I B.Tech.

I SEMESTER
(ACER23 Academic Regulation)

DEPARTMENT OF HUMANITIES & BASIC SCIENCES

CHEMISTRY LAB MANUAL

CUM OBSERVATION BOOK

Name of the Student:

Regd No:

Branch/ Section:
CODE OF CONDUCT

1. Students should report to the concerned lab as per the time-table schedule.

2. Students who turn up late to the labs will in no case be permitted to perform the
experiment scheduled for the day.

3. After completion of the experiment, certification of the concerned staff in-charge in the
observation book is necessary.

4. The record of observations along with the detailed experimental procedure of the
experiment performed in the immediate last session should be submitted and certified by
the staffmember in-charge.

5. The group-wise division made in the beginning should be adhered to, and no mix up of
students among different groups will be permitted later.

6. The components required pertaining to the experiment should be collected from the lab
assistants.

7. When the experiment is completed, students should clean the apparatus, carefully
disposethe leftover chemicals and disconnect the setup made by them and should return
all the components/instruments taken for the purpose.

8. Any damage to apparatus that occurs during the experimentation should be brought to the
notice of lab in-charge, consequently, the cost of the repair or new apparatus should be
brought by the students.

9. Students should be present in the labs for the total scheduled duration.

10. Students are required to prepare thoroughly to perform the experiment before coming to
Laboratory.

11. Procedure sheets/data sheets provided to the students’ groups should be maintained
neatlyand to be returned after the experiment.
 L T P C
I Year – I SEM 0 0 2 1
CHEMISTRY LABORATORY SYLLABUS

Course Objectives:
 Verify the fundamental concepts with experiments.

Course Outcomes (COs): At the end of the course, the student will be able to:

CO1: Analyze the water quality parameters

CO2: Determine the quality of ore and Vitamin-C
CO3: Utilize basic instruments for analysis
CO4: Synthesize polymer and nano materials

List of Experiments:

1. Determination of Hardness of a ground water sample

2. Determination of Chloride content in given water sample
3. Estimation of dissolved oxygen in given water sample
4. Estimation of Vitamin-C
5. Analysis of Mn in Pyrolusite
6. Determination of Strength of an acid in Pb-Acid battery
7. Conductometric titration of strong acid vs strong base
8. Potentiometric determination of strong acid -strong base
9. Preparation of a polymer (Bakelite)
10. Preparation of nanomaterials
Augmented Experiments (Demonstration)
1. Wavelength measurement of sample through UV-Visible Spectroscopy
2. Identification of simple organic compounds by IR

Reference:
 "Vogel's Quantitative Chemical Analysis 6th Edition " Pearson Publications by J. Mendham,
R.C. Denney, J.D. Barnes, and B. Sivasankar

Of the above experiments at-least 10 assessment experiments should be completed in a

semester.
 LAB GUIDELINES

 Always work under the supervision of instructor in the lab.

 Wear an apron and closed-toe shoes to limit your chemical exposure and to save clothing
fromchemical stains.
 Keep the water and gas taps closed except when these utilities are needed.
 Read the procedure carefully before starting the experiment.
 Tie hair back and avoid bulky sleeves which interfere with work.
 Food and drink should not be taken to the lab, and never taste any lab chemical.
 Wash your hands after each session, before leaving the lab.
 Getting any kind of a chemical into the eyes, into the mouth or spills on the skin should
beflushed with tap water on the affected area at least 15 minutes and inform the instructor.
 In the case of a burn, apply cold water or ice immediately to the burned area until the
painsubsides.
 In the case of fire accident, it is the responsibility of the closest person to use the fire
extinguisher.
 In the case of bleeding from a cut, wash with soap water and inform the instructor
immediately.
 Submit the apparatus cleanly after completion of experiment.
 Take the permission of lab instructor before leaving the lab.
S. No Date Name of the Experiment CO Faculty Signature
 INTRODUCTION TO CHEMISTRY LAB
In all chemistry laboratories chemical analysis is carried out. Chemical analysis is the
resolution of a chemical compound into its proximate or ultimate parts.
It is divided into two types. They are,
I. Qualitative analysis and
II. Quantitative analysis.

I. QUALITATIVE ANALYSIS: It deals with identification and confirmation of the nature

of thesubstances or impurities present in a given sample.

II. QUANTITATIVE ANALYSIS: It deals with the determination of how much of each
component or of specified component is present.
QUANTITATIVE CHEMICAL ANALYSIS IS FURTHER DIVIDED INTO TWO
TYPES:

i. VOLUMETRIC ANALYSIS: The process of estimation of a substance based on

volume is called volumetric analysis. The volumetric analysis is carried out by a process known
as Titration. Hence, volumetric analysis is called titrimetric analysis.

LAW OF VOLUMETRIC ANALYSIS:

Whenever two Substances react together, they react in the ratio of their equivalent mass. One
liter of a normal solution of a substance will react exactly with same volume of a normal
solution of another substance. In other words, equal volumes of equal normal solutions will
exactly react with each other. This result is stated in the form law of volumetric analysis. If V 1
mL of a solution of strength N1 is required or complete reaction by V2 mL of the second
solution of strength N2 then,

N1 V1 = N2 V2

If any three factors (V1, V2 & N1) are known, the fourth factor N2 can be calculated. The
following are theimportant formula used in all volumetric estimations
Mass of solute per liter of the solution = Equivalent mass x Normality

ii. GRAVIMETRIC ANALYSIS: The process of estimation of a substance based on weight

is called gravimetric analysis.
Of the two methods gravimetric analysis is more accurate but volumetric analysis is much more
readily carried out.

ESSENTIAL CONDITIONS FOR ACCURATE TITRIMETRY:

i. The equation governing the reaction must be known.
ii. The reaction must go to completion, and there must be no complicating side reaction.
iii. There must be some means to assess the completion of the reaction (usually an indicator
isemployed).
iv. The standard solution must not alter in its strength during the period of experimentation.
Thesolution must be stable to light, atmosphere and must not react with the solvent.
TERMS USED IN VOLUMETRIC ANALYSIS:

(a) TITRATION: It is a process of adding one solution from the burette to another in

the conicalflask, in order to complete the chemical reaction. Out of the two solutions one must

be standard.
(b) TITRANT: The reagent from the burette is called as Titrant.
(c) TITRAND (TITRATE): The substances being titrated is termed as titrand or titrates
(d) EQUIVALENCE POINT OR STOICHIOMETRIC END POINT: It is the point at
which the amount of reagent (Titrant) and substance (titrate) being determined are
chemically equivalent or it is the exact stage at which the chemical reaction involved in the
titration is just completed.
(e) END POINT: The point at which the reaction between Titrant and titrate is just
complete is called Endpoint or Equivalence point.
The determination of end point accurately is very essential in volumetric analysis. Generally,
the endpoint in the titration is detected by using an indicator.
(f) INDICATOR: chemical species which indicate the end-point by a sharp visual color
change is called indicator. There are three types of indicators. They are,
i. Internal indicators,
ii. External indicators and
iii. Self – indicators.

i. INTERNAL INDICATORS:

The indicator added to the titrating solution is called internal indicator.

Ex: Phenolphthalein (or) methyl orange in acid-base titrations.

ii. EXTERNAL INDICATORS:

It is not added to the titrating solution, but used externally to detect the end point.
Ex: Potassium ferricyanide, the most familiar example of external indicator, is used during the
titration of ferrous ions as it gives blue color with ferrous ions and a brown coloration with
ferricions and thus tells us when a ferrous solution has been completely oxidized to the ferric
state. The indicator is used as external since if it is added to the ferrous solution to start with,
it would have been reacted with it.

iii. SELF - INDICATORS:

If one of the reacting solutions is in color, it acts as indicator in the titration. This kind of
indicator is called as Self-indicator. Ex: In the estimation of Mohr’s salt by KMnO4, KMnO4
acts as Self-indicator.
ACIDIMETRY AND ALKALIMETRY TITRATION:

Acidimetric refers to the titration of alkali with a standard acid and alkalimetry refers to the
titration of an acid with a standard alkali.
PERMANGANOMETRY TITRATION:

The titration involving KMnO4 is called permanganometry titration. In presence of dilute

H2SO4,KMnO4 oxidizes ferrous sulphate to ferric sulphate and oxidizes oxalic acid to CO 2
and H2O.

(g)TITRATION ERROR: Ideally, the visible end point and the equivalence point should
coincide but in practice there is always a difference between the two, this difference is
calledthe titration error.

SOLUTION: A solution is a homogeneous mixture of one or more solutes dissolved in a

solvent.
 Solvent: the substance in which a solute dissolve to produce a homogeneous mixture
 Solute: the substance that dissolves in a solvent to produce a homogeneous mixture

STANDARD SOLUTION: A solution of accurately known strength is called as standard

solution.
Standard solution is prepared by dissolving a definite known amount of a substance, called
primary standard substance in a definite volume of solvent.

PRIMARY STANDARD SUBSTANCE SHOULD SATISFY THE FOLLOWING

REQUIREMENTS:

 It must be easy to obtain in high purity and to preserve in a pure state.

 The substance should maintain its composition unchanged during storage and unaltered

inair during weighing; it is neither oxidized by air nor affected by carbon dioxide.

 It should neither be hygroscopic nor efflorescent.

 The total amount of impurities should not in general, exceed 0.01 – 0.02%.

 It should have a high equivalent weight so that the weighing errors may be negligible.

 The substance should be readily soluble in water under the conditions in which it is

employed. In practice, an ideal primary standard is difficult to obtain.

CONCENTRATION OF A STANDARD SOLUTION IS GENERALLY EXPRESSED

INTHE FOLLOWINGCHEMICAL UNITS:

MOLARITY (M):
Molarity is defined as the number of moles of solute present in one literof solution at given
temperature.

Weight of the Solute 1000

Molarity (M)=Gram Molecular weigh * V (in mL)

NORMALITY (N):
Normality is defined as the number of gram equivalents of solute present in one liter of
solution at given temperature.

𝑾𝒆𝒊𝒈𝒉𝒕 𝒐𝒇 𝒕𝒉𝒆 𝑺𝒐𝒍𝒖𝒕𝒆

Normality (N) = 𝑮𝒓𝒂𝒎 𝑬𝒖𝒖𝒊𝒗𝒒𝒍𝒆𝒏𝒕 𝒘𝒆𝒊𝒈𝒉𝒕 𝟏𝟎𝟎𝟎
* 𝑽 (𝒊𝒏 𝒎𝑳)
CLASSIFICATION OF VOLUMETRIC TITRATIONS:
Volumetric titrations are classified into four classes depending upon the type of reaction taking
place during the titration. They are

1. Acid – base titrations (neutralization titrations)

2. Red-ox titrations (oxidation-reduction)
3. Precipitation titrations
4. Complexometric titrations
1. ACID – BASE TITRATIONS (NEUTRALIZATION TITRATIONS):
Titrations based on neutralization reactions are called neutralization titrations or acid-base
titrations. In neutralization reaction an acid and a base react with each other and both become
neutral.

Ex: Estimation of HCl by using Na2CO3

ACID – BASE INDICATORS:

An acid-base indicator is a substance which has one color in acidic medium and a completely
different color in the base medium. In fact, the change in color of an acid-base indicator does
not take place at a particular pH value but takes place within a small range of pH (usually about
2 pH units). This range of pH is known as “color change interval” of the indicator. This is
different for different indicators.

2. REDOX TITRATIONS (OXIDATION-REDUCTION):

Titrations based on oxidation-reduction reactions are called oxidation-reduction titrations or
Redox titrations. The reactions which proceed with simultaneous loss and gain of electrons
among the reacting substances are called red-ox reactions or oxidation-reduction reaction.

Ex: Estimation of Oxalic acid by using KMnO4

COMMON OXIDIZING & REDUCING AGENTS:

OXIDIZING AGENTS: Potassium permanganate and potassium dichromate

REDUCING AGENTS: Mohr’s salt and oxalic acid.

INDICATORS FOR REDOX TITRATIONS:

These are of three types:

a. Self- indicators
b. External indicators
c. Redox indicators
3. PRECIPITATION TITRATIONS:
Titrations based upon the formation of insoluble precipitates when the reacting solutions are
brought together, such titrations are called precipitation titrations.

Ex: Estimation of Zinc using standard Potassium ferrocyanide solution.

4. COMPLEXOMETRIC TITRATIONS:
The titrations involving the formation of complex compounds are called complexometric

titrations.

Ex: Determination of hardness of water by using EDTA

EDTA forms very stable metal chelates with many metals. To simplify the representation of
EDTA, reactions with various metals, it is assigned the formula H4Y. Hence the disodium salt
of EDTA written as Na2H2Y which gives the complex forming ion H2Y2- in aqueous
solution, the reaction with differentcations may be written as:

M2+ + H2Y2- MY2- + 2H+

EDTA - STRUCTURE:

Ethylene Diamine Tetra Acetic Acid

Experiment No: Date:

DETERMINATION OF TOTAL HARDNESS OF GIVEN WATER

SAMPLE
AIM: To determine the total hardness of given water sample using standard (0.01 M) EDTA
solution.
APPARATUS REQUIRED: Burette, burette stand, pipette, conical flask, volumetric flask,
beaker, glazed tile and wash bottle.
CHEMICALS REQUIRED: Standard EDTA Solution, pH 10 Buffer (NH4Cl + NH4OH),
EBT (Eriochrome black T) indicator, Water sample
INDICATOR: EBT (Eriochrome black T) indicator
ENDPOINT: Wine red color to blue color.
INTRODUCTION:
Hardness of water is due to the presence of bicarbonates, chloride and sulphates of calcium and
magnesium. Hard water does not give lather easily with soap, as the hardness causing ions
react with soap to form insoluble precipitate (scum).
C17H35COONa + Ca+2 / Mg+2 → (C17H35COO) 2 Ca / Mg 
(Sodium stearate) (Insoluble scum)
Temporary hardness is due to the presence of bicarbonates of calcium and magnesium which
canbe removed by boiling the water. On boiling, the bicarbonates are converted into insoluble
carbonates of calcium and magnesium.
∆
Ca (HCO3)2 → CaCO3↓ + H2O + CO2 (Boiling)

∆
Mg (HCO3)2 → Mg (OH) 2 + CO2 + 2H2O

Permanent hardness is due to the presence of chlorides and sulphates of calcium and
magnesium which can be removed by only chemical treatment.The sum of temporary hardness
and permanent hardness is known as total hardness. The hardness is expressed in ppm (parts
per million).Hardness of water can be expressed as CaCO 3 equivalents as it is highly insoluble
salt and its Molecular Weight is 100.
PRINCIPLE:
Hardness of water is determined by titrating a known volume of water sample with EDTA
using EBT as indicator in the presence of pH10 buffer. EDTA is a strong Complexing agent
reacts quantitatively with the metal ions to form soluble stable 1: 1 complex.
DETERMINATION OF TOTAL HARDNESS OF THE GIVEN WATER SAMPLE:

Volume of water Volume of EDTA

Burette readings(mL)
S. No sample (mL) taken solution consumed (mL)
Initial Final
1

Consumed Volume of EDTA: mL

CALCULATION:
𝐌𝟏 𝐌𝟐 𝐕𝟐
𝐕𝟏 = 𝒏𝟐
𝒏𝟏

Where,

M2= Molarity of water sample =? M1= Molarity of EDTA solution = 0.01M

V2= Volume of water sample = 50 mL V1=Volume of EDTA solution rundown =

mL

n2 = no of moles of water = 1 n1 = no of moles of EDTA = 1

Molarity of water sample M2 = 𝐌𝟏 𝐕𝟏 𝐧𝟐

𝒏𝟏 𝑽𝟐

Total hardness of water = M2 * Molecular weight of CaCO3 * 1000 ppm (or)

mg/L

= M2* 100 * 1000 ppm (or) mg/L

The Total hardness of the given water sample = ppm

REPORT: The Total hardness of the given water sample = ppm

 EDTA + M2+  [EDTA – M] +2
Metal ion stable complex

When a few drops of the indicator EBT are added, it forms a wine-red complex with metal
ions.
M2+ + EBT  [M – EBT] +2 Complex
(Blue color) (Wine Red color)
When the solution is titrated, EDTA reacts, preferentially with the free metal ions present in
the solution. Near the end point, when the free metal ions are exhausted in the solution, further
addition of EDTA dissociates the [M-EBT] Complex, consumes the metal ions and releases
free indicator, which is blue in color. Therefore, the color change is from wine red to blue.

[M – EBT] + EDTA [M – EDTA] + EBT

Wine red color colorless colorless blue color

The indicator EBT shows the color change at pH range 9 – 11. Therefore, the pH of the solution

is maintained at about 10, using pH 10 buffers. EDTA being insoluble in water, it is generally

usedas a disodium salt of which readily dissolves in water.

METAL EDTA COMPLEX: EDTA is a hexadentate ligand and forms complexes with many
metal ions and the general structure of which is shown as follows.

METAL-EDTA COMPLEX STRUCTURE

PROCEDURE:
 All the apparatus were washed with tap water and rinsed with Distilled water.
 50 mL of the given water sample is taken into conical flask.
 2 mL of pH 10 buffer solution is added and it is shaken well.
 To these 2 drops of EBT indicator is added.
 The contents are titrated with EDTA solution which is taken in burette until the color
change from wine red to clear blue.
 The results are tabulated.

REPORT: The Total hardness of the given water sample = ppm

FACULTY SIGNATURE
 Experiment No: Date:

DETERMINATION OF CHLORIDE CONTENT OF WATER BY

ARGENTOMETRY (MOHR’S METHOD)
Aim: To estimate the chloride content present in given water sample using standard AgNO 3
solution.
Apparatus: Burette, Measuring jar, Pipette, Conical flask, Burette stand
Chemicals: Sample water, silver nitrate solution, potassium chromate (K2CrO4) solution.
Principle: -
The amount of chloride in water can be simply determined by titrating the water sample with
silver nitrate solution by using potassium chromate indicator. The reaction is quantitative. The
AgNO3 reacts with chloride ion in a 1:1 ratio.
When silver nitrate solution is gradually added into the flask, then silver ions react with
chloride ions and forms silver chloride. It is precipitated in bottom of the flask. The
precipitation is white in color.
AgNO3 (aq) + Cl–(aq) → AgCl(s) + NO3- (aq)

The end point of the titration takes place when all the chloride ions reacts and precipitated.
Then slightly extra silver ions react with the chromate ions and form a brownish-red precipitate
of silver chromate.
2AgNO3 (aq) + K2CrO4 (aq) → Ag2CrO4(s) + 2KNO3 (aq)

Procedure:
Determination of chloride content of water.

 All the apparatus were washed with tap water and rinsed with Distilled water.
 Burette is rinsed and filled with Silver Nitrate solution, including burette nozzle
without air bubbles.
 20 mL of water sample pipetted out into a clean conical flask.
 2-3 drops of Potassium chromate (K2CrO4) indicator was added to the conical flask,
the solution turns into Light Yellow color.
 The Resultant yellow color solution is Titrated against silver nitrate present in the
burette, turns into Permanent brick Red Color.
 Repeated the titrations to get concurrent values.
Tabular column:

S. No Volume of sample Burette reading in Volume of AgNO3

water (mL) (mL) Solution consumed
Initial Final (mL)

Calculations:
M1V1=M2V2

M1= Molarity of AgNO3 Solution = 0.01M

M2=Molarity of Water sample =?

V1=Volume of AgNO3 Consumed =

V2=Volume of Water sample taken =

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

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

Cl– present in the given water sample = mg/litre or ppm

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

FACULTY SIGNATURE
Experiment No: Date:

Determination of Dissolved Oxygen in a Water Sample

Aim: To determine the dissolved Oxygen content present in the given sample of water
Apparatus: Burette, Pipette, Conical flask, volumetric flask, DO bottle
Chemical Required: Potassium dichromate solution, Hypo solution, Manganese sulphate
solution, Alkaline Iodide- Azide solution, Starch Indicator, 10% Potassium Iodide solution.
Theory & Principle:
Dissolved Oxygen is one of the essential constituents for the existence of fish & other
aquatic life. The maximum amount of Oxygen, which can be dissolved in one liter of water, is
8.15mg and the minimum of D.O, which must be present per liter of oceans, is 5-8mg.
Dissolved Oxygen is basis of determining B.O.D which is a measure of pollution in water. It
can be determined iodometrically by Winkler’s method. The dissolved Oxygen present in water
Oxidizes Potassium Iodide liberating an equivalent amount of Iodine which is titrated against
a standard Hypo (Hypo) using starch as an Indicator. Oxygen carrier like Manganese
Hydroxide must be used to bring about the reaction between Potassium Iodide and dissolved
Oxygen because dissolved molecular Oxygen in water is not capable of reacting with
Potassium Iodide. Manganese Hydroxide is produced by the action of Potassium hydroxide
and manganese sulphate.

2 KOH + MnSO4 Mn (OH)2 + K2SO4

(Manganese hydroxide)
2 Mn(OH)2 + O2 2MnO(OH)2 (Manganic hydroxide)

MnO(OH)2 + 2H2SO4 Mn(SO4)2 + 3H2O

Mn(SO4)2 + 2KI MnSO4 + K2SO4 + I2

I2 + 2Na2S2O3 2NaI + Na2S4O6 (Sodium tetra thionate)

The Nitrates present in water interfere with the estimation of dissolved Oxygen of water, since
these ions liberate Iodine from Potassium Iodide, Sodium Azide is added to remove nitrate.
2NaN3 + H2SO4 2HN3 + Na2SO4
HNO2 + HN3 N2O + N2 + H2O
Table: - Determination of D.O of water sample by titrating with Standardized Hypo
solution

Burette reading Hypo

Volume of water (mL) Volume of Hypo
S. No
sample (mL) rundown (mL)
Initial Final

According to law of equivalence

N1V1= N2V2

N1 = Normality of Hypo = N
V1 = Volume of Hypo solution = Titre value with water sample (in mL)
N2 = Normality of Oxygen in water sample = ?
V2 = Volume of water sample = 50 mL

N1V1
N2 = V2

Amount of Dissolved Oxygen in water sample = N2 x 8 x 1000 = ppm

Result: Amount of Dissolved Oxygen in water sample = ppm

PROCEDURE:
Determination of D.O in water sample.

 All the apparatus were washed with tap water and rinsed with Distilled water.
 250mL of water sample is taken in a bottle having stopper to prevent possible contact
with air and is not agitated as there may be a change in the dissolved Oxygen
concentration.
 2mL of Manganese Sulphate and 2mL of Alkaline Iodide- Azide solutions are added to
the water sample.
 The contents in the bottle are shaken well and allowed to stand so that brown precipitate
of basic manganese oxide MnO (OH)2 (Manganic Hydroxide) settles down.
 2mL of concentrated H2SO4 is added drop wise with stirring to dissolve the precipitates
and again allowed to stand for 5minutes.
 Now 50mL of above solution is taken and titrated against standardized Hypo solution
till a pale-yellow color is obtained.
 1-2mL Starch solution is added which turns the solution into blue color and titrated
against Hypo solution until blue color disappears.
 The titrations are continued until 3 concurrent readings are obtained and the readings
are tabulated in Table.

Report: Amount of Dissolved Oxygen in water sample = ppm

FACULTY SIGNATURE
Experiment No: Date:

CONDUCTOMETRIC TITRATIONS BETWEEN STRONG ACID AND STRONG BASE

AIM: To determine the strength of strong acid (HCl) by titrating with strong base (NaOH)
conductometrically.

APPARATUS REQUIRED:

Conductivity meter, conductivity cells, micro burette, volumetric flasks and

beaker. CHEMICALS REQUIRED: HCl, NaOH and Conductivity water

PRINCIPLE:

When an acid is added to an alkali the conductance of the solution is initially high because HCl is
a strong electrolyte and dissociates to give the fast-moving H + ions. However,when NaOH solution
is added to the HCl solution fast moving H + ions are replaced by the slow-moving Na + ions and
hence the conductance of the solution decreases. The conductance goes ondecreasing on the addition
of NaOH solution till whole of the H+ ions are replaced by Na+ ions.

After the end point has reached, further addition of NaOH results in increase in conductance, since
the OH- ions are no longer used up in chemical reaction. At the neutral point the conductance of the
system will have a minimum value from which the equivalence point can be determined. Therefore,
when the conductance of the solution is plotted against the number of mL of the base added two
curves are obtained. The point of intersection of the two curves gives the end point of the titration.

PROCEDURE:
 All the apparatus were washed with tap water and rinsed with Distilled water.
 50 mL of acid is taken in 100 mL beaker.

 Then conductivity cell is kept in the beaker.

 The conductance of the solution is determined using conductivity meter.

 The titrating solution which is 10 times more concentrated than the acid is taken in a micro
burette and is allowedto run down in small quantities (0.5mL) and after each addition the
solution is well stirred and the conductivity is measured.

 This is continued up to neutral point is reached.

 The corrected conductance can be obtained

𝟓𝟎+𝑽
from, Corrected conductance, C’ = C ( ) µho
𝟓𝟎
Where,
C = Observed
conductance v = Volume
of NaOH
CONDUCTOMETRIC TITRATIONS BETWEEN STRONG ACID AND STRONG BASE:

S. No Volume of NaOH (V in Conductance (C in Corrected

mL) µho) conductance(C’)
C’ = C ( 𝟓𝟎+𝐕 / 50 ) µho

Calculations:
𝑵𝟐 𝑽𝟐
N1V1 = N2V2 N1 =
𝑽𝟏
Where N1= Normality of HCl solution = ?

V1= Consumed Volume of HCl solution =_ mL

N2= Normality of NaOH = 0.1N

V2 = Volume of NaOH =_______________mL (From Graph – End Point)

𝑵𝟐 𝑽𝟐
N1 = 𝑽𝟏 =
 GRAPH:

A graph is drawn with corrected conductance against the volume of NaOH added, and
the point of intersection of curves gives the equivalence point.

MODEL GRAPH: NaOH vs. Corrected Conductance:

REPORT: The strength of given HCl solution by conductance is = _N

FACULTY SIGNATURE
Experiment No: Date:
POTENTIOMETRIC TITRATIONS BETWEEN STRONGACID AND
STRONG BASE
AIM: To determine the end point of an acid base reaction [HCl & NaOH] by potentiometer.

APPARATUS REQUIRED: Potentiometer, Wheatstone bridge, calomel electrode, Battery,

Quinhydrone, Platinum electrode, magnetic stirrer, micro burette.

CHEMICALS REQUIRED: HCl solution (unknown), 0.1N NaOH solution and distilled
water.

PRINCEPLE: The following cell,

H2 (pt)/ Acid solution // Aq. KCl /calomel electrode
Have its E. M. F dependent on the pH of the solution. On adding small Quantities of the
standard solution of an alkali to the acid, the E.M.F of the cell vary slowly at first, because the
change in the electrode potential depends on the fraction of Hydrogen ions removed. As the
amount of alkali added approaches equivalence to the amount of Hydrogen ions in the solution,
the fraction of the Hydrogen ion concentration removed by each drop of the alkali rapidly
increases and there is a correspondingly rapid change in the E.M.F thus the endpoint of the
reaction is characterized by the sudden jump in the potential.
PROCEDURE:
 All the apparatus were washed with tap water and rinsed with Distilled water.

 Exactly 50 mL of the acid is pipetted out into a 100 mL beaker and it is saturated with
Quinhydrone and a Platinum electrode is dipped into the solution.

 A calomel electrode is placed in the solution and the cell thus formed is connected to a
potentiometer.

 The beaker is placed under a burette filled with standard Sodium hydroxide solution.

 A magnetic stirrer is used to stir the solution uniformly and effectively.

 The E.M.F of the cell is measured by means of the potentiometer.

 The alkali is added from the burette at the rate of 1mLfor rough titration and the
approximate end point is noted.

 Then the titration is repeated by adding 0.1mLof the alkali near the end point and the
E.M.F is measured after each addition.
POTENTIOMETRIC TITRATIONS BETWEEN STRONG ACID AND STRONG BASE:

Pilot titration

S. No. Volume of E.M.F in milli volts

alkali(NaOH) (V in mL)
GRAPH: Two graphs are drawn, one between the E.M.F measured and the volume of alkali
added and another between the value of ∆E/∆V and the volume of alkali added.
MODEL GRAPHS:

GRAPH 1: EMF Vs. volume of NaOH: GRAPH 2: ∆E /∆V vs. volume of NaOH:

REPORT: The strength of given HCl solution by potentiometer is = N

Accurate Titration:

Volume of
E.M.F inmilli ∆𝐄 / ∆𝐕
S. No alkali (NaOH)(V in ∆V ∆E
volts (E)
mL)

Calculations:

Calculations:
𝑵𝟐 𝑽𝟐
N1V1 = N2V2 N1 = =
𝑽𝟏
Where,
N1= Normality of HCl solution = ?
V1= Consumed Volume of HCl solution = mL
N2= Normality of NaOH = 0.1N
V2 = Volume of NaOH = ___ mL (From Graph – End Point)

Strength of HCl, N1 = 𝑵𝟐 𝑽𝟐 =
𝑽𝟏

REPORT: The strength of given HCl solution = N

FACULTY SIGNATURE
Experiment No: Date:

PREPARATION PHENOL-FORMALDEHYDE RESIN (BAKELITE)

AIM: To prepare phenol formaldehyde resin.

REQUIRED CHEMICALS: Glacial Acetic acid, 40% formaldehyde solution, Phenol,

Conc. H2SO4

APPARATUS: Glass rod, beakers, funnel and filter paper

PRINCIPLE:
Phenolic resins are condensation polymerization products of Phenolic derivatives with
aldehydes (like formaldehyde, furfural). It is prepared by condensing phenol with
formaldehyde in presence of acidic catalyst.
PROCEDURE:

 All the apparatus were washed with tap water and rinsed with Distilled water.
 5 mL of Glacial Acetic acid and 3 mL of 40% Formaldehyde Solution added into a
beaker.
 2 grams of Phenol added to the beaker solution.
 2-3 mL of Concentrated Sulfuric Acid solution into the beaker resultant solution.
 Within five minutes a large mass of Plastic is formed.
 The Resultant Residue is washed several times with distilled water and filtered.
 The resultant product is dried and yield is calculated.

REPORT:

The Yield of the phenol-formaldehyde resin is = g

FACULTY SIGNATURE
Experiment No: Date:
DETERMINATION OF VITAMIN – C

AIM:
To determine the amount of Vitamin-C (ascorbic acid) present in given 100mL solutionusing
standard tri-iodide solution.

APPARATUS REQUIRED:
Burette, pipette, conical flask, burette stand, volumetric flask, measuring jar, white glazed tile
and wash bottle.

CHEMICALS REQUIRED:

Vitamin-C tablets / lemon juice / orange juice, 0.05N tri-iodide solution (potassium iodide+
potassium iodate), freshly prepared starch indicator and distilled water.

PRINCIPLE: Vitamin-C can be oxidized to dehydro ascorbic acid by tri-iodide ion.

C6H8O6 + I2 → C6H6O6 + 2 HI

Ascorbic acid dehydro ascorbic acid Hydrogen Iodide

During The titration, presence of iodine is possible only when all the vitamin-C is completely
oxidized. Then left over iodine reacts with the starch to give blue color as the end point.

VITAMIN-C STRUCTURE:

PROCEDURE:

DETERMINATION OF VITAMINE-C SOLUTION.

 All the apparatus were washed with tap water and rinsed with Distilled water.
 10 mL of Vitamin – C solution pipetted out into a conical flask.
 2-3 drops of 1% freshly prepared starch indicator added to the conical flask.
 Rinsed burette is filled with tri-iodide solution, including burette nozzle without air
bubbles.
 The Resultant conical flask solution is titrated against burette containing tri-iodide
solution.
 It turns into blue color.
 Repeat the titration to get concordant values.

Report: The amount of Vitamin-C present in given solution = grams

Calculation:

Volume of Vitamin-C Burette readings(mL) Volume of

S. No. solution (mL) triiodide solution
Initial Final consumed(mL)

CALCULATION: Formula, N1 V1 = N2 V2

N1 - Normality of I3 solution = 0.05N

V1 - Volume of I3 Solution = mL
N2 - Normality of Vitamin - C solution =?

V2 - Volume of Vitamin-C = 10 mL

Normality of Vitamin - C in the given solution, N2

N1V1 = N2V2

𝑵𝟏 𝑽𝟏
N2 = 𝑽𝟐
The amount of Vitamin-C present in the given solution (100mL) is

𝐍𝟐 𝒙 𝐄𝐪𝐮𝐢.𝒘𝒆𝒊𝒈𝒉𝒕 𝑽𝒊𝒕𝒂𝒎𝒊𝒏–𝑪 𝒙 𝒗𝒐𝒍.𝒐𝒇 𝒈𝒊𝒗𝒆𝒏 𝒔𝒐𝒍𝒖𝒕𝒊𝒐𝒏

= 𝟏𝟎𝟎𝟎
𝐍𝟐 𝒙 𝟖𝟖 𝒙 𝟏𝟎𝟎
= 𝟏𝟎𝟎𝟎

Report: The amount of Vitamin-C present in the given solution (100mL) is = g

FACULTY SIGNATURE
Experiment No: Date:

DETERMINATION OF STRENGTH OF SULFURIC ACID IN Pb-ACID

BATTERY

AIM:
To determine the strength of a sulfuric acid solution in Pb-acid battery by titration with standard
NaOH solution

CHEMICALS REQUIRED: H2SO4, NaOH, Phenolphthalein indicator

APPARATUS REQUIRED: Burette, Pipette, Conical Flask, Flask, Burette Stand.

PRINCIPLE:
Titration is the process, of determining the concentration of a substance in solution (The
analyte) by adding it to a standard reagent of known concentration (the Titrant) in carefully
measured amounts until a reaction of definite and known proportion is completed, as shown by
a color change or electrical measurement, and then calculating the unknown concentration. In
this experiment, sulfuric acid is titrated with sodium hydroxide.
2 NaOH + H2SO4 → Na2SO4 + 2 H2O
The titration is done in the presence of phenolphthalein indicator that is colorless in acid
solution but turns pink in basic solution. At the equivalence point, all of the analyte has reacted,
and only a tiny excess of Titrant has been added, just enough to change the color of the
indicator.
PROCEDURE:
 All the apparatus were washed with tap water and rinsed with Distilled water.
 The burette is rinsed with the given acid solution and filledwith same without air
bubbles, including nozzle.
 10ml standard sodium hydroxide solution is pipetted outinto a clean conical flask
carefully. Two drops of phenolphthalein indicator are added directly to the contents
of conical flask.
 The conical flask contents are titrated with given acid solution after noting the initial
reading.
 The titration is continued till the color changes from pink to colorless. The final
reading of burette is noted.
 A number of titrations are repeated for getting concurrent results.
CALCULATIONS:

Volume of NaOH Consumed Volume of

Burette readings(mL)
S. No sample (mL) taken Sulfuric acid solution
Initial Final (mL)

Calculations:

Normality of NaOH N1 = 0.1 N

Volume of NaOH Consumed V1 = ml
Normality of H2SO4 N2 = ? N
Volume of H2SO4 Pipette out V2= ml

N1V1 =N2V2

N2 = N1V1 / V2

RESULT: Strength of Sulfuric acid in Pb-acid battery is = N

FACULTY SIGNATURE
Experiment No: Date:

ESTIMATION OF Mn IN PYROLUSITE

AIM: To estimate the Mn content present in the given sample of pyrolusite

APPARATUS: Pipette, burette, conical flask, beaker, Bunsen burner

CHEMICALS REQUIRED: Pyrolusite, Oxalic acid, dilute H2SO4, KMnO4

INDICATOR: KMnO4 acts as self indicator

END POINT: Colourless – Pale Pink

PRINCIPLE:

MnO2 occurs in the nature in the form of pyrolusite. Pyrolusite is not only used as asource of
mangane4se but also as an oxidizing agent in many industrial processes. For such purposes, ore
is graded on the basis of its available oxygen content rather than on itspercentage of manganese.

The percentage of MnO2 is usually determined by treatment with an excess of acidified solution
of a reducing agent, oxalic acid. The excess of reducing agent isdetermined by titration with
standard KMnO4 where KMnO4 acts as a self-indicator with pale pink color as the end point.

MnO2 + H2C2O4 + H2SO4 MnSO4 + 2CO2 + 2H2O

2 KMnO4 + 3 H2SO4 + 5 H2C2O4 → 2MnSO4 + K2SO4 + 10CO2 + 8H2O

PROCEDURE:
 All the apparatus were washed with tap water and rinsed with Distilled water.
 Rinsed burette and it is filled with KMnO4 solution.
 0.25 g of pyrolusite sample is finely grounded and dissolved in 100 mL.
 10 mL of Pyrolusite solution is pipetted out into a conical flask, 20 mL of Oxalic Acid
solution and 5 mL of Diluted sulfuric acid is added to the conical flask solution.
The conical flask contents were heated to about 600C to increase the rate of reaction.
 The Resultant solution is titrated against KMnO4 solution until permanent pink color
is observed.
 Titration was repeated with another sample of Pyrolusite
 Amount of Mn present ion Pyrolusite can be calculated from the volume of oxalic acid
reacted equivalently with pyrolusite.
 OBSERVATION AND CALCULATIONS:

Volume of the Burette Reading

S. No Volume ofKMnO4
Oxalic acid
solution taken Initial Final consumed (mL)
(mL)

Calculations:

N1V1 =N2V2

N1 = Normality of Pyrolusite = ?

V1 = Volume of Oxalic acid solution reacted = 20- mL

N2 = Normality of KMnO4 Solution = 0.02 N

V2 = Volume of KMnO4 Solution = mL (Burette reading)

N1 =N2V2/V1

Amount of Mn Present in given 100 mL of Sample =

N1 X Gram Equivalent weight of Mn in MnO2 X Volume of Solution /1000

g
(Gram Equivalent weight of Mn in MnO2 = 43.5)

% Mn present in given sample = Amount of Mn/ Weight of Sample taken *100

ESULT: % Mn present in given sample is %

FACULTY SIGNATURE
Experiment No: Date:

SYNTHESIS OF NANO-SIZED ZnO BY PRECIPITATION METHOD

AIM: To Prepare Nano-sized ZnO material by precipitation method

Chemicals Required:
Zinc nitrate hexahydrate (Zn (NO3)2.6H2O), Sodium carbonate (Na2CO3),
Ethanol (C2H5OH, 95%,).
Apparatus: Beakers, Measuring Jars
Procedure for Preparation of ZnO nanoparticles.
 All the apparatus were washed with tap water and rinsed with Distilled water.
 Two solutions are prepared
 Solution A: 0.1 mol Zn (NO3)2.6H2O is prepared by dissolving 29.75g of Zinc nitrate
hexahydrate in 200 ml distilled water;
 Solution B: 0.12 mol Na2CO3 is prepared by dissolving 12.72 g of sodium carbonate in
240ml distilled water.
 After that solution A is added to solution B drop wise under vigorous stirring.
 The white precipitate is collected by filtration and rinsed with distilled water three
times. The solid is then washed with ethanol and dried at 100°C for 6 h.
 Finally, ZnO nanoparticles areobtained after annealing of the solid in air at 250, 300,
350, 400, 500, and 600°C for 2 h, respectively.

Characterization:
 The optical properties of prepared ZnO NPs are analyzed by UV-visible
Spectrophotometer (Shimadzu, UV-2450). A broad absorption peak is observed in
each spectrum at 355-380 nm which is a characteristic band for the pure ZnO.
 The FT-IR shows a broad absorption band related to Zn-O vibration band at 500 cm-1.
 The SEM results show the formation of spherical shaped nano particles.

Report:--

FACULTY SIGNATURE