Chemistry Lab R23 Manual NRI

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NRI INSTITUTE OF TECHNOLOGY

(AUTONOMOUS)
Approved by AICTE, New Delhi: Permanently Affiliated to JNTUK, Kakinada
Accredited by NAAC with "A" GRADE, Accredited by NBA (CSE, ECE&EEE)
An ISO 9001:2015 Certified Institution
Pothavarappadu (V), Agiripalli (M), Eluru District, A.P., India, Pin: 521 212
URL: www.nriit.edu.in, email: principal@nriit.edu.in, Mobile: + 91 8333882444

NRIA23

CHEMISTRY

LAB MANUAL
NRIA23 Chemistry Lab Manual

NRI Institute of Technology (Autonomous)


Freshman Engineering Department
Academic year 2023-24
As Per NRIA23 Regulations
Common to (CSE, CSE -R, CSM, CSD, IT, AIML, ECE, EEE)
Subject: Chemistry Lab

Labs / Instructions
3 Internal Marks: 30
Hours/Week
Credits: 1 External Marks: 70
Prerequisites: Knowledge on Volumetric analysis.
Course Objectives:
 To make the students to analyze the different parameters of water sample like
hardness and alkalinity and different volumetric titrations.
 To make the students to acquire the basic knowledge of instrumentation based on
different Engineering applications.
Course Outcomes: At the end of the course, the students will be able to

CO1 Carry out the acid -base titration by volumetric analysis.


CO2 Determine the cell constant and conductance of solutions.
CO3 Prepare polymer material.
CO4 Do the redox titration by classical and instrumental methods.
CO5 Analyse organic and inorganic compounds by advance techniques.

Contribution of Course Outcomes towards achievement of Program Outcomes (1 –


Low, 2- Medium, 3 – High)

PO PO PO PO PO PO PO PO PO PO PO PO
1 2 3 4 5 6 7 8 9 10 11 12
CO1 2 1 1
CO2 2 1 1
CO3 2 1 1
CO4 2 1 1
CO5 2 1 1

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NRIA23 Chemistry Lab Manual

Chemistry Lab
Common to (CSE, CSE -R, CSM, CSD, IT, AIML, ECE, EEE)
Regulation: R23 Academic Year: 2023-24

List of Experiments as per Syllabus


1. Measurement of 10Dq by spectrophotometric method.
2. Conductometric titration of strong acid vs. strong base
3. Conductometric titration of weak acid vs. strong base
4. Determination of cell constant and conductance of solutions
5. Potentiometry - determination of redox potentials and emfs
6. Determination of Strength of an acid in Pb-Acid battery
7. Preparation of a Bakelite
8. Verify Lambert-Beer’s law
9. Wavelength measurement of sample through UV-Visible Spectroscopy
10. Identification of simple organic compounds by IR
11. Preparation of nanomaterials by precipitation method
12. Estimation of Ferrous Iron by Dichrometry
13. Determination of HCl using standard Na2CO3 solution.
14. Determination of KMnO4 using standard Oxalic acid solution.
15. Determination of total hardness of water using standard EDTA solution.
16. Determination of Copper using standard EDTA solution.
17. Determination of total alkalinity of given water sample
18. Estimation of vitamin C.

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NRIA23 Chemistry Lab Manual

Chemistry Lab
Common to (CSE, CSE -R, CSM, CSD, IT, AIML, ECE, EEE)
Regulation: R23 Academic Year: 2023-24

List of Experiments to be done


1. Determination of Strength of an acid in Pb-Acid battery.
2. Determination of total alkalinity of given water sample.
3. Estimation of Ferrous Iron by Dichrometry.
4. Determination of KMnO4 using standard Oxalic acid solution.
5. Determination of total hardness of water using standard EDTA solution.
6. Determination of Copper using standard EDTA solution.
7. Preparation of a Bakelite.
8. Verify Lambert-Beer’s law.
9. Conductometric titration of strong acid vs. strong base.
10. Potentiometry - determination of redox potentials and emfs.

Distribution and weightage of marks for Chemistry Practical:


The assessment of a student’s performance shall be evaluated as suggested below:
For practical subject there shall be continuous evaluation during the semester for 30 Internal
Marks and 70 Marks for End Semester Examination.
1) Out of 30 Internal Marks,
Day to Day Assessment – 10 M
Record –5M
Internal Exam – 15M
2) Out of 70 External Marks,
Procedure – 20 M
Experimental work – 20 M
Result – 10 M
Viva Voce – 20 M

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NRIA23 Chemistry Lab Manual

INTRODUCTION TO CHEMISTRY LABORATORY

Chemical analysis includes both qualitative and quantitative analysis.

 Quantitative analysis is carried out by conventional methods as well as modern


instrumental methods.
 The conventional methods include Volumetric analysis, Gravimetric analysis, etc.
 The modern methods involve use of electronic instruments like pH-meter,
conductometer, colorimeter, spectrophotometer, polarograph, chromatograph, etc.
among others.
Solution:
 It is a homogeneous mixture of two or more components.
 The solution, which contains two components is known as Binary solution.
 The two components are Solute & Solvent.
 Solute: In a solution, the substance present in relatively low quantity is called a solute.
 Solvent: In a solution, the substance present in relatively high quantity is called a
solvent.
Concentration:
 The relative amounts of solute and solvent present in a solution is also called
concentration of the solution.
 Concentration can be expressed in terms of
1. Molarity
2. Molality
3. Normality
4. Mole Fraction

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NRIA23 Chemistry Lab Manual

Molarity (M):
 It is the number of moles of solute present in one liter of solution.
 Molarity= No. of moles/volume of the solution in liters.

Molality (m):
 It is the number of moles of solute present in one Kg of solvent.
 Molality= No. of moles/weight of the solvent in Kg.

Normality (N):
 It is the number of gram equivalents of the solute present in one liter of the solution.

Mole Fraction (X):


 The ratio of number of moles of one component to total number of moles of components
in a solution is called mole fraction.

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NRIA23 Chemistry Lab Manual

Standard Solution:
 It is the solution whose concentration is exactly known.
Standardizations:
 Determination of the concentration of a solution by any suitable analytical method is
known as standardization.
Primary standard solution:
 If the concentration of a solution is known by dissolving a known mass of the desired
substance into a known volume of solvent, then the solution is called a primary standard
solution.
Secondary standard solution:
 If the concentration of a solution is determined by using a suitable primary standard
solution, then the solution is called secondary standard solution.

VOLUMETRIC ANALYSIS
 Volumetric analysis is a widely used quantitative analytical method.
 A Chemical procedure used for determining the concentration of a solution.
 A known volume of a solution of a unknown concentration is reacted with a known volume
of a solution of known concentration (standard).
 Titration: It is a technique where a solution of known concentration is used to determine
the concentration of an unknown solution.
 Titrant: It is the solution of known concentration that is delivered by a burette.
 Titrand or Analyte: It is the substance whose concentration is to be determined by
titration.
 Indicator: The completion of the titration is detected by the addition of an auxiliary reagent,
known as an indicator.
 End point: The end point is the point at which the titration is complete, as determined by
an indicator.

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NRIA23 Chemistry Lab Manual

 Equivalence point: It is the point at which the reaction between the titrant and analyte
completes. It is the theoretical end point.

TYPES OF TITRATIONS

Acid-Base Titrations:
 Acid is the substance which donates H+ ion.
 Base is the substance which accepts H+ ion.
 Strong electrolyte is the substance which dissociates completely.
 Weak electrolyte is the substance which dissociates partially.
 Acid Base Titrations are also known as Neutralization titrations.
 There are four types of Acid- Base Titrations.
 Strong Acid with Strong Base
 Strong Acid with Weak Base
 Weak Acid with Strong Base
 Weak Acid with Weak Base

Redox Titrations:
 The titrations which involve simultaneous oxidation and reduction are called redox
titrations.
 The phenomenon of loss of electrons (or) removal of hydrogens (or) addition of
oxygens is called oxidation.
 The phenomenon of gain of electrons (or) removal of oxygens (or) addition of
hydrogens is called reduction.
 The substance which undergoes reduction is called oxidizing agent.
 The substance which undergoes oxidation is called reducing agent.
 Redox titrations involving KMnO4 as the oxidizing agent are called
Permanganometry.

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NRIA23 Chemistry Lab Manual

 Redox titrations involving K2Cr2 O7 as the oxidizing agent are called Dichrometry.
 Redox titrations involving Iodine solution as the oxidizing agent are called Iodine
Titrations.

Complexometric Titrations:
 Titrations depending upon the combination of ions, other than H+ or OH- ions, to form
a soluble complex compound are called complexometric titrations.
 A commonly used complexing agent is EDTA.

Precipitation Titrations:
 It is based on the formation of a product which is insoluble in solvent and forms
precipitate, by the reaction between the analyte and the titrant.
 A classic example is the reaction between Ag+ and Cl- to form the very insoluble salt
AgCl.

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NRIA23 Chemistry Lab Manual

DETERMINATION OF STRENGTH OF AN ACID IN LEAD-ACID BATTERY

Aim: To determine the strength of acid in Lead-Acid battery using standard NaOH solution.

Apparatus Required: Burette, Conical flask, Beaker, Burette stand, Pipette, Wash bottles and
Volumetric flask.

Chemicals Required: Acid from Lead acid battery, NaOH, Standard Oxalic acid,
Phenolphthalein indicator.

Principle:
Strength of acid in Lead-Acid battery is the measure of its ability to neutralize with bases to
resist change of pH value of acid due to presence of mineral acids like H2SO4.

Chemical Equations:
(𝐶𝑂𝑂𝐻)2 + 2𝑁𝑎𝑂𝐻 → (𝐶𝑂𝑂𝑁𝑎)2 + 𝐻2 𝑂
𝐻2 𝑆𝑂4 + 2𝑁𝑎𝑂𝐻 → 𝑁𝑎2 𝑆𝑂4 + 𝐻2 𝑂

Procedure:

Step-I: Standardization of Sodium Hydroxide:


Take 10 ml of Standard Oxalic Acid solution into the conical flask and add 1 or 2 drops of
Phenolphthalein indicator. The Burette is filled with Sodium Hydroxide solution and the
contents in the conical flask are titrated against Sodium Hydroxide solution till the colour
changes to pale pink. The titration is repeated until the concurrent reading are obtained.

Step-II: Determination of Strength of an acid:


Take 10 ml of Acid solution (from battery) into the conical flask and add 1 or 2 drops of
Phenolphthalein indicator. The Burette is filled with Sodium Hydroxide solution and the
contents in the conical flask are titrated against Sodium Hydroxide solution till the colour
changes to pale pink. The titration is repeated until the concurrent reading are obtained.

Step -I : Standardization of Sodium Hydroxide:

Volume of Oxalic Burette reading (ml) Volume of NaOH Solution run


S.No.
Acid solution (ml) Initial Final down (ml)

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NRIA23 Chemistry Lab Manual

Formula:
𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2
Where
M1 = Molarity of Oxalic acid solution = 0.15 M

V1 = Volume of Oxalic acid solution = 10ml

n1 = No. of moles of Oxalic acid solution taken part in the reaction = 1

M2 = Molarity of NaOH solution = ?

V2 = Volume of NaOH solution = (Burette reading) =

n2= No. of moles of NaOH solution taken part in the reaction = 2

𝑀1 𝑉1 𝑛2
𝑀2 = ×
𝑛1 𝑉2
=
=

Step -II: Determination of strength of an acid:

Volume of Acid Burette reading (ml) Volume of NaOH Solution run


S.No.
solution (ml) Initial Final down (ml)

Formula:
𝑀2 𝑉2 𝑀3 𝑉3
=
𝑛2 𝑛3

Where
M2 = Molarity of NaOH solution =

V2 = Volume of NaOH solution = (Burette reading) =

n2= No. of moles of NaOH solution taken part in the reaction = 2

M3 = Molarity of Acid solution =?

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NRIA23 Chemistry Lab Manual

V3 = Volume of Acid solution = 10ml

n3 = No. of moles of Acid solution taken part in the reaction = 1


𝑀2 𝑉2 𝑛3
𝑀3 = ×
𝑛2 𝑉3
=
=
The strength of Sulphuric acid present in one litre of solution
= 𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 × 𝑀𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡
= 𝑀3 × 98
= 𝑔𝑚/𝑙

Result: The strength of acid present in the given sample solution is ---------g/L

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NRIA23 Chemistry Lab Manual

DETERMINATION OF TOTAL ALKALINITY OF WATER SAMPLE


(Acid – Base titration)
Aim: To determine the total alkalinity of water sample using standard HCl solution.
Apparatus Required: Burette, Conical flask, Beaker, Burette stand, Pipette, Wash bottles and
Volumetric flask.

Chemicals Required: Standard Na2CO3 solution, HCl solution, water sample, methyl orange
indicator and phenolphthalein indicator.
Principle:
Alkalinity may be defined as the power of a solution to neutralize hydrogen ions. It is due to
the presence of salts of weak acids – carbonates, bicarbonates, hydroxides etc. But usually,
alkalinity is expressed in terms of carbonates, bicarbonates and hydroxides and is reported in
terms of calcium carbonate equivalents.
Chemical equations:
𝑁𝑎2 𝐶𝑂3 + 2𝐻𝐶𝑙 → 2𝑁𝑎𝐶𝑙 + 𝐻2 𝐶𝑂3

H   CO32  HCO3

H   OH   H 2 O

HCO3  H   CO2  H 2 O

Procedure:
Step-I: Standardization of HCl:
Take 10 ml of Standard sodium carbonate solution into the conical flask and add 1 or 2 drops
of methyl orange indicator, then the solution turns to pale yellow. The Burette is filled with
HCl solution and the contents in the conical flask are titrated against HCl solution till the colour
changes from pale yellow to pale pink. The titration is repeated until the concurrent reading are
obtained.

Step -II: Determination of alkalinity:


Take 10 ml of water sample into the conical flask and add 1 or 2 drops of methyl orange
indicator, then the solution turns to pale yellow. The Burette is filled with HCl solution and the
contents in the conical flask are titrated against HCl solution till the colour changes from pale
yellow to pale pink. The titration is repeated until the concurrent reading are obtained.

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NRIA23 Chemistry Lab Manual

Observations and calculations:


Step -I : Standardization of HCl solution:

Volume of Sodium Burette reading (ml)


Volume of HCl Solution run
S.No. carbonate solution
Initial Final down (ml)
(ml)

Formula:
𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2
Where
M1 = Molarity of Sodium carbonate solution = 0.05 M

V1 = Volume of Sodium carbonate solution = 10ml

n1 = No. of moles of Sodium carbonate solution taken part in the reaction = 1

M2 = Molarity of HCl solution = ?

V2 = Volume of HCl solution = (Burette reading) =

n2= No. of moles of HCl solution taken part in the reaction = 2

𝑀1 𝑉1 𝑛2
𝑀2 = ×
𝑛1 𝑉2
=
=

Step -II : Determination of Total Alkalinity:

Volume of water Burette reading (ml) Volume of HCl Solution run


S.No.
sample (ml) Initial Final down (‘v’ ml)

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NRIA23 Chemistry Lab Manual

Total alkalinity in terms of CaCO3


𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐻𝐶𝑙 × 𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑜𝑓 𝐻𝐶𝑙 × 50 × 1000
= 𝑝𝑝𝑚
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 𝑠𝑎𝑚𝑝𝑙𝑒
𝑣 × 𝑀2 × 50 × 1000
= 𝑝𝑝𝑚
10
Result:
Total alkalinity of water sample in terms of CaCO3 is --------------- ppm

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NRIA23 Chemistry Lab Manual

DETERMINATION OF FERROUS ION USING STANDARD K2Cr2O7 SOLUTION


(Redox Titration)

Aim: To estimate the amount of Ferrous ion present in the given solution using potassium
dichromate.

Apparatus Required: Burette, Conical flask, Beaker, Burette stand, Pipette, Wash bottles and
Volumetric flask.

Chemicals Required: Potassium dichromate solution, Ferrous ion solution, 10% sulphuric
acid and diphenylamine indicator.

Principle:
Dichrometry titrations are based on oxidation reactions by dichromate ion. Its oxidizing
action is due to conversion of Cr2O7- ions (containing Cr6+) into Cr3+ ions. Potassium
dichromate acts as an oxidizing agent in the presence of sulphuric acid. It oxidizes Fe2+ ion and
itself is reduced to green chromic salt.
To detect the end point, diphenylamine is used as indicator in the titration. Indicator used in
oxidation – reduction titrations are known as oxidation – reduction or Redox indicators. Redox
indicators change color when the oxidation potential of titrated solution reaches a define value.
These indicators can be reversibly oxidized or reduced with different color in the oxidized and
reduced forms. Diphenylamine changes from colourless to blue – violet between 0.73V and
0.79V. Effective potential range of Redox indicator must be within the limits of the sharp
change of potential near the equivalence point.

Chemical Equation:

6𝐹𝑒𝑆𝑂4 + 𝐾2 𝐶𝑟2 𝑂7 + 7𝐻2 𝑆𝑂4 → 3𝐹𝑒2 (𝑆𝑂4 )3 + 𝐶𝑟2 (𝑆𝑂4 )3 + 𝐾2 𝑆𝑂4 + 7𝐻2 𝑂

Procedure:
Estimation of Ferrous Ion:
Pipette out 10ml of Ferrous ion solution into a conical flask and add 5ml of 10% H2SO4
and 1 or 2 drops of diphenylamine indicator. The burette is filled with Potassium dichromate
solution and the contents in the conical flask are titrated against potassium dichromate solution
till the colour changes from green to bluish violet. The titration is repeated until the concurrent
reading are obtained.

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NRIA23 Chemistry Lab Manual

Observations and Calculations:

Estimation of Ferrous Ion:

Volume of Ferrous Burette reading (ml) Volume of K2Cr2 O7 Solution


S.No.
ion solution (ml) Initial Final run down (ml)

Formula:
𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2

Where
M1 = Molarity of potassium dichromate solution = 0.01M

V1 = Volume of potassium dichromate solution (Burette reading) =

n1 = No. of moles of potassium dichromate solution =1

M2 = Molarity of ferrous ion solution = ?

V2 = Volume of ferrous ion solution = 10 ml

n2 = No. of moles of ferrous ion solution = 6

𝑀1 𝑉1 𝑛2
𝑀2 = ×
𝑛1 𝑉2

Amount of ferrous ion present in one litre of solution


= 𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 × 𝐴𝑡𝑜𝑚𝑖𝑐 𝑤𝑒𝑖𝑔ℎ𝑡
= 𝑀2 × 56
= 𝑔𝑚/𝑙
Result:

The amount of ferrous ion present in the given solution is____________ g/L

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NRIA23 Chemistry Lab Manual

DETERMINATION OF KMnO4 USING STANDARD OXALIC ACID SOLUTION


(Redox Titration)

Aim: To estimate the amount of Potassium permanganate present in the given solution using
standard oxalic acid.

Apparatus Required: Burette, Conical flask, Beaker, Burette stand, Pipette, Wash bottles and
Volumetric flask.

Chemicals Required: Oxalic acid solution, Potassium permanganate solution and 10%
sulphuric acid solution.

Principle:
Potassium permanganate is an oxidizing agent in the presence of dilute sulphuric acid.
Potassium permanganate oxidizes oxalic acid to carbon dioxide and water.
The following reaction takes place:
2KMnO4+3H2SO4 →K2SO4+2MnSO4+ 3 H2O+ 5 (O)
5H2C2O4+ 5 (O) → 5 H2O+10CO2
2KMnO4+3H2SO4+5H2C2O4→ K2SO4+2MnSO4+8H2O+10CO2
Here KMnO4 acts as self-indicator. If the reagent is strongly coloured and is discoloured or
changed to different colour during titration, it is called as a self- indicator.

Chemical Equations:

5𝐻2 𝐶2 𝑂4 + 2𝐾𝑀𝑛𝑂4 + 3𝐻2 𝑆𝑂4 → 𝐾2 𝑆𝑂4 + 2𝑀𝑛𝑆𝑂4 + 8𝐻2 𝑂 + 10𝐶𝑂2

Procedure:
Estimation of potassium permanganate solution:
Pipette out 10ml of Standard oxalic acid solution into a conical flask and add 5ml of 10%
H2SO4 and heat the solution to about 70Oc. The burette is filled with Potassium Permanganate
solution and the contents in the conical flask are titrated against Potassium Permanganate
solution till the colour changes to pale pink. The titration is repeated until the concurrent
reading are obtained.

Observations and Calculations:

Estimation of Potassium Permanganate:

Volume of Oxalic Burette reading (ml) Volume of KMnO4Solution run


S.No.
acid solution (ml) Initial Final down (ml)

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NRIA23 Chemistry Lab Manual

Formula:
𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2

Where
M1 = Molarity of Oxalic acid solution = 0.05M

V1 = Volume of Oxalic acid solution = 10 ml

n1 = No. of moles of Oxalic acid solution =5

M2 = Molarity of Potassium Permanganate solution = ?

V2 = Volume of Potassium Permanganate solution (Burette reading) =

n2 = No. of moles of Potassium Permanganate solution = 2

𝑀1 𝑉1 𝑛2
𝑀2 = ×
𝑛1 𝑉2

Amount of Potassium Permanganate present in one litre of solution


= 𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 × 𝑀𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡
= 𝑀2 × 158
= 𝑔𝑚/𝑙

Result:

The Amount of Potassium Permanganate present in the given solution is ____________ g/L

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NRIA23 Chemistry Lab Manual

DETERMINATION OF TOTAL HARDNESS OF WATER SAMPLE


(EDTA method)

Aim: To determine the total hardness of the given water sample using standard EDTA solution.

Apparatus Required: Burette, Conical flask, Beaker, Burette stand, Pipette, Wash bottles and
Volumetric flask.

Chemicals Required: Standard zinc salt solution, EDTA solution, Water sample, Eriochrome
black- T indicator and ammonia – ammonium chloride buffer solution (pH = 10).

Principle:
Ethylene diamine tetra acetic acid (EDTA) forms colourless, stable complexes with Ca2+ and
Mg2+ ions present in water at pH 9-10. To maintain the pH of the solution at 9-10, NH4Cl-
NH4OH buffer is used. Eriochrome black-T (EBT) is used as an indicator. The sample of hard
water must be treated with buffer solution and EBT indicator, which forms unstable, wine-red
coloured complexes with Ca2+ and Mg2+ present in water. The stability of a metal indicator
complex is less than that of metal EDTA complex. During the titration, the wine-red coloured
complex reacts with EDTA, when free metal ions are not available. EDTA extracts the metal
ions from the metal ion-EBT complex and forms stable, colourless complexes by releasing the
free indicator. At the end point of the titration is the colour change from wine red to blue.

Chemical equations:
𝑀𝑛+ + 𝐼𝑛𝑑𝑖𝑐𝑎𝑡𝑜𝑟 → [𝑀𝑒𝑡𝑎𝑙 − 𝐼𝑛𝑑𝑖𝑐𝑎𝑡𝑜𝑟]
(Less stable and wine-red color)

[𝑀𝑒𝑡𝑎𝑙 − 𝐼𝑛𝑑𝑖𝑐𝑎𝑡𝑜𝑟] + 𝐸𝐷𝑇𝐴 → [𝑀𝑒𝑡𝑎𝑙 − 𝐸𝐷𝑇𝐴] + 𝐼𝑛𝑑𝑖𝑐𝑎𝑡𝑜𝑟


(Wine red) (Stable and colourless) (Blue)

Procedure:
Step-1: Standardization of EDTA solution:
Pipette out 10ml of Standard Zinc sulphate solution into a conical flask and add 2-3ml of buffer
solution and add 2-3 drops of EBT indicator. Then the solution changes to wine red colour.
The burette is filled with EDTA solution and the contents in the conical flask are titrated against
EDTA solution till the colour changes from wine red to blue. The titration is repeated until the
concurrent reading are obtained.

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NRIA23 Chemistry Lab Manual

Step -2: Determination of Total Hardness of water:


Pipette out 10ml of water sample into a conical flask and add 2-3ml of buffer solution and add
2-3 drops of EBT indicator. Then the solution changes to wine red colour. The burette is filled
with EDTA solution and the contents in the conical flask are titrated against EDTA solution till
the colour changes from wine red to blue. The titration is repeated until the concurrent reading
are obtained.

Observations & Calculations:

Step -I: Standardization of EDTA:

Volume of Zinc Burette reading (ml)


Volume of EDTA Solution run
S.No. sulphate solution
Initial Final down (ml)
(ml)

Formula:
𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2

Where
M1 = Molarity of Zinc sulphate solution = 0.01M

V1 = Volume of Zinc sulphate solution = 10 ml

n1 = No. of moles of Zinc sulphate solution =1

M2 = Molarity of EDTA solution = ?

V2 = Volume of EDTA solution (Burette reading) =

n2 = No. of moles of EDTA solution = 1

𝑀1 𝑉1 𝑛2
𝑀2 = ×
𝑛1 𝑉2
=

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NRIA23 Chemistry Lab Manual

Step -II: Determination of total hardness of water sample:

Volume of water Burette reading (ml) Volume of EDTA Solution run


S.No.
sample (ml) Initial Final down (ml)

Formula:
𝑀2 𝑉2 𝑀3 𝑉3
=
𝑛2 𝑛3

Where

M2 = Molarity of EDTA solution =

V2 = Volume of EDTA solution (Burette reading) =

n2 = No. of moles of EDTA solution = 1

M3 = Molarity of Hard water =?

V3 = Volume of Hard water = 10 ml

n3 = No. of moles of Hard water = 1

𝑀2 𝑉2 𝑛3
𝑀3 = ×
𝑛2 𝑉3
=
=
The total hardness of water sample in terms of CaCO3 is
= 𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 × 100 × 1000
= 𝑀3 × 100 × 1000
= 𝑚𝑔/𝑙

(or)
Formula:
Total hardness of water sample
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐸𝐷𝑇𝐴 × 𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑜𝑓 𝐸𝐷𝑇𝐴 × 100 × 1000
= 𝑝𝑝𝑚 𝑜𝑓 𝐶𝑎𝐶𝑂3
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 𝑠𝑎𝑚𝑝𝑙𝑒

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NRIA23 Chemistry Lab Manual

𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐸𝐷𝑇𝐴 × 𝑀2 × 100 × 1000


= 𝑝𝑝𝑚 𝑜𝑓 𝐶𝑎𝐶𝑂3
10
Result:

The total hardness of water sample is ____________ ppm of CaCO3

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NRIA23 Chemistry Lab Manual

DETERMINATION OF COPPER BY EDTA METHOD


(Complexometric titration)

Aim: To determine the amount of copper present in the given solution using standard EDTA
solution.

Apparatus Required: Burette, Conical flask, Beaker, Burette stand, Pipette, Wash bottles and
Volumetric flask.

Chemicals Required: Standard zinc salt solution, EDTA solution, Copper sulphate,
Eriochrome black- T indicator, Fast sulphone black – F (FSB) indicator and ammonia –
ammonium chloride buffer solution (pH = 10).

Principle:
Ethylene diamine tetra acetic acid (EDTA) forms colourless, stable complexes
with Ca and Mg2+ ions present in water at pH 9-10. To maintain the pH of the solution at 9-
2+

10, NH4Cl-NH4OH buffer is used. Fast sulphone Black-F indicator is specific in its reaction
with copper in ammonia solution and it forms blue coloured complex with copper. In the
titration of copper in ammonical solution the colour changes from blue to dark green at the end
point.

Chemical equations:
𝐶𝑢2+ + 𝐼𝑛𝑑𝑖𝑐𝑎𝑡𝑜𝑟 → [𝐶𝑢 − 𝐼𝑛𝑑𝑖𝑐𝑎𝑡𝑜𝑟]
(Less stable and Blue color)

[𝐶𝑢 − 𝐼𝑛𝑑𝑖𝑐𝑎𝑡𝑜𝑟] + 𝐸𝐷𝑇𝐴 → [𝐶𝑢 − 𝐸𝐷𝑇𝐴] + 𝐼𝑛𝑑𝑖𝑐𝑎𝑡𝑜𝑟


(Blue) (Stable and colorless) (Dark green)

Procedure:
Step-1: Standardization of EDTA solution:
Pipette out 10ml of Standard Zinc sulphate solution into a conical flask and add 2-3ml of buffer
solution and add 2-3 drops of EBT indicator. Then the solution changes to wine red colour.
The burette is filled with EDTA solution and the contents in the conical flask are titrated against
EDTA solution till the colour changes from wine red to blue. The titration is repeated until the
concurrent reading are obtained.

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NRIA23 Chemistry Lab Manual

Step t-2: Estimation of Copper:


Pipette out 10ml of Copper sulphate into a conical flask and add 2-3ml of buffer solution and
add 2-3 drops of FSB indicator. Then the solution changes to Blue colour. The burette is filled
with EDTA solution and the contents in the conical flask are titrated against EDTA solution till
the colour changes from Blue to dark Green. The titration is repeated until the concurrent
reading are obtained.

Observations & Calculations:

Step -I: Standardization of EDTA:

Volume of Zinc Burette reading (ml)


Volume of EDTA Solution run
S.No. sulphate solution
Initial Final down (ml)
(ml)

Formula:
𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2

Where
M1 = Molarity of Zinc sulphate solution = 0.01M

V1 = Volume of Zinc sulphate solution = 10 ml

n1 = No. of moles of Zinc sulphate solution =1

M2 = Molarity of EDTA solution = ?

V2 = Volume of EDTA solution (Burette reading) =

n2 = No. of moles of EDTA solution = 1

𝑀1 𝑉1 𝑛2
𝑀2 = ×
𝑛1 𝑉2
=

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NRIA23 Chemistry Lab Manual

Step -II: Estimation of Copper:

Volume of Copper Burette reading (ml) Volume of EDTA Solution run


S.No.
sulphate solution(ml) Initial Final down (ml)

Formula:
𝑀2 𝑉2 𝑀3 𝑉3
=
𝑛2 𝑛3

Where

M2 = Molarity of EDTA solution =

V2 = Volume of EDTA solution (Burette reading) =

n2 = No. of moles of EDTA solution = 1

M3 = Molarity of Copper sulphate solution =?

V3 = Volume of Copper sulphate solution = 10 ml

n3 = No. of moles of Copper sulphate solution =1

𝑀2 𝑉2 𝑛3
𝑀3 = ×
𝑛2 𝑉3
=
=
The amount of copper present in one litre of solution
= 𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 × 𝐴𝑡𝑜𝑚𝑖𝑐 𝑤𝑒𝑖𝑔ℎ𝑡
= 𝑀3 × 63.5
= 𝑔𝑚/𝑙

Result:

The amount of copper present in the given solution is ----------------- gm/l

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NRIA23 Chemistry Lab Manual

PREPARATION OF BAKELITE

Aim: To prepare Phenol- Formaldehyde resin.

Apparatus Required: Beakers, Glass rod, funnel, filter paper etc.

Chemicals Required: Glacial Acetic Acid, 40% Formaldehyde solution, Phenol, Concentrated
HCl solution.
Theory:
Phenol and formaldehyde undergo condensation polymerization to produce a
three-dimensional phenol- Formaldehyde resin. The products formed during the formation of
resin of mono methylol, di methylol and tri methylol phenol. Polymerization can take place
from mono, di or tri methylol phenol or possibly through all the three with the formation of
long chains. Thermosetting of the resin takes place during the moulding process. For moulding,
the methylol derivatives or compounded with fillers, plasticizers, pigments, etc. and then are
subjected to heat and pressure, resulting in a hard and infusible product.

Chemical Equations:
Step I:- Formation of ortho and para hydroxy benzyl alcohols from phenol and formaldehyde

Step II:- Formation of Novalac from ortho-hydroxy, benzyl alcohol

Step III:- Formation of Bakelite from Novalac.

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NRIA23 Chemistry Lab Manual

Procedure:
1. Place 5ml of glacial acetic acid and 2.5ml of 40% formaldehyde solution in a 500ml
beaker.
2. Add 2g of phenol to it.
3. Wrap a cloth loosely around the beaker. Add a few ml of conc. HCl into the mixture
carefully and heat it gently.
4. A large mass of plastic, pink in color is formed.
5. The residue is washed with water and filtered.
6. The product is dried.

Precautions:
1. Handle phenol carefully.
2. While adding conc. HCl, it is better to stay a little distance away from the beaker since
the reaction sometimes becomes vigorous.
3. The reaction mixture should be stirred continuously.

Result:
The phenol Formaldehyde resin was prepared.

NRI INSTITUTE OF TECHNOLOGY, POTHAVARAPPADU 28


NRIA23 Chemistry Lab Manual

VERIFY LAMBERT-BEER’S LAW


Aim: To verify Lambert – Beer’s law by using colorimeter.

Apparatus Required: Colorimeter, Cuvette, Beakers, Measuring Cylinders, Test tubes etc.

Chemicals Required: Potassium Permanganate (KMnO4), Distilled water.

Principle:
Lambert – Beer’s states that when a beam of monochromatic light is passed through a solution
of an absorbing substance, the rate of decrease of intensity of radiation is directly proportional
to the intensity of incident radiation as well as concentration of the solution.
(OR)
It states that the absorbance of light is directly proportional to the concentration of the sample
and path length.
𝐴 =∈ 𝐶 𝑙
Where, ‘A’ is the Absorbance or Optical Density
‘C’ is the concentration of the solution,
‘l’ is the path length,
‘ϵ’ is the molar absorption coefficient.
Colorimeter measures the absorbance or optical density of an absorbing substance.
𝐼0
Optical Density 𝑂𝐷 = 𝐴 = log 𝐼
Where, I0 is Intensity of incident light and
I is Intensity of transmitted light

Procedure:
 A standard solution of 0.005 M Potassium Permanganate is prepared and then select
the filter with maximum absorbance by using standard solution.
 Prepare the following five sample solutions in test tubes as
I. 2 ml of KMnO4 solution + 8 ml of Distilled water
II. 4 ml of KMnO4 solution + 6 ml of Distilled water
III. 6 ml of KMnO4 solution + 4 ml of Distilled water
IV. 8 ml of KMnO4 solution + 2 ml of Distilled water
V. 10 ml of KMnO4 solution + 0 ml of Distilled water
 Take the first sample solution (I) into the cuvette and measure the absorbance value.
 Repeat the same procedure with all the sample solutions (II, III, IV, V) and tabulate the
result.

Graph:
Plot a graph with concentration on X- axis and absorbance on Y-axis which gives a
straight line passing through origin.

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NRIA23 Chemistry Lab Manual

Observations & Calculations:


𝜆𝑀𝐴𝑋 =

S. No. Concentration Absorbance


1 0.001 M
2 0.002 M
3 0.003 M
4 0.004 M
5 0.005 M

Result:
Lambert – Beer’s Law is verified.

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NRIA23 Chemistry Lab Manual

CONDUCTOMETRIC TITRATION OF STRONG ACID Vs STRONG BASE

Aim: To determine the strength of HCl present in the given solution by using Conductometric
titration.

Apparatus Required: Conductometer, Conductivity cell, Beakers, Burette, Pipette,


Measuring cylinders, Volumetric flask etc.

Chemicals Required: HCl solution, NaOH solution, Distilled water.

Principle:
Conductance of any solution depends upon the number of ions and mobility of ions and it is
measured in ‘mho’. The conductance of strong acid like HCl is high due the fast-moving H+
ions. When a strong base like NaOH is added, the conductance of acid decreases due to the
formation of H2O. The conductance goes on decreasing till the equivalence point or
neutralization point is reached. After equivalence point, by the addition of base the conductance
increases due to increase in OH- ions concentration.

Chemical Equations:
𝐻𝐶𝑙 + 𝑁𝑎𝑂𝐻 → 𝑁𝑎𝐶𝑙 + 𝐻2 𝑂
Procedure:
Estimation of HCl by using Conductometer:
 The Conductometer is calibrated and kept ready along with the conductivity cell.
 Burette is filled with NaOH solution.
 10ml of HCl is pipetted out into a beaker and add 100ml of distilled water and the
conductance is measured.
 1ml of NaOH is added to HCl solution through the burette. The solution is mixed, and
conductivity is measured.
 This procedure is repeated for every addition of 1ml of NaOH and the values are
tabulated.

Graph:
A graph is plotted between volume of NaOH added on X axis and conductance on Y axis. From
the graph the volume of NaOH at equivalence point is noted.

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NRIA23 Chemistry Lab Manual

Observations and calculations:

Estimation of HCl by using Conductometer:

S.No. Volume of NaOH Added(ml) Conductance (mS)

Formula:
𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2

Where
M1 = Molarity of NaOH solution = 0.1 M

V1 = Volume of NaOH solution = (From Graph) =

n1 = No. of moles of NaOH solution taken part in the reaction = 1

M2 = Molarity of HCl solution = ?

V2 = Volume of HCl solution = 10 ml

n2= No. of moles of HCl solution taken part in the reaction = 1

𝑀1 𝑉1 𝑛2
𝑀2 = ×
𝑛1 𝑉2
=
=

The strength of HCl present in one litre of the solution =

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NRIA23 Chemistry Lab Manual

= 𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 × 𝑀𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡


= 𝑀2 × 36.5
= 𝑔𝑚/𝑙

Result:
The Strength of HCl present in the given solution is ____________ gm/l

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NRIA23 Chemistry Lab Manual

POTENTIOMETRY - DETERMINATION OF REDOX POTENTIALS AND EMFS

Aim: To determine the strength of Ferrous present in the given solution by using Potentiometric
titration.

Apparatus Required: Potentiometer, Calomel electrode, Platinum electrode, Beakers,


Burette, Pipette, Measuring cylinders, Volumetric flask etc.

Chemicals Required: Ferrous solution, Standard Potassium Dichromate solution (K2Cr2O7),


10% Sulphuric acid.

Theory:
In a potentiometric titration, a suitable electrode is immersed in the solution to be titrated acts
as the indicator electrode. The indicator electrode is paired with a reference electrode and the
two electrodes are connected to the Potentiometer. Since the reference electrode potential has
a constant value, any change in the indicator electrode potential is reflected by a similar change
in the cell potential. Therefore, the equivalence point can be found by plotting a graph between
the cell e.m.f and the volume of titrant added from the burette.
Chemical Equations:
6𝐹𝑒𝑆𝑂4 + 𝐾2 𝐶𝑟2 𝑂7 + 7𝐻2 𝑆𝑂4 → 3𝐹𝑒2 (𝑆𝑂4 )3 + 𝐶𝑟2 (𝑆𝑂4 )3 + 𝐾2 𝑆𝑂4 + 7𝐻2 𝑂

Principle:
Dichrometry titrations are based on oxidation reactions by dichromate ion. Its oxidizing
action is due to conversion of Cr2 O7- ions (containing Cr6+) into Cr3+ ions. Potassium
dichromate acts as an oxidizing agent in the presence of sulphuric acid. It oxidizes Fe2+ ion and
itself is reduced to green chromic salt.

Procedure:
Step-I: Estimation of Ferrous by using Potentiometer:
 The Potentiometer is calibrated and kept ready along with the electrodes.
 Burette is filled with standard Potassium Dichromate solution.
 10ml of Ferrous solution is pipetted out into a beaker and add 5 ml of 10% sulphuric
acid and the emf is measured.
 1ml of Potassium Dichromate is added to Ferrous solution through the burette. The
solution is mixed, and the emf is measured.
 This procedure is repeated for every addition of 1ml of Potassium dichromate solution
and the values are tabulated.

Graph:
A graph is plotted between volume of titrant (K2Cr2O7) added on X axis and emf on Y axis.
From the graph the volume of Potassium dichromate at equivalence point is noted.

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NRIA23 Chemistry Lab Manual

Observations and calculations:


Step-I : Estimation of Ferrous by using Potentiometer:

S.No. Volume of K2Cr2O7 Added(ml) emf (mV)

Formula:
𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2

Where,
M1 = Molarity of potassium dichromate solution = 0.01 M

V1 = Volume of potassium dichromate solution (From graph) =

n1 = No. of moles of potassium dichromate solution =1

M2 = Molarity of ferrous solution = ?

V2 = Volume of ferrous solution = 10 ml

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NRIA23 Chemistry Lab Manual

n2 = No. of moles of ferrous solution = 6

𝑀1 𝑉1 𝑛2
𝑀2 = ×
𝑛1 𝑉2

=
The strength of Ferrous present in one litre of the solution =
= 𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 × 𝑀𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡
= 𝑀2 × 56
= 𝑔𝑚/𝑙

Result:

The strength of ferrous present in the given solution is___________ gm/l

NRI INSTITUTE OF TECHNOLOGY, POTHAVARAPPADU 36

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