Applied Chemistry (Ar23) Student Manual
Applied Chemistry (Ar23) Student Manual
Applied Chemistry (Ar23) Student Manual
(AR-23)
APPLIED CHEMISTRY LABORATORY
STUDENT MANUAL CUM OBSERVATION BOOK
(Common to EEE,ECE,CSE,CSM,CSD,CSC &CSO)
Prepared by
Dr.G.V.Siva Prasad (HoD) Dr.Anindita Chatterjee Dr.M.Ravikumar Dr.D.Vasundhara
Professor Professor Professor Associate professor
Dr.D.Varaprasad Dr.G.Jaishree
Associate professor Associate professor
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CERTIFICATE
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Signature of Instructor
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I-I 23BS203 APPLIED CHEMISTRY LABORATORY L T P C
I-II 23BS203 LIST OF EXPERIMENTS 0 0 2 1
Be punctual.
Bring manual, record, notebook, calculator etc.
Maintain discipline and cleanliness in the laboratory.
Handle the apparatus and reagent bottles with almost care.
Report, breakage of glass wares to the laboratory Assistant immediately.
Keep the reagent bottles in their respective places after use.
Do not misplace the stoppers of the bottle.
Do not throw waste paper, match - stick, broken glass wares etc., inside the sink; put them
into the dust bin.
Do not discharge concentrated acid into the sink, dilute it before discharging.
In case of accident, inform the faculty immediately
Before taking any liquid in the burette or the pipette, these should be rinsed with the liquid.
The conical flask should not be rinsed with any liquid. It should simply be washed with
distilled water.
Read the lower meniscus in case of colorless liquids and the upper one in the case of colored
liquids.
The solution should be filled in the burette by means of a funnel which must be removed
before titrations.
The readings should be entered immediately in the practical note-book and not on some piece
of paper.
When the experimental is over, wash all the glass wares and handover to the laboratory
assistant before you leave the lab.
Playing of radios, tapes, CDs is not permitted.
Do not eat, drink in the laboratory.
Never attempt any unauthorized or unassigned experiments
For those experiments where students are to work in pairs, lab partners will be assigned
randomly as announced by the instructor at the beginning of the lab period. You may not
exchange lab partners. Both lab partners must be present for the entire experiment.
All lab reports are to be your own. Lab partners are to independently produce their lab
reports.
Lab reports are due one week from the date of performance, at the beginning of the lab
period.
In the event of copying, all students involved will receive a grade of zero; therefore do not
give a copy of your lab report to another student.
Using mobiles phones are strictly prohibited in laboratory.
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COMMON LABORATORY GLASSWARES
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SAFETY SYMBOLS
*Not hazardous, but these compounds need to be stored in anhydrous conditions. While
preparing reagents, due to their hygroscopic nature, their weight may vary and have effect on
calculations.
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Expt. No Date
0
BASIC CONCEPTS OF VOLUMETRIC ANALYSIS
Titration: The process of finding out the volume of one of the solution (titrant) required to react
completely with the definite volume of other solution (analyte).
Titrant: The solution of known strength. (Usually taken in burette)
Titrate (analyte): The solution which contains a substance whose strength is to be estimated. (Taken
in conical flask)
Indicator: The substance which indicates the end point of titration by changing its color is called
indicator. Eg: Phenolphthalein, methyl orange, EBT, FSBF, Starch, potassium chromate etc.,
End point: the point where the titrant is added to slightly excess to the equivalence point and the
indicator changes its color is known as end point.
Equivalence point: the point where the titrant is added until it chemically equivalent to the analyte is
known as equivalence point. It is an exact point.
Strength: The amount of substance dissolved in one liter of a solution expressed in termed as
strength of a solution. Strength of solution can also be expressed in any of the following ways.
i. Normality: It is the number of gram equivalents of the substance dissolved per liter of the solution.
It is denoted by N.
ii. Molarity: It is the number of moles of solute per litre of the solution. It is denoted by M.
iii. Molality: It is the number of moles of the substance dissolved in 1000gm or 1kg of the solvent. It
is denoted by m.
iv. Percentage by weight: It is the weight in grams of a solute present in 100gms of the solution.
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Weightof solute×100
Percentage weight =
Weight of solute + weight of solvent
v. Equivalent Weight: The equivalent weight of a substance is defined as the number of parts by
weight of it that combine with or displace one part by weight of hydrogen or eight parts by weight of
oxygen.
Atomic weight
Equivalent weight of a metal =
Valency
Primary Standard substance: A standard solution is one which is prepared by dissolving an exactly
weighed quantity of a (such as K2Cr2O7, Na2CO3, H2C2O4 etc.,) in a known volume of distilled
water.
However, strength of these solutions should be ascertained by titrating against a standard solution
referred above, before using.
2) Complexometric reactions: The titration involving the formation of a stable soluble complex
between the metal and the complexing agent (ligand).
4) Oxidation – Redox reactions: These reactions involve the change in oxidation number or
transfer of electrons among the reacting substances.
Click on:
1. https://youtu.be/IbkreR5VDmo
2. https://youtu.be/sFpFCPTDv2w
TITRATION ERRORS
Many errors occur due to analyst or method or reagent or uncalibrated glassware and
interference of the indicator. To avoid these errors statistical treatment of the titration values is
necessary. Hence, ‘Most Probable value’ is taken as the result.
MOST PROBABLE VALUE: Even when a quantity is measured with possible accuracy,
the results of a successive observation differ among themselves. The average value of these results is
taken as most probable value. Hence, it is not a true value.
ACCURACY: It is the concordance between measured value and most probable value or
true value.
RELATIVE ERROR: It is the absolute error divided by true or most probable value. It is usually
expressed in terms of % ppm.
RELATIVE MEAN DEVIATION: It is the mean deviation divided by the mean. It is expressed in
% or ppm. It is a measure of precision.
STANDARD DEVIATION: It measures the closeness of the results with the mean. Smaller
the Standard deviation, more closely are the results to the mean value.
RELATIVE STANDARD DEVIATION (RSD): It is a measure of the quality of the sample. Large
the RSD, shows the poor the quality of the sample.
1. Calculate the weight of sodium carbonate required to prepare 250 ml of 0.05N solution.
2. Calculate the normality of oxalic acid solution when 0.63 g of substance is dissolved in
100ml of the solution.
6. 21ml of 0.05M Na2CO3 Solution is titrated with HCl solution for standardization of HCl and
11.3mLof HCl is consumed when methy orange indicator is used. Calculate the molarity of
HCl.
Marks awarded
Signature of the Instructor
| 13
Expt. No 1 Date
APPARATUS CHEMICALS
1. 250ml conical flask, 1. Standard MgSO4
2. 50ml Burette, 2. EDTA solution
3. Burette stand, 3. Water sample
4. Wash bottle 4. Buffer solution (NH4Cl+NH4OH) (pH-10)
5. 10ml,50ml measuring cylinders, 5. Eriochrome black-T,
6. 250mlVolumetric flask
7. 250ml Beaker
8. Hot plate
9. Funnel
10. Filter paper
PRINCIPLE:
EDTA is a well known complexing agent, forms stable complex with Ca and Mg ions as well as
many other metal ions in aqueous solution. It reacts with metal ions 1:1 ratio.
Hard water which contains Ca2+ and Mg2+ ions react with EBT forms unstable wine red color
complex at pH 9-10.
Ca2+ (or) Mg2+ + EBT→ [Ca-EBT] (or) [Mg-EBT]
(Wine red color complex)
During the titration, the wine red coloured complexes [Ca-EBT] (or) [Mg-EBT] react with EDTA
and forms a stable colorless complexs [Ca-EDTA] (or) [Mg-EDTA] by releasing blue colour
indicator into the solution. Hence the color change at end point is wine red to blue.
PROCEDURE:
Rinse the burette with EDTA and fill the same solution up to the mark avoiding air gaps.
Pipette out 10 ml of standard MgSO4 into a conical flask, add 3 ml of buffer solution, 2-3
drops of Eriochrome Black-T indicator and 20ml distilled water.
Titrate the above wine red solution with standard EDTA solution taken in the burette, till the
wine red color changes to blue and tabulate the volume.
Repeat the same procedure until two concurrent values are obtained.
End Point: Wine red color solution changes to pale blue
OBSERVATIONS:
M1V1 M2V2
= ;
𝑛1 n2
n1=n2=1
OBSERVATIONS:
Trail-1 50.0
Trail-2 50.0
Trail-3 50.0
M3V3 M4V4
𝑛3
= ; n3=n4=1
n4
RESULT: The hardness of the given water sample has been found to be as follows:
SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
THEORY
Strength of acid in Lead-Acid battery, measure of its ability to neutralize with bases to resist change
of pH value of acid due to presence of mineral acids like H2SO4.
PROCEDURE:
Step-1: preparation of standard Oxalic acid:
Rinse the burette with NaOH solution; take NaOH solution into the burette.
Pipette out 10ml of standard oxalic acid into a conical flask, add 2-3 drops of phenolphthalein
indicator and 20ml distilled water.
Titrate the colorless solution with NaOH till pale pink color is obtained as end point.
Repeat the titration to get concurrent values.
OBSERVATIONS:
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Volume of oxalic acid Burette readings Volume of NaOH
S.No. solution taken in ml. Initial Final Solution
(V1) consumed in ml.( V2)
Trail-1
Trail-2
Trail-3
CALCULATIONS:
By volumetric principle V1 N1 = V2 N2
OBSERVATIONS:
CALCULATIONS:
By volumetric principle V3 N3 = V4 N4
Amount of H2SO4 present in100ml of given solution= N3× Eq.Wt H2SO4 × 100/1000
= × 49/10 gms/100cc
= × 49 /10 gms/100cc
RESULT:
SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
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THEORY/ PRINCIPLE:
Ferrous iron is oxidized to ferric iron by potassium dichromate in acid solution. The completion of
the oxidation of reaction is marked by the appearance of blue violet color of the diphenylamine
which is used as an internal indicator.
PROCEDURE:
Step-1: preparation of standard K2Cr2O7:
CALCULATIONS:
Volume of ferrous iron solution (V1) =10 ml
Normality of ferrous iron solution (N1) = ?
Volume of K2Cr2O7 (V2) = ml (titre value)
Normality of K2Cr2O7 (N2) =0.05N
By volumetric principle V1 N1 = V2 N2
Amount of ferrous iron present in 100ml of the given solution = N1× Eq.wt of ferrous iron×
100/1000
= × 55.85 /10
SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
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Application of the Experiment:
To estimate the amount iron of Fe+2 in test solution by preparing a Standard FAS solution &
using K2Cr2O7.
To Estimation of Iron in haematite ore solution using standard K2Cr2O7 solution
To Estimation of Iron in rust solution using standard K2Cr2O7 solution
APPARATUS CHEMICALS
1. Crucible 1. Anhydrous Calcium chloride
2. Muffle furnace
3. Electric oven
4. Desiccator
5. Tongs
Theory:
Coal is fossil fuel which occurs in large the earth crust. It was been formed by the partial decay of
plant materials accumulated millions years and further altered by action of heat and pressure. Coal is
highly carbon matter and important fuel. The process of conversion of wood into coal be represented
as
Wood ------> Peat ------->Lignite---> Bituminous---------->Anthracite
The coal is classified according to rank which measure of change. It has underground in the
transition from wood to anthracite rank based on carbon content. The composition of coal varies
widely and hence it is necessary to analyze and interpret the result from the point of commercial
classification , the price fixation and proper industrial utilize, the following methods are analyze can
be used for moisture content in coal.
PROXIMATE ANALYSIS
This includes the determination of moisture, volatile matter, ash and fixed carbon content, which
give value information regarding the commercial classification. This is known as proximate analysis.
Procedure:
Determination of Percentage Moisture:
Weight of Weight of the Weight of Crucible along with Weight of crucible along with
crucible Sample (W3) substance (Before Heating) W1 substance (After heating) W2
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Calculation of moisture content:
Calculate the present of moisture in the analysis in the sample as follows
Loss in wt.of coal
% of moisture in coal = ×100
wt.of coal initially taken
W1−W2
% Moisture content = W3 ×100
Where
W1= mass of the crucible and sampler
W2=mass of crucible
W3= mass of sample in grams
SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
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Expt. No 5 Date
Procedure:
1. ZnO nano particles:
The aqueous solution (0.2M) of zinc nitrate (Zn (NO3)2.6H2O) and the solution (0.4 M) of KOH were
prepared with deionized water, respectively. The KOH solution was slowly added into zinc nitrate
solution at room temperature under vigorous stirring, which resulted in the formation of a white
suspension. The white product was centrifuged at 5000 rpm for 20 min and washed three times with
distilled water, and washed with absolute alcohol at last. The obtained product was calcined at 500
°C in air atmosphere for 3 hr.
SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
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Expt. No Date
6
CONDUCTOMETRIC TITRATION OF STRONG ACID VS. STRONG BASE
AIM: To determine the amount of strong acid (HCl) present in the given sample by conductometric
titration with NaOH solution of strength 0.1N.
APPARATUS CHEMICALS
1. Conductivity meter 1. 0.1N standard oxalic acid
2. Conductivity cell 2. 0.1N NaOH solution
3. 50ml Burette, 3. HCl solution,
4. 100ml Beaker, 4. Distilled water
5. Glass rod,
6. 20ml Pipette
PRINCIPLE
The conductmetric titration is a volumetric analysis based upon the measurement of conductance
during the course of titration. Conductance of the solution (electrolyte) depends on the number of
ions and their mobility. When one electrolyte is added to another electrolyte, the change in number of
free ions causes a change in the conductance.
For example when a strong acid (HCl) is titrated against a strong base (NaOH), before NaOH added
from the burette, the acid solution has high conductivity due to the highly mobile H+ ions. When
NaOH added is added to the acid, the conductivity of the acid solution decreases due to the
neutralization of highly mobile H+ ions of the acid with OH- ions of base.
Thus the conductance of the solution continues to decrease until the equivalence point reached.
Further addition of NaOH will increase the conductance by highly mobile OH- ions.
The point of intersection of the graph plotted by conductance of the solution against volume of base
added corresponds to the end point of the titration.
PROCEDURE
Step-1: preparation of standard Oxalic acid:
Rinse the burette with NaOH solution; take NaOH solution into the burette.
Pipette out 10ml of standard oxalic acid into a conical flask, add 2-3 drops of phenolphthalein
indicator and 20ml distilled water.
Titrate the colorless solution with NaOH till pale pink color is obtained as end point.
Repeat the titration to get concurrent values.
OBSERVATIONS:
CALCULATIONS:
By volumetric principle V1 N1 = V2 N2
Fill the burette with standard NaOH solution and clamp it to burette stand.
20 ml of the given HCl is pipetted out in to a clean 100 ml beaker and then diluted to 50 ml
by adding distilled water.
The conductivity cell is washed with water and then immersed in the solution.
Initial conductance is read in the instrument for the acid alone without the addition of NaOH.
Now 0.5 ml of NaOH solution from the burette is added to the solution taken in the beaker,
stirred and then conductivity is measured.
The process is continued up to the end point i.e at least five points beyond the equivalence
point.
After the end point, further NaOH is gradually added and few more readings are noted.
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S.No Vol.of Measured Corrected S.No Vol.of Measured Corrected
NaOH Conductance conductance NaOH Conductance conductance
(V1) (C) C1 = (C) C1 =
C(V+V1/V) C(V+V1/V)
1 16
2 17
3 18
4 19
5 20
6 21
7 22
8 23
9 24
10 25
11 26
12 27
13 28
14 29
15 30
GRAPH:
A plot is made between volume of NaOH added along X-axis and the conductance of solution along
Y- axis. The end point is intersection of the two lines.
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CALCULATION:
= N
Concentration of HCl(N2) = N
The amount of HCl present in the whole of the given solution =N2 × Eq.wt. of HCl
= ×36.45
= g/lit
RESULT:The amount of HCl present in the whole of the given solution (or)
SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
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Probable viva-voce questions
1. What are conductometeric titrations?
Ans: The volumetric titration which involves the determination of strength of given solution by
measuring conductance of the solution is called conductometric titration
2. Give the factors on which conductance of a given solution depends ?
Ans: Conductance depends on two factors:-
1. No’s of ions
2. Mobility of ions
3. In the experiment you have done, what is the pH of the solution before & after the titration?
Ans: In metal the conductance is due to movement of free ions. Before titration solution contains
HCl therefore pH is acidic, after titration solution contains NaOH therefore pH is basic.
4. What is specific conductivity ? Give its units
Ans: Specific conductivity is defined as the conductance of ions per centimeter cube of solution.
It is denoted by k { kappa }.
Specific conductance = cell constant / absorbed resistance
Its units are ohm-1cm-1 or mhocm-1 or scm-1
5. What is the difference between conductance of metal and electrolytic solutions?
Ans: In metals the conductance is due to movements of free electrons. In electrolytic solution, the
conductance is due to moving ions.
6.What are the advantages of conductometric titrations over volumetric titrations?
More accurate results are obtained because the end point is determined graphically
Titration can be carried out along with coloured solution
These are successful even in weak acids and strong base
This method gives more accurate results even with weak acids against weak bases.
7. What could be the shape of graph of strong acid vs strong base? Ans: V-shape
8. What is the equivalent weight of HCl? Ans: 36.5
9. What is a conductivity cell? Ans: The vessel in which the measurement of conductivity of the
solution is to be made is known as conductivity cell. They are of various shapes and sizes depending
upon the nature of the solution taken.
10. What is cell constant? Ans: It is the ratio between the distance of two parallel plates of the cell
and the area of the electrode. Its unit is cm-1.
11. What is the relationship between conductance and concentration of electrolyte?
12. What is an electrolyte?
13. What are the factors affecting conductance of an electrolyte?
14. What are the units of conductance?
15. What is the cell constant of a conductivity cell you used in this experiment?
16. What are the units of cell constant?
17. What is corrected conductance?
18. Discuss the pattern of graph obtained during this titration.
19. How the end point for a particular reaction is calculated using this, titration method?
Ans: Plotting a graph between conductance and volume of the base, the point of Intersection of the
straight lines gives the end point.
20.Why conductance decreases on addition of NaOH to HCI ?
Ans: During the titration the fast moving hydrogen ions are replaced by the slow moving Sodium
ions, as a result the conductance of the solution decreases.
21.What is the unit for conductance? Ans: The unit for conductance is mho.
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Expt. No 7 Date
AIM: To determine the amount of Weak acid (CH3COOH) present in the given sample by
conductometric titration.
APPARATUS CHEMICALS
1. Conductivity meter 1. 0.1N standard oxalic acid
2. Conductivity cell 2. 0.1N NaOH solution
3. 50ml Burette, 3. CH3COOH solution,
4. 100ml Beaker, 4. Distilled water
5. Glass rod,
6. 20ml Pipette
PRINCIPLE
The conductmetric titration is a volumetric analysis based upon the measurement of conductance
during the course of titration. Conductance of the solution (electrolyte) depends on the number of
ions and their mobility. When one electrolyte is added to another electrolyte, the change in number of
free ions causes a change in the conductance.
When weak acid is titrated with strong base, the conductance of the solution is low in the beginning,
since the dissociation of weak acid is very low. On addition of base, highly dissociated sodium
acetate is formed. Due to the common ion effect, the acetate ion tends to suppress the ionization of
acetic acid. Later the conductivity begins to increase due to the conductivity power of the highly
ionized salt exceeds that of weak acid. After end point, the addition of NaOH contributes sharp
increase in the conductivity of the solution. The point of intersection of the two cures gives the end
point of the titration.
PROCEDURE
Step-1: preparation of standard Oxalic acid:
Rinse the burette with NaOH solution; take NaOH solution into the burette.
Pipette out 10ml of standard oxalic acid into a conical flask, add 2-3 drops of phenolphthalein
indicator and 20ml distilled water.
Titrate the colorless solution with NaOH till pale pink color is obtained as end point.
Repeat the titration to get concurrent values.
OBSERVATIONS:
CALCULATIONS:
By volumetric principle V1 N1 = V2 N2
Fill the burette with standard NaOH solution and clamp it to burette stand.
20 ml of the given CH3COOH is pipetted out in to a clean 100 ml beaker and then diluted to
50 ml by adding distilled water.
The conductivity cell is washed with water and then immersed in the solution.
Initial conductance is read in the instrument for the acid alone without the addition of NaOH.
Now 0.5 ml of NaOH solution from the burette is added to the solution taken in the beaker,
stirred and then conductivity is measured.
The process is continued up to the end point i.e at least five points beyond the equivalence
point.
After the end point, further NaOH is gradually added and few more readings are noted.
| 35
S.No Vol.of Measured Corrected S.No Vol.of Measured Corrected
NaOH Conductance conductance NaOH Conductance conductance
(V1) (C) C1 = (C) C1 =
C(V+V1/V) C(V+V1/V)
1 16
2 17
3 18
4 19
5 20
6 21
7 22
8 23
9 24
10 25
11 26
12 27
13 28
14 29
15 30
GRAPH:
A plot is made between volume of NaOH added along X-axis and the conductance of solution along
Y- axis. The end point is intersection of the two lines.
CALCULATION:
= N
The amount of CH3COOH present in the whole of the given solution =N2 × Eq.wt. of CH3COOH
= × 60
= g/lit
RESULT:The amount of CH3COOH present in the whole of the given solution (or)
SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
| 37
Expt. No 8 Date
APPARATUS CHEMICALS
1. Conductivity meter 1. Potassium chloride
2. Conductivity cell 2. Distilled water
3. Beaker
4. Standard flask
5. Glass rod
Theory: -
Conductance is the reciprocal of resistance. It is depend upon three factors, number of ions, and
nature of ions and mobility of ions towards their respective electrodes. The specific conductance of
electrolyte is decreased by increasing its dilution and equivalent conductance is increased by
increasing its dilution. The observed conductivity of an electrolyte will be equal to its specific
conductivity if cell constant is one.
Procedure: -
Prepare 0.1M KCl solution by weighing accurately 0.7455gm of KCl into a clean 100ml
standard flask.
From this 0.1M KCl solution prepare 100ml each of 0.05M, 0.02M, 0.01M, 0.005 and
0.001M KCl solutions.
Take about 40ml of each solution in to a clean and dry 100ml beaker and dip the conductivity
cell and make necessary connections. Measure the conductance of each solution and note
down.
Specific conductance
Cell constant =
observed conductance
| 38
Part-B: determine the conductance of all the prepared solutions of KCl and calculate the their
specific and equivalent conductance.
Result:
Cell constant =_______________ cm-1
Equivalent conductance of KCl at infinite dilution ( Λ0 ) =………………. ohm-1 cm2 gr.eq-1
SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
APPARATUS CHEMICALS
1. pH meter 1. 0.1N Oxalic acid
2. Glass electrode 2. 0.1N NaOH
3. Buffer solutions (pH-4.0, 9.0) 3. 0.1N Acetic acid
4. 100cc Beaker 4. Distilled water
5. 50cc Burette 5. Phenolphthalein indicator
6. 100cc Volumetric flasks(3)
7. 250cc Conical flask
8. 10cc Pipette
9. 50cc Measuring cylinder
PRINCIPLE
The titration of a weak acid with a strong base involves the direct transfer of protons from the weak
acid to the hydoxide ion. The reaction of the weak acid, acetic acid, with a strong base, NaOH, can
be seen below. In the reaction the acid and base react in a one to one ratio.
Rinse the burette with NaOH solution; take NaOH solution into the burette.
Pipette out 10ml of standard oxalic acid into a conical flask, add 2-3 drops of phenolphthalein
indicator and 20ml distilled water.
Titrate the colorless solution with NaOH till pale pink color is obtained as end point.
Repeat the titration to get concurrent values.
CALCULATIONS:
By volumetric principle V1 N1 = V2 N2
Fill the burette with standard NaOH solution and clamp it to burette stand.
Make up the given CH3COOH solution up to the mark with distilled water and shake the
flask well for uniform concentration.
Pipette out 25.0 ml of the given CH3COOH in to a clean beaker and add 3-4 drops of
phenolphthalein indicator.
Put the rinsed pH probe into the beaker of CH3COOH, swirl and record the initial pH.
Add small quantity of NaOH from the burette using following scheme
| 41
S.No Volume pH ∆pH S.No Volume pH ∆pH S.No Volume pH ∆pH
of NaOH ∆V of NaOH ∆V of NaOH ∆V
added added added
1 0.0 16 31
2 17 32
3 18 33
4 19 34
5 20 35
6 21 36
7 22 37
8 23 38
9 24 39
10 25 40
11 26 41
12 27 42
13 28 43
14 29 44
15 30 45
Plotting graph: Plot a graph taking pH on ordinate and Volume of NaOH added on abscissa
CALCULATION:
Volume of NaOH (V3) = ml (titer value from graph)
Normality of NaOH (N3) = M (given)
Volume of CH3COOH(V4) = ml (taken in beaker)
Normality of CH3COOH (N4) =----------------? (to be find)
Principle: Beer’s law is applicable to only to dilute solutions. It states that when a monochromatic
light is passed through a solution intensity of light decreases with thickness and this decrease in
intensity is directly proportional to the intensity of incident light and the concentration of the
solution.
I = I0 e-ε c l
Where I = Intensity of the transmitted light;
I0 = Intensity of the incident light
C = Concentration of the solution;
l = Path length of the cuvette
ε = Molar extinction coefficient
ln (I/ I0)= -εcl
The value of ε (epsilon) depends on the nature of the absorbing solute but independent of the
concentration of the solution. Decrease in the intensity of the transmitted light is due to the
absorption of light, which may lead to photochemical reactivity.
In colorimetric studies transmittance is defined as the fraction of light passes through the sample.
% Transmittance (T) = (I /I0) x 100
A more useful and convenient quantity in performing analysis is the absorbance or negative log of
transmittance.
Absorbance or Optical density= A= log (1/T) = - log (T)
A linear relation exists between absorbance (O. D) and concentration of the sample is known as
Beer’s law.
Absorbance or Optical density= A= log (I0/I) = εcl
| 44
Before verification of Beer’s law, it is necessary to a select a suitable wave length and determines
whether Beer’s law is valid at the wavelength selected. The most suitable wavelength is that at which
maximum absorbance is observed, called λmax. The λmax will always be at the same wavelength for
a given solution under any condition.
Filter Selection: (Calculation of λmax)
Prepare 100 ml, 0.2M CuSO4 solution (stock solution), fill it in a burette
Switch on the instrument; wait for 10 minutes for ‘warmup’ of the instrument.
Take one clean and dry glass (only for visible range scan) or quartz cuvette with a given
path length (say, 1 cm).
Prepare a blank by filling a cuvette 3/4 full with distilled water
By using blank cuvette (with distilled water) calibrate the colorimeter (absorbance = 0,
transmittance =100 %) at filter 1 and putout the blank cuvette.
Then fill cuvette with the stock solution and measure absorbance, note the reading in table.
Repeat the above step for all the filters (wave length range)
From table we can see the λmax i.e. wave length at which solution show maximum
absorbance/ O.D.
Model graph: A graph is plotted between optical density and concentration of CuSO4 .A straight
line passing through the origin is obtained. Slope of the line is equal to Molar extinction co-efficient
Result: A straight line passing through origin is obtained in the graph. Hence, Beer’s law is verified.
SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
| 46
Expt. No 11 Date
PREPARATION OF BAKELITE
(DEMONSTRATION ONLY)
APPARATUS CHEMICALS
1. Beaker 1. 36-45% formaldehyde
2. Measuring cylinder 2. Phenol
3. Fume hood 3. Glacial acetic acid
4. Glass rod 4. Conc. HCl
5. Copper bath
Theory: Phenol formaldehyde resin or P-F resin or phenolic resins (also called phenoplasts) are
important class of polymers which are formed by condensation polymerization of phenol and
formaldehyde in acidic or alkaline medium. Following steps are involved
| 47
Procedure:
1. Place 5 mL of glacial acetic acid and 2.5 mL of 40 % aq formaldehyde solution in a 100 mL
beaker. Add 2 g phenol safely.
2. Wrap the beaker with a wet cloth or place it in a 250 mL beaker having small amount of
water in it.
3. Add conc. HCl drop wise with vigorous stirring by a glass rod till a pink coloured gummy
mass appears.
4. Wash the pink residue several times with to make it free from acid.
5. Filter the product and weigh it after drying in folds of a filter or in an oven. Report the yield
of polymer formed.
Precautions:-
1. While adding conc. HCl, it is better to stay little away from the beaker since the reaction
sometimes becomes vigorous.
2. The reaction mixture should be stirred continuously.
Observation:
Weight of empty watch glass = W1 g
Result:
SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
| 48
Expt. No 12 Date
APPARATUS CHEMICALS
1. Volumetric flask
2. Stoppered bottles 1. 0.25M Acetic acid
3. 50ml Burette, 2. 0.1M NaOH solution
4. 100ml Beaker, 3. Phenolphthalein indicator
5. Water bath 4. Distilled water
6. 20ml Pipette 5. Activated charcoal
7. Conical flask
PROCEDURE
Step-1: preparation of standard NaOH:
Rinse the burette with NaOH solution; take NaOH solution into the burette.
Pipette out 10ml of CH3COOH into a conical flask, add 2-3 drops of phenolphthalein
indicator and 20ml distilled water.
Titrate the colorless solution with NaOH till pale pink color is obtained as end point.
Repeat the titration to get concurrent values.
OBSERVATIONS:
CALCULATIONS:
M1V1 M2V2
By volumetric principle = ; n1=1; n2=1
𝑛1 n2
Step-3:
Take well cleaned and dried 6 stoppered reagent bottles and label them
With help of two burettes transfer the acetic acid and distilled water into these bottles as
shown below.
Bottle No 1 2 3 4 5 6
Acetic acid 50 40 30 20 10 0
Distilled water 50 60 70 80 90 100
Initial 50 40 30 20 10
concentration × 𝑀2 × 𝑀2 × 𝑀2 × 𝑀2 × 𝑀2
100 100 100 100 100
of acetic acid zero
(C1) a= b= c= d= e=
Mix the solution well and keep all the six bottles in a water bath for some time to aquire the
temperature of the water bath.
Weigh exactly 2 gms of activated charcoal and add the same to each bottle.
Shake the bottle well and keep in the water bath for 1 hour while shaking the bottles from
time to time.
Filter contents of all the six bottles into six different labelled, dried conical flasks.
Titrate the six samples with 0.1M NaOH taken in the burette using phenolphthalein indicator
till pale pink coloured end point is obtained.
Let the titre values be V3,V4,V5,V6,V7,V8 respectively for bottle numbers 1,2,3,4,5,6.
Take 20ml of the stock solution into a clean 250ml conical flask add 2drops of
phenolphthalein indicator and titrate against 0.1M NaOH till pale pink coloured end point is
obtained.
Repeat the titration to get concurrent values.
Let the titre value be x ml.
| 50
Calculations:
M1V1 M2V2
= n2 ;
𝑛1
V1×M1×n2
M2 = =
n1×V2
Bottle No-1 Bottle No-2 Bottle No-3 Bottle No-4 Bottle No-5 Bottle No-6
M Acetic acid M Acetic acid M Acetic acid M Acetic acid M Acetic acid Zero
𝑀(𝑁𝑎𝑂𝐻)×𝑉3 𝑀(𝑁𝑎𝑂𝐻)×𝑉4 𝑀(𝑁𝑎𝑂𝐻)×𝑉5 𝑀(𝑁𝑎𝑂𝐻)×𝑉6 𝑀(𝑁𝑎𝑂𝐻)×𝑉7
= = = = =
50 50 50 50 50
=p =q =r =s =t
(𝐶1−𝐶2)×60×100 (𝐶1−𝐶2)×60
Amount of Acetic acid absorbed (X) = =
1000 10
Where C1=Initial concentration
C2= concentration after adsorption
Amount of the adsorbent (acetic acid) m = 2 gms
Initial concentration of six bottles (c) = a,b,c,d,e,f respectively
Bottle Initial concentration Amount of acetic acid X/m Log (X/m) Log c
No conc. C1 after absorbed
(𝐶1−𝐶2)×60
=X
adsorption C2 10
1 a= p= (𝑎 − 𝑝) × 60
=
10
2 b= q= (𝑏 − 𝑞) × 60
=
10
3 c= r= (𝑐 − 𝑟) × 60
=
10
4 d= s= (𝑑 − 𝑠) × 60
=
10
5 e= t= (𝑒 − 𝑡) × 60
=
10
Plotting graphs:
Log C
Langmuir adsorption isotherm:
The Langmuir adsorption isotherm is, c/(X/m) = 1/(k1k2) + c/k2
A graph may be plotted between c/(X/m) and c. A straight line indicates the validity of
Langmuir adsorption isotherm. k1 and k2 are obtained from the graphs as; Slope = 1/k1 and
intercept = 1/(k1k2).
RESULT:
The adsorption of acetic acid on activated charcoal is studied and the constants of the equations of
Langmuir and Freundlich isotherms are estimated and are:
SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
| 53
Annexure-1
1. 0.1N standard sodium carbonate: Dissolve exactly 5.3 grams of sodium carbonate in 1000
ml of distilled water in a standard volumetric flask (Eq.wt 53)
2. 0.1N standard potassium permanganate: Dissolve exactly 1.6 grams of potassium
permanganate 500 ml of distilled water in a standard volumetric flask (Eq.wt 158 )
3. 0.1N standard oxalic acid: Dissolve exactly 0.63 grams of oxalic acid in 100 ml of distilled
water in a standard volumetric flask. (Eq.wt 63)
4. 0.1 N standard potassium dichromate: Dissolve 0.49 grams of potassium dichromate in
100 ml of distilled water in a standard volumetric flask. (Mol.wt 294.18)
5. 0.1 N Hypo solution: Dissolve 12.4 gms of hypo into 1000ml of distilled water.
| 55
6. Preparation of KI: Dissolve 20 gms of KI in 100ml of water and stir well.
7. Preparation of dil.CH3COOH (2N): Dissolve 11.6 ml of glacial acetic acid in 100ml of
distilled water.
8. 0.01M EDTA: Dissolve 3.72 grams of EDTA in 1000 ml of distilled water in a standard
volumetric flask. (Mol.wt 372.24)
9. 0.01M Magnesium sulphateheptahydrate:Dissolve exactly 0.246 grams of magnesium
sulphatehepta hydrate in 100 ml of distilled water in a standard volumetric flask (Mol.wt 246)
10. 0.1M standard zinc sulphate solution: Dissolve exactly 2.87 grams of zinc sulphate in 100
ml of distilled water in a standard volumetric flask (Mol.wt 287)
11. 0.1 N sodium hydroxide:Dissolve approximately 0.4 grams of sodium hydroxide 100 ml of
distilled water in a standard volumetric flask (Mol.wt 40)
12. 0.1 N HCl : Use 8.6 ml of 11.6 M/N acid (36% HCI) in 1000ml (9.9 mL of acid in 1000mL
if 37% HCl)
13. Ammonium hydroxide (0.1 M, 0.1 N): Dilute 6.75 ml of concentrated solution (14.8 M,
28% NH3) to 1 liter.
14. Ammonium buffer of PH-10: dissolve 67.5 grams of ammonium chloride in 570ml of
ammonia solution and then make upto 1000ml
15. Methyl orange indicator. Dissolve 1 g of methyl orange in 1 liter of water. Filter, if
necessary.
16. Methyl red indicator. Dissolve 1 g of methyl red in 600 ml of alcohol and dilute with 400
ml of water.
17. Phenolphthalein. Dissolve 1 g of phenolphthalein in 50 ml of alcohol and add 50 ml of
water.
18. Diphenylamine: Dissolve 1 g in 100 ml of concentrated sulfuric acid.
19. EBT indicator: dissolve 0.5 grams of EBT in 100ml of alcohol
20. Fast Sulphone Black F: The indicator solution is 0.5% solution in water (or) dissolve 1 gm
of fast sulphone black-F indicator in 100ml of alcohol
21. 1% starch solution: In a 250ml beaker, place 100ml of distilled water and then add 1 grams
of starch. Heat the contents for about 10-15 min.
22. Murexide: This is the Ammonium salt of purpuric acid. Suspend 0.5g of the powdered
dyestuff in water, shake thoroughly and allow to settle. The saturated supernatant is used as
the indicator.
23. Preparation of acid mixture: Mix up 100 ml of phosphoric with 300ml of concentrated
H2SO4 in a reagent bottle and stopper it.
24. Conductivity standard (0.01N): dissolve 0.7459 g KCl in 1000ml. its conductivity at 25 OC
is 1413 microsemen/cm.
25. pH standard: 1. dissolve 10.12 g potassium hydrogrnphthalate in 1000ml distilled and its pH
is 4.004.
2. Dissolve 2.0992 g sodium bicarbonate in 1000ml distilled water (or) Dissolve 2.64 g
sodium carbonate in 1000ml distilled water (pH =10.014)
𝒘×𝒅×𝟏𝟎
26. Molarity =
𝒈𝒎𝒘
27. Molarity of Concentrated Acids & Bases
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