Chemistry Lab R23 Manual NRI
Chemistry Lab R23 Manual NRI
Chemistry Lab R23 Manual NRI
(AUTONOMOUS)
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NRIA23
CHEMISTRY
LAB MANUAL
NRIA23 Chemistry Lab Manual
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
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
Chemistry Lab
Common to (CSE, CSE -R, CSM, CSD, IT, AIML, ECE, EEE)
Regulation: R23 Academic Year: 2023-24
Chemistry Lab
Common to (CSE, CSE -R, CSM, CSD, IT, AIML, ECE, EEE)
Regulation: R23 Academic Year: 2023-24
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.
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.
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.
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.
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:
Formula:
𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2
Where
M1 = Molarity of Oxalic acid solution = 0.15 M
𝑀1 𝑉1 𝑛2
𝑀2 = ×
𝑛1 𝑉2
=
=
Formula:
𝑀2 𝑉2 𝑀3 𝑉3
=
𝑛2 𝑛3
Where
M2 = Molarity of NaOH solution =
Result: The strength of acid present in the given sample solution is ---------g/L
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.
Formula:
𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2
Where
M1 = Molarity of Sodium carbonate solution = 0.05 M
𝑀1 𝑉1 𝑛2
𝑀2 = ×
𝑛1 𝑉2
=
=
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.
Formula:
𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2
Where
M1 = Molarity of potassium dichromate solution = 0.01M
𝑀1 𝑉1 𝑛2
𝑀2 = ×
𝑛1 𝑉2
The amount of ferrous ion present in the given solution is____________ g/L
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:
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.
Formula:
𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2
Where
M1 = Molarity of Oxalic acid solution = 0.05M
𝑀1 𝑉1 𝑛2
𝑀2 = ×
𝑛1 𝑉2
Result:
The Amount of Potassium Permanganate present in the given solution is ____________ g/L
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)
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.
Formula:
𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2
Where
M1 = Molarity of Zinc sulphate solution = 0.01M
𝑀1 𝑉1 𝑛2
𝑀2 = ×
𝑛1 𝑉2
=
Formula:
𝑀2 𝑉2 𝑀3 𝑉3
=
𝑛2 𝑛3
Where
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
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)
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.
Formula:
𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2
Where
M1 = Molarity of Zinc sulphate solution = 0.01M
𝑀1 𝑉1 𝑛2
𝑀2 = ×
𝑛1 𝑉2
=
Formula:
𝑀2 𝑉2 𝑀3 𝑉3
=
𝑛2 𝑛3
Where
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:
PREPARATION OF BAKELITE
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
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.
Apparatus Required: Colorimeter, Cuvette, Beakers, Measuring Cylinders, Test tubes etc.
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.
Result:
Lambert – Beer’s Law is verified.
Aim: To determine the strength of HCl present in the given solution by using Conductometric
titration.
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.
Formula:
𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2
Where
M1 = Molarity of NaOH solution = 0.1 M
𝑀1 𝑉1 𝑛2
𝑀2 = ×
𝑛1 𝑉2
=
=
Result:
The Strength of HCl present in the given solution is ____________ gm/l
Aim: To determine the strength of Ferrous present in the given solution by using Potentiometric
titration.
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.
Formula:
𝑀1 𝑉1 𝑀2 𝑉2
=
𝑛1 𝑛2
Where,
M1 = Molarity of potassium dichromate solution = 0.01 M
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: