgNO3solution:

At first AgNO3 is taken in a burette. Now 25 ml of standard NaCl solution is taken out by pipette in a
conical flask. To this 5 ml of K2CrO4 is added as an indicator. The solution turned to yellow. It is then titrated
against AgNO3 till the colour changes from yellow to permanent reddish brown, followed by the coagulation
of red precipitate. The titration is repeated to get the concordantvalue.

32
(ii) Determination of chloride ion in test watersample:

25 ml of supplied test water sample is taken out by pipette in a conical flask. To this 5 ml of K2CrO4 is
added as an indicator. The solution turned to yellow. It is then titrated against AgNO3 taken in the burette till
the colour changes from yellow to permanent reddish brown, followed by the coagulation of red precipitate.
The titration is repeated to get the concordant value.

Observation

Table 1: Standardization of AgNO3 solution

Burette Reading
No. Volume of Mean Volume of
(ml) Volume of AgNO3
of NaCl solution AgNO3 Solution
Solution (ml)
Titration (ml) Initial Final (mL)

Vl

Table 2: Determination of chloride ion in test water sample

No. Volume of Burette Reading Mean Volume of

Volume of AgNO3
of Test Water (ml) AgNO3 Solution
Solution (ml)
Titration Sample (ml) Initial Final (mL)

V2

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Calculation

(i) Standardization of AgNO3solution:

(ii) Determination of chloride ion in test watersample:

34
Conclusion

The amount of chloride ion present in the supplied test water sample =

Questions:

Teacher’s
signature……………….…………………..

35
 ExperimentNumber…8 Date…………………

Objective: Determination of Rate Constant for the Hydrolysis of Ethyl acetate

Catalyzed by Hydrochloric acid

Theory

The hydrolysis of ethyl acetate by dilute HCl is a first order reaction as the concentration of water is in large
excess and does not change significantly during the progress of the reaction. It is thus called pseudo uni-
molecular reaction.

The essential step of the reaction is following:

dilHCL
CH 3 COOC 2H 5H2 OCH 3 COOHC 2 H 5 OH
The specific rate constant of this reaction K is given by:
2.303 a
K log10
t ax
Where ‘a’ is the initial concentration of ethyl acetate and (a-x) is that of remaining concentration after time ‘t’.

The progress of the reaction can be studied by withdrawing measured volume of aliquot from the reaction
mixture from time to time and titrating with alkali. The volume of alkali required at any stage is equivalent to the
sum of acetic acid produced and acid used initially, which is a constant quantity.

If V0, Vt and V∞ are the volume of alkali required for the same volume of aliquots initially, at time t and at infinite
time, then
a = V∞- V0 and (a-x) = V∞- Vt

2.303 V  V0
 K  log 10
t V  Vt

As the reaction between ester and acid is very fast, the determination of V0 becomes difficult, it is better to take
the difference of two times such that

2.303 V  V0
t1 log 10
K V  V1

and

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 2.303 V  V0
t n  log 10
K V  Vn

2.303 VV1
t n  t n  t1  log10
K VVn

Where, V1 and Vn are the volume of alkali required at time t1 and tn respectively.

Iflog 10V  V1is plotted against tn, a straight line passing through origin is obtained.
V  Vn

From the slope of which ‘K’ can be determined.

Procedure

1. 100 ml 0.5 (N) HCl solution was pipette out in a 250 ml conical flask and it was set in a water-bath at room
temperature.

2. The burette was filled with 0.1 (N) NaOHsolution.

3. Six 50 ml conical flasks were taken and 15 gm ices were added in each of the aboveflask.

4. Now, 5 ml of ethyl acetate was pipette out and added to the 250 ml previous flask. A stopwatch was
started when the pipette is halfdischarged.

5. Immediately, 10 ml of the reaction mixture was pipetted out and transferred to first conical flask containing
ice. Time was noted when the pipette is half discharged. It was titrated against 0.1 (N) NaOH solution
using phenolphthalein as indicator. Appearance of light pink colour, marked theend-point.

6. The above step (procedure 5) was repeated at least for six times at 5 minutes regular intervals noting the
time of half discharge in eachcase.

7. Finally, the above 250 ml flask was removed from the water bath and it was placed in a separate water
bath at temperature of 600C for about one hour. 10 ml of reaction mixture was pipetted again and titrated
against 0.1 (N) NaOH solution using phenolphthalein as indicator. This givesV∞.

Observation

Experimentaltemperature= C

Volume of alkali at infinite time,V∞= ml

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Table1: Determination of rateconstant

Time of half Vol. of aliquot Burette reading

No. of Mean reading V Vn
discharge (ester in HCl) (ml)
obs. (vol. of NaOH)
(sec) (ml) Initial Final

Table 2: For drawing of graph

V V1
y-axis log10
V  V n

x-axis t = tn – t1

The slope of the line =

The specific rate constant K = 2.303 × slope =

38
Paste graph

39
Conclusion

The rate constant of the reaction =

Questions:

Teacher’s
signature……………….…………………..

40
 ExperimentNumber…9 Date…………………

Objective: Analysis of components of given mixture by thin layerchromatography

Theory

In thin-layer chromatography, the stationary phase is a polar absorbent, usually finely ground alumina or
silica particles. This absorbent is coated on a glass slide or plastic sheet creating a thin layer of the particular
stationary phase. Almost all mixtures of solvents can be used as the mobile phase. By manipulating the
mobile phase, organic compounds can be separated. TLC is a quick, inexpensive microscale technique that
can be used to determine the number of components in a mixture, verify a substance’s identity, monitor the
progress of a reaction, determine appropriate conditions for column chromatography, analyze the fractions
obtained from columnchromatography.

In addition to qualitative results, TLC can also provide a chromatographic measurement known as an
Rfvalue. The Rfvalue is the “retardation factor” or the “ratio-to-front” value expressed as a decimal fraction.

The Rfvalue can be calculated as:

Rf= distance spot travels/distance solvent travels

Procedure:

A large stock TLC plate is made from the box into rectangles measuring the dimensions for 1.5 x 4 cm
plates. From the bottom straight across the plate a line of about 0.5 cm is drawn using pencil. Separate dots
are spotted on the plates with the unknown mixture and different standards. Each dot should be as small as
possible, preferably less than 2 mm in diameter. Now the plate is examined under the UV light to see that
enough of the compound has been applied by observing a visible dark purple dot; if not visible, more is added
and then the dots are labelled.

Now the plate is dipped into the mobile phase( mixture of polar & non-polar solvent) kept in a container so
that dots can move upward along with the mobile phases.

After the solvent has risen to the top of the plate or at least within a cm of the top, the plate is removed
with forceps and immediately the solvent is marked front with a pencil. The solvent is allowed to completely
evaporate. Now under the UV lamp the plate is examined to see the components as dark spots. The spots can
also be visualized by putting the plate in an iodine chamber. The spots are marked with a pencil and the
distances travelled are measured using ascale.

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 Preparation of mobile phase

n- butanol 12 ml
Acetic acid 10ml
water 5 ml

Observation Table:

Table 1: Determination of Rf values:

Distance
Mixture of Distance Travelled
S. No. Travelled by Rf values
Amino Acids by Amino acids
Solvent
1.

2.

3.

4. Unknown

Calculation:

Rfvalue for each spots and identify the components present in given sample.

Rƒ = (distance spot travels) ÷ (distance solvent travel)

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Conclusion:

The Unknown sample contains ……………………………………

Question:

Teacher’s
Signature.....................................

43
ExperimentNumber…10 Date…………………

Objective:DeterminationofRedoxPotentialsandcellEMFsbypotentiometric
method.

Theory

In the Daniel cell, copper and zinc electrodes are immersed in a solution of copper (II) sulfate [CuSO4 (aq))
and zinc (II) sulfate (ZnSO4 (aq)] respectively. The two half cells are connected through a salt bridge. Here
zinc acts as anode and copper acts as cathode.

At the anode, zinc undergoes oxidation to form zinc ions and electrons. The zinc ions pass into the solution.
If the two electrodes are connected using an external wire, the electrons produced by the oxidation of zinc
travel through the wire and enter into the copper cathode, where they reduce the copper ions present in the
solution and form copper atoms that are deposited on thecathode.

The anode reaction is represented as:

The cathode reaction is represented as:

Total cell reaction is the sum of the two half-cell reactions:

A salt bridge have to prepare by using salts like, KCl, KNO3, NH4NO3 are used as the electrolyte. Its main
function is to prevent the potential differences that arise between the two solutions when they are in contact
with each other. This potential difference is called the liquid junction potential. It completes the electrical
circuitbyconnectingtheelectrolytesinthetwohalfcells.Itpreventsthediffusionofsolutionsfromonehalf

44
cell to the other. It maintains the electrical neutrality of the solutions in the two half cells.

In Daniel cell, the electrode potentials of the half cells are written as:

So Nernst equation is generally represented as:

Where, is the activity (Concentration) of reducedspecies,and is the activity (Concentration) of

oxidised species.

Procedure

Preparation of electrolytes of different concentration

The following solutions of various concentrations are prepared from the supplied 1(M) CuSO4 and ZnSO4
solution respectively by dilution.

Conc. of CuSO4 Volume taken (ml) Conc. of ZnSO4 Volume taken (ml)
1(M) water 1(M) water
0.5(M) 100 ml 100ml 0.5(M) 100 100
0.025(M) 5 195 0.025(M) 5 195
0.0125(M) 2.5 197.5 0.0125 2.5 197.5

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 Estimation of cell emf

 The Zn bar is dipped into ZnSO4 and Cu bar into CuSO4 solution followed by inserting the salt bridge
(dipped in KNO3 solution) for bridging both cellcompartments.
 Twofinelypiecescopperwireareusedto maketheelectricalcontactoftwometalbarwithavoltmeter.
 Then switched on the voltmeter to observe the cell potential value and continued to take the reading by
varying the concentration of theelectrolytes.

Observation

Table 1: Determination of EMF of the Cell:

Concentration of Concentration of EMF of the cell E0(cell)
SL. No.
ZnSO4 (M) CuSO4 (M) (volt)

1.

2.

3.

4.

5.

6.

Calculation

The Redox potential of cell for following pairs:

1.

2.

3.

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4.

5.

6.

Conclusion:

1. The Redox potential ofDanielcell is

Questions:

Teacher’s
signature……………….…………………..

47
AdditionalExperiment Date…………………

48
50