GEC I B.TECH. Chemistry Lab Experiments

GUDLAVALLERU ENGINEERING COLLEGE
(An Autonomous Institute Affiliated to JNTUK, Kakinada)

Seshadri Rao Knowledge Village, Gudlavalleru 521 356. Krishna District, Andhra Pradesh
I B.TECH. R14 REGULATION
P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 1

List of Experiments
Introduction to Chemistry Lab (the teachers are expected to teach fundamentals like
Primary, Secondary Standard Solutions , Normality, Molarity, Molality etc. and
laboratory ware used, error ,accuracy, precision, Theory of indicators, use of
volumetric titrations.
1) Practice experiment-Determination of the amount of HCl using standard Na2CO3.

2) Determination of alkalinity of water sample.
3) Determination of acidity of water sample.
4) Determination of Ferrous iron by permanganometric method.
5) Determination of Ferric Iron using standard K2Cr2O7 solution.
6) Determination of Total hardness of the water sample by EDTA method.
7) pH metric titrations - Determination of concentration of HCl using glass electrode.
8) Determination of pH of the water sample by using pH meter.
9) Determination of conductivity of the water sample by using conductivity meter.
10) Conductometric titrations between strong acid and strong base
11) Determination of turbidity of the water sample by using turbidity meter.
12) Estimation of total dissolved salts in water sample.
13) Preparation of Phenol - Formaldehyde resin.

Ex.No:1
Date:
INTRODUCTION TO CHEMISTRY LAB
Analytical chemistry is mainly divided into two.

1. Qualitative analysis 2. Quantitative analysis
1. Qualitative analysis: It deals with the detection and identification of the constituents
present in the given substance whether an element, compound or a mixture.
2. Quantitative analysis: It deals with the determination of the respective amounts of
any constituents of chemical substances.
Quantitative chemical analysis is further divided into two types.

i) Volumetric analysis ii) Gravimetrical analysis .
i) Volumetric Analysis: In volumetric analysis, the substance to be estimated is made
to react in solution, with another solution of a substance of a known strength.
ii) Gravimetrical Analysis: In Gravimetric analysis, the estimation of a substance is
carried out by the process of weighing. In this analysis the component to be estimated
is converted into an insoluble compound of known chemical composition, and this
compound is separated, purified, dried and weighed.
Terms used in Volumetric Analysis:

TITRATION: It is a process of one solution from the burette to another in the conical flask,
in order to complete the chemical reaction. Out of the two solutions, one must be standard.
END POINT (OR) EQUIVALENT POINT: The point at which the colour change of the
indicator is visible to the eye is called the End Point.
TITRANT: The reagent from the burette is called as Titrant.
TITRATE: The substance being titrated is termed as Titrate.
STANDARD SOLUTION: A standard solution is one, whose concentration or strength is
known, that is the amount of the substance dissolved in one liter (1000ml) of the solution.
If a reagent is available in pure state, its standard solution is prepared by dissolving an
accurately weighed amount of it in water and making the solution to a known volume by
dilution. It is called the Direct Method. All such substances whose standard solutions are
made by the direct method are termed Standard Substances or primary standards.
Oxalic acid crystals, succinic acid, anhydrous sodium carbonate, potassium dichromate,

ferrous ammonium sulphate (Mohrs salt), silver nitrate, sodium chloride, potassium chloride,
etc. belong to this category.
A standard substance is required to fulfill the following conditions:
1. It must be obtainable in a highly purified state
2. It must be stable in air.
3. It must be readily soluble in water.
4. It should possess a large equivalent weight so as to minimize the weighing error.
5. The error in determining the end point must be negligible.
The direct method is not possible in case of those substances which, in general, fall short of
the above conditions eg. Alkali hydroxides, inorganic acids (like HCl, H2SO4, HNO3, etc.).
These are called the Secondary Standards. Their standard solutions are prepared by the so
called Indirect method. An approximately desired weight of the substance is dissolved in
water and the solution is made up to a known volume. The exact strength of the solution is
then determined by Standardisation, i.e., titration with a suitable standard reagent.
The concentration or strength of a solution can be represented in different ways.
Eg. Molarity, Normality, Molality.
Molarity (M): The molarity of a solution is defined as the no. of moles of the solute present
in one litre of solution.
No. of moles
Molarity( M )
No. of litre s of Solution
Weight of Solute 1000

gram molecular wt . of solute Vol. of solution in ml
V1M 1 V2 M 2
in volumetric analysis, Molarity expression is
n1 n2
where V1, M1 and n1 represent the volume, molarity and no. of moles of the first solution.
sssV2, M2 and n2 represent volume, molarity and no. of moles of the second solution.
Normality (N): The Normality of a solution is defined as the no. of gram equivalents of the solute
present in one litre of solution.
No. of gm. equivalents . of Solute

Normality (N)
No. of liters of solution
Weight of Solute 1000

gram equiv. wt . of solute Vol. of solution in ml

in volumetric analysis, Normality expression is V1N1 = V2N2
Where V1 and N1 represent the volume and normality of the first solution.
V2 and N2 represent volume and normality of the second solution.
Molality (m): Molality is the number of moles of the solute present per 1000 grams (1 kg) of the
solvent and is denoted by m.
Laboratory Ware used:
1) Pipette: It is used to transport a measured volume of liquid.
2) Burette: It is a vertical cylindrical piece of laboratory glassware with a volumentric graudation
on its full length and a precision tap, or stopcock, on the bottom. It is used to dispense known
amounts of liquid in experiments.
3) Conical Flask: It is a widely used type of laboratory flask which features a conical base and
cylindrical neck.
4) Volumetric Flask: It is a piece of laboratory glassware used in analytical chemistry for the
preparation of solutions. It is made of glass or plastic and consists of a flat-bottomed bulb with
a long neck, usually fitted with a stopper.
General Precautions:
1) Do not touch the bulb of pipette.
2) Do not blow the last drop of pipette.
3) Use pointing finger to control the flow from pipette.
4) The tip of pipette should immerse completely into solution, while taking the sample with
pipette.
5) Rinse the pipette and burette with the solution that you going to take in it.
6) Do no wash or rinse the conical flask with any solution except with distilled water.
7) Use glazed tile.
8) Take reading without any parallax errors.
9) For colorless solutions lower meniscus is considered for reading.
10) For coloured solutions upper meniscus is considered for reading.
Error: Error of a measurement is the difference between the measured value and the true value.
Accuracy: It is the closeness of a measured value to the true or accepted value.
Precision: Precision describes the reproducibility of measurements, i.e., the closeness of
results that have been obtained in exactly the same way.
Titrimetric/Volumetric Analysis & Type of Reactions:
1) Neutralisation reactions (or) Acidimetry and Alkalimetry:

a) Titration of free bases/salts of weak acids by hydrolysis with a standard acid
(Acidimetry).
b) Titration of free acids/hydrolysis of salts of weak bases with a standard base
(Alkalimetry).
2) Complex Formation Reactions: The combination of ions to form a soluble, slightly
dissociated ion/compound.
EDTA is the most important reagent used in titrimetric analysis of complexometry.
3) Precipitation Reactions: The combination of ions to form a simple precipitate.
Ag+ with a solution of a chloride.
No change in Oxidation state occurs.
4) Oxidation-Reduction Reactions: All reactions involving change of Oxidation number
or transfer of electrons among the reacting substances. The standard solutions are either
Oxidizing or reducing agents.
Indicator: Indicator is a substance which indicate by a sharp change in colour at the end
point in a titration.
Working(Theory) of Indicators:
Indicators are of various types. These are used in
1. Acid Base titrations
2. Complexometric titrations
3. Precipitation titrations
4. Redox titrations.
But there are some titrations in which one of the reactants itself acts as
indicator. There is no need of adding indicator from outside. Such titrations are called self
indicator titrations.
Working of acid base indicator:

There are many acid base indicators.
Example Colour change pH range

Methyl orange Red Orange 3.1 4.4
Phenolphthalein Colourless Pink 8.3 10.0
Methyl red Red Yellow 4.4 6.0
Litmus Red Blue 5.0 8.0
Every indicator shows colour change at its respective pHrange mentioned above. For instance
methyl orange shows red colour up to pH 3.1 and orange colour beyond pH 4.4. Methyl
orange exists in two structures, one is benzenoid (yellow in basic medium) and another one is
quinonoid (red in acidic medium). These two structures are in equilibrium with each other.

CH3
N N=N SO3 Yellow (Basic solution)
CH 3
Benzenoid
CH3
N N HN SO3H Red (Acid solution)
CH3
Quinonoid
Below pH 3.1, it exists in quinonoid structure and shows red colour and
above pH 4.4, it exists in benzenoid structure with orange colour or yellow colour.
Selection of an acid base indicator depends mainly on two factors.
1. pH range of the indicator.
2. Change in pH of the solution at the end point.
An indicator shows colour change when the above two factors match with each other.
Working of indicator in Complexometric titration:

In analytical chemistry Complexometric indicators are used in Complexometric titration to
indicate the exact moment when all the metal ions in the solution are sequestered by a
chelating agent (most usually EDTA). Such indicators are also called metallochromic
indicators.
To carry out metal cation titrations using EDTA, it is almost always necessary to use a
Complexometric indicator to determine when the end point has been reached. Common
indicators are organic dyes such as Fast Sulphon Black, Eriochrome Black T, Eriochrome
Red B or Murexide. These dyes bind to the metal cations in solution to form colored
complexes. However, since EDTA binds to metal cations much more strongly than does the
dye used as an indicator, the EDTA will displace the dye from the metal cations as it is added
to the solution of analyte. A colour change in the solution being titrated indicates that all of
the dye has been displaced from the metal cations in solution, and that the endpoint has been
reached. Thus, the free indicator (rather than the metal complex) serves as the endpoint
indicator.
EBT + M2+ (Ca2+, Mg2+) (EBT) M2+

Wine red
(EBT) M2+ + EDTA (EDTA) M 2+ + EBT

Wine red Colourless Blue

Working of indicator in Precipitation titration:
Indicator is precipitated in readily visible form from the solution at or near the
equivalence point of a titration.
Ex: During the estimation of chlorides in water, potassium chromate (yellow) is used as
indicator. Potassium chromate is precipitated as brick red coloured silver chromate at the end
point.
K2CrO4 + 2AgNO3 2KNO3 + Ag2CrO4

Yellow Brick red
Working of indicator in Redox Titrations:

I. Redox Indicators
A. Redox titrations Using Colored Titrant
6 Fe+2 + 14 H+ + Cr2O7-2 6 Fe+3 + 2 Cr+3 + 7 H2O

Titrant
No Color -----> Orange
5 Fe+2 + MnO4- + 8H+ 5 Fe+3 + Mn+2 + 4 H2O

Titrant
No Color -----> Pink
B. Redox Indicators
1. Highly colored substances that may be reversibly oxidized or reduced and change
colors upon oxidation and reduction
Inox + ne- + m H+ Inred
one color another color
2. Each redox indicator changes color over a certain potential range
Hence indicator must have a transition potential corresponding closely to the
equivalence point potential of the titration
Inox + ne- + m H+ Inred

Expt.No:1
Date:
ESTIMATION OF HYDROCHLORIC ACID

Aim: To determine the normality and amount of Hydrochloric acid present in given 1 litre solution
using 0.05N standard sodium carbonate solution.
Apparatus: 1) Burette 2) Pipette3) Conical Flask 4) Beakers 5) Burette stand 6)
Glazed tile 7) Wash bottle.
Chemicals required: Hydrochloric acid solution ,Standard Sodium carbonate solution , Methyl
orange indicator.
Principle: Hydrochloric acid reacts with Sodium carbonate solution according to the following
equation. This is known as neutralization reaction.
Na2CO3 + 2 HCl 2 NaCl + H2O + CO2
Procedure:
1. The burette is rinsed with tap water, then with distilled water finally with the given
Hydrochloric acid solution. The burette is filled with Hydrochloric acid and the
nozzle portion is also completely filled with the solution with out any air bubbles in it.
The initial reading of the burette is adjusted to Zero ml.. The burette is clamped
vertically to a burette stand.
2. A 10ml pipette is taken. It is rinsed with tap water, then with distilled water and
finally with the given sodium carbonate solution. 10ml of Sodium Carbonate is
transferred into a clean Conical flask by means of a Pipette.
3. 1 or 2 drops of methyl orange are added to the solution. The solution turns yellow in
colour.
4. The flask is placed under the burette on a glazed tile. The HCl is added slowly while
shaking the flask. The addition is continued till the color changes from yellow to
pink. It is the End Point. Just before the end point, any drops of the solution
adhering to inner walls of the flask are washed down into the flask with a few drops of
distilled water.
5. The final reading of the burette is noted. The difference between the two readings
gives the volumes of Hydrochloric acid rundown. The contents of flask are thrown
away.

6. Again 10 ml sodium carbonate solution is transferred to the flask and is titrated in a
similar way. The titrations are repeated till two consecutive reading coincide. The
readings are entered in a tabular form.
Observations & Calculations:

Volume of Na2CO3 Burette readings Volume of HCl \
S.No.
solution in ml. V2 Initial Final rundown V1 ml.
V1N1 = V2N2
V1 : Volume of Hydrochloric acid
N1 : Normality of Hydrochloric acid
V2 : Volume of Sodium Carbonate solution
N2 : Normality of Sodium Carbonate solution
V2 N 2
N1
V1
Amount of HCl present in 1 liter = Normality x Gram molecular weight of HCl.

= N1 x 36.5
Result: 1) The normality of the given HCl (N1) = N

2) Amount of HCl present in given 1 liter solution = gms

Expt.No:2
Date:
DETERMINATION OF TOTAL ALKALINITY OF WATER SAMPLE
Aim: To determine the total alkalinity of the given water sample by using 0.02N H2SO4.
Apparatus: Burette, Pipette, Conical Flask, Beakers, Wash Bottles, Burette Stand, Glazed
tile.
Chemicals Required: Standard H2SO4 solution, methyl orange indicator, phenolphthalein
indicator, water sample.
Chemical equations:
OH- + H+ H2O
2- +
CO3 + H HCO3-
HCO3- + H+ H2CO3 H2O+CO2
Theory:
The alkalinity of water is due to the presence of hydroxides, bicarbonates and
carbonates, and the total alkalinity is the sum of the alkalinities caused by one or more of
these present in the water sample.
Titration to pH=8.3 with phenolphthalein or the disappearance of pink colour will
indicate phenolphthalein alkalinity.
OH- + H+ H2O ------- 1
CO32- + H+ HCO3- ------- 2
Titration to pH=4.5with methyl orange or the appearance of pink colour will indicate
total alkalinity.
HCO3- + H+ H2CO3 H2O+CO2 ------ 3
Formula:
The amount of alkalinity interms of CaCO3 equivalents
Titre value Conc.of H 2 SO4 50 1000

= ppm
volume of sample(Vs )
Procedure:
Part-A: Phenolphthalein Alkalinity (or) Partial Alkalinity::
1. The burette is first cleaned with tap water and then with distilled water.
2. Finally, it is rinsed with given H2SO4 solution. Then it is filled with H2SO4 Solution.
3. The H2SO4 is allowed to run out to fill the nozzle portion without any air bubble.
4. The initial reading of the burette is adjusted to zero mark and fixed vertically to the
stand.
5. First the pipette is rinsed with distilled water.
6. Pipette out 20ml of water sample into a conical flask.
7. Add few drops of Phenolphthalein indicator.
8. The color of conical flask solution is pink.
9. Titrate water sample against H2SO4 solution until the color of the solution changes
from Pink to Colourless.
10. This is the endpoint of the titration.
11. The titrations are repeated until concurrent readings are obtained.
Part-B: Total Alkalinity:
2. Finally, it is rinsed with given H2SO4 solution. Then it is filled with H2SO4 Solution.
3. The H2SO4 is allowed to run out to fill the nozzle portion without any air bubble.
4. The initial reading of the burette is adjusted to zero mark and fixed vertically to the
stand.
6. Pipette out 20ml of water sample in to a conical flask.
7. Add few drops of methyl orange indicator.
8. The color of conical flask solution is yellow.
9. Titrate water sample against H2SO4 solution until the color of the solution changes
from yellow to pink.
11. The titrations are repeated until concurrent readings are obtained.
Observations and Calculations:

Determination of Phenolphthalein Alkalinity (or) Partial Alkalinity:
Volume of water Burette reading (ml) Volume of H2SO4 Solution

S.No.
sample (ml)Vs Initial Final run down V1ml
V1 0.02 50 1000
Phenolphthalein Alkalinity in terms of CaCO3equivalent = ppm
Vs
= .ppm
Determination of total alkalinity:
Volume of water Burette reading (ml) Volume of H2SO4Solution

S.No.
sample (ml) Vs Initial Final run down V2 ml
V2 0.02 50 1000
Total Alkalinity in terms of CaCO3 equivalents = ppm
Vs
= ..ppm
Result:
Phenolphthalein alkalinity of the given water sample= ------------------- ppm
Total alkalinity of the given water sample = ppm

Expt.No:3
Date:
DETERMINATION OF ACIDITY OF WATER SAMPLE
Aim: To determine the total acidity of the given water sample by using 0.02N NaOH
solution.
Apparatus: Burette, Pipette, Conical Flask, Beakers, Wash Bottle, Burette Stand.
Chemicals required: Standard sodium hydroxide(0.02N), Phenolphthalein indicator, Methyl
orange indicator, sodium thiosulphate, water sample.
Theory: The acidity of a solution is a measure of its capacity to neutralize bases.
Acidity is due to the presence of mineral acids like H2SO4, HCl, HNO3 and dissolved CO2 in
the form of H2CO3. These acids can be estimated by titration against standard sodium
hydroxide using methyl orange and Phenolphthalein indicators.If methyl orange indicator is
used in the titration (at pH=4.5), it gives acidity of mineral acids only. This acidity is called a
partial acidity or methyl orange acidity. If Phenolphthalein indicator is used (at pH=8.3) in
the titration, it gives acidity of all compounds(mineral acidity and CO2). This acidity is called
total acidity or Phenolphthalein acidity. The difference of these two is equal to carbonic
acid acidity. Interference due to the presence of residual Chlorine is removed by adding two
drops of Na2S2O3(hypo) solution to the water sample.
Procedure:
(A)Titration of water sample using Methyl orange indicator (Partial Acidity)
2. Finally, it is rinsed with given NaOH solution. Then it is filled with NaOH Solution.
3. The NaOH is allowed to run out to fill the nozzle portion without any air bubble.
4. The initial reading of the burette is adjusted to 0 mark and fixed vertically in the
stand.
7. Add 2 drops of hypo and two drops of methyl orange indicator.
8. The color of conical flask solution becomes pink.

9. Titrate water sample against NaOH solution until the color of the solution changes
from pink to Yellow.
Determination of Partial Acidity:
Volume of water Burette reading (ml) Volume of NaOH Solution

S.No.
sample (ml)Vs Initial Final run down V1 ml
Titre value conc.of NaOH 50 1000

Partial or Methyl Orange acidity in terms of CaCO3 equivalents =
volume of sample (Vs )
V1 0.02 50 1000
= ppm
20
= ppm or mg/litre.
(B)Titration of water sample using Phenolphthalein indicator (Total Acidity)

2. Finally, it is rinsed with given NaOH solution. Then it is filled with NaOH Solution.
3. The NaOH is allowed to run out to fill the nozzle portion without any air bubble.
4. The initial reading of the burette is adjusted to 0 mark and fixed vertically in the
stand.
7. Add 2 drops of hypo and two drops of Phenolphthalein indicator.
8. The color of conical flask solution is colourless.

9. Titrate water sample against NaOH solution until the color of the solution changes
from colourless to Faint pink.
Determination of Total Acidity:
Volume of water Burette reading (ml) Volume of NaOH Solution

S.No.
sample (ml) Vs Initial Final run down V2 ml
Total or Phenolphthalein acidity in terms of

Titre value conc.of NaOH 50 1000
CaCO3 equivalents =
volume of sample(Vs )
V2 0.02 50 1000
= ppm
20
= . ppm or mg/litre.
(C) Acidity due to carbonic acid=Total acidity-Partial acidity.
= ppm or mg/litre
Result:
Partial acidity of water sample =
Total acidity of water sample =
Carbonic acidity of water sample =

Expt.No:4
Date:
DETERMINATION OF FERROUS IRON BY PERMANGANOMETRIC

METHOD
Aim: To determine the Normality and amount of Ferrous Iron present in given 250ml
solution using Potassium Permangamate solution.
Apparatus: 1) Burette 2) Pipette 3) Conical flask 4) Beakers 5) Burette stand
6) Wash bottle 7) Glazed tile 8) Measuring jar
Chemicals required: 1. Standard Oxalic acid solution , 2. KMnO4 solution. 3. Dilute
H2SO4. 4. Mohrs salt solution.
Theory: Standardisation of KMnO4 solution is done by using standard oxalic acid solution
and then estimation of mohrs salt is done by using KMnO4 solution.
The chemical reaction is:
2 KMnO4 + 3 H2SO4 + 5 (COOH)2 K2SO4 + 2 MnSO4 + 8 H2O + 10 CO2
This is a redox titration. No external indicator is required. KMnO4 acts as self indicator.
Procedure:
1.Preparation of standard oxalic acid solution:
Accurately weigh the oxalic acid solid ( to prepare 0.05N) and transfer it to 250ml
volumetric flask. Dissolve the sample in little distilled water. Make up the solution with
distilled water till the lower meniscus of the solution touch the mark on the stem of the
standard flask, shake the flask well for uniform concentration.
Wt of oxalic acid transferred to 250ml volumetric flask= g

Wt.of oxalic acid 1000
Normality(N1) of oxalic acid=
g.equ. of oxalic acid V in ml
wt 1000

63 250
= N
2. Standardisation of KMnO4 solution:
Principle: KMnO4 is an oxidizing agent and it oxidizes oxalic acid in the presence of
dil.H2SO4 to CO2 and H2O. The chemical reaction involved in this redox titration.
2 KMnO4 + 3 H2SO4 + 5 (COOH)2 K2SO4 + 2 MnSO4 + 8 H2O + 10 CO2

1) Rinse and fill the burette with the given KMnO4 solution.
2) Rinse the pipette with the standard Oxalic acid solution and pipette out 10ml of it in a
washed conical flask.
3) Add 5ml of dilute Sulphuric acid to the solution with the help of measuring jar.
4) Heat the flask to 60 70oC and titrate the solution against KMnO4 in the burette till a
permanent pale pink color is obtained.
5) Note the burette reading and repeat the titration till two consecutive readings coincide.
Burette readings Volume of

Volume of
S.No. Initial Final KMnO4 rundown
Oxalic acid V1 (ml)
(ml) (ml) V2 (ml)
V1N1 = V2N2
Where V1 = Volume of Oxalic acid=10ml
N1 = Normality of Oxalic acid= N
V2 = Volume of KMnO4 solution= ml
N2 = Normality of KMnO4 solution=?
V1 N 1
N2
V2
= ...........N
Estimation of Mohrs salt solution.
Principle: Potassium Permanganate oxidizes Ferrous Sulphate present in the Mohrs salt in
the presence of dil.H2SO4 to Ferric Sulahate according to the following chemical reaction.
2KMnO4 + 8H2SO4 + 10FeSO4 K2SO4 + 2 MnSO4 + 5 Fe2(SO4)3 + 8H2O
1. Rinse and fill the burette with the standard KMnO4 solution till the upper meniscus of
the KMnO4 solution touches the zero mark on the burette.

2. Rinse the pipette with the given Mohrs salt solution and pipette out 10ml of it in a
washed conical flask.
3. Add 5ml of dilute Sulphuric acid to the solution in a conical flask.
4. Titrate the Mohrs salt solution against KMnO4 solution till the solution attains
permanent pale pink colour..
5. Note the final reading of the burette.
6. Repeat the titration till two consecutive readings coincide. Tabulate the readings.

Burette readings Volume of
Volume of
S.No. Initial Final KMnO4 rundown
Mohrsalt V3 (ml)
(ml) (ml) V2 (ml)
V3N3 = V2N2
Where V3 = Volume of Mohrs salt solution=10ml
N3 = Normality of Mohrs salt solution=?
V2 = Volume of KMnO4 solution=.. ml
N2 = Normality of KMnO4 solution= .. N
V2 N 2
N3
V3
Amount of Ferrous Iron present in the given 250 ml solution =
= N3 x g.equ. wt. of Iron x 250 / 1000
=. X 56 X 250 / 1000
Result: 1) The normality of the given Mohrs salt solution (N3) = .N
2) Amount of Ferrous Iron present in given 250 ml solution = g

Expt. No:5
Date:
ESTIMATION OF FERRIC IRON USING STANDARD K2Cr2O7

SOLUTION
Aim: To estimate the amount of ferric iron present in the given 100ml solution using
potassium dichromate as an intermediate solution.
Apparatus: weighing bottle, volumetric flask, funnel, burette, pipette, conical flask and
wash bottles.
Chemicals required: Ferric chloride salt, potassium dichromate, stannous chloride,
mercuric chloride, concentrated hydrochloric acid, concentrated sulphuric acid,
orthophosphoric acid and diphenylamine indicator
Determination of ferric iron:
Chemical reaction:
+ 6 + 14 6 +2 +7
Theory: Ferric ion is first reduced to ferrous ion with the help of stannous chloride.
2FeCl3 + SnCl2 2FeCl2 + SnCl4
The excess unreacted Stannous Chloride is oxidized by the addition of few drops of mercuric
chloride solution.
SnCl4 + 2HgCl2 SnCl4 + Hg2Cl2
The precipitated mercurous chloride settles down. Now the solution is titrated with standard
potassium dichromate solution and concentration of the ferric ion is estimated.
Estimation of Fe3+ present in given solution: Pipette out 10ml of ferric iron solution into a
clean conical flask. Add 5ml of concentrated hydrochloric acid and heat solution to boiling.
Now add stannous chloride solution drop wise until the solution becomes colorless. Cool the
solution under tap water. Now add, drop by drop, mercuric chloride solution until a white
silky precipitate is formed. Avoid adding excess of SnCl2. If excess has been added a grey
precipitate is formed, reject the solution and start the reduction process once again. Dilute the
solution to about 100ml with distilled water then add 5ml concentrated sulphuric acid and
2ml of phosphoric acid and 3 to 4 drops of diphenylamine indicator. Note down the initial
burette reading. Titrate the solution against standard potassium dichromate solution until
violet color persists. Note down the final burette reading. Repeat the titration for concurrent
readings.

Observations and calculations
S. Volume of Ferric Burette Volume of

No chloride salt readings K2Cr2O7
solution taken(ml) (ml) run
initial final down(ml)
1.
2.
3.
Volume of K2Cr2O7 salt solution = V1 = ml

Normality of K2Cr2O7 salt =N1 = .N
Volume of Ferric chloride salt solution = V2 = 20ml
Normality of Ferric chloride = N2 =?
N1V1 =N2V2
N2 =N1V1/V2
= ..N
Amount of Fe3+ present in the given 100 ml solution =
Gram euivalent wt. X Normality X Volume(ml)
1000
= = -----------g
Report: Amount of Fe3+ present in the given 100 ml solution = .g

Expt. No:6
Date:
ESTIMATION OF TOTAL HARDNESS OF WATER SAMPLE BY

EDTA METHOD
Aim: To determine the total hardness of the given water sample by using EDTA solution.
Apparatus: Burette, Pipette, Conical Flask, Beakers, Wash Bottles, Burette Stand, Glazed
Tile.
Chemicals required: Standard hard water solution(0.02N),Buffer (PH=10), EBT indicator,
EDTA solution
Introduction: Water is classified as soft water and hard water.
Soft water gives lather readily with soap. But hard water does not give lather readily with
soap due to dissolved salts like CaCl2, CaSO4, MgCl2, MgSO4, Ca(HCO3)2 and Mg(HCO3)2.
The Ca2+ or Mg2+ can be estimated by titrating with EDTA solution using Eriochrome
black-T indicator at range of pH=10.
Theory: Disodium salt of EDTA solution react with hard water to form complex with
EDTA solution. When the titration is carried out in the presence of Eriochrome black-T,
buffered to pH value 10, combines with Ca2+/Mg2+ to form a complex of wine red colour.
Chemical equations:
[Ca2+, Mg2+] + Eriochrome black-T [Ca2+,Mg2+ Eriochromeblack-T]
Hard water (Unstable and wine red color)
This when titrated with EDTA solution, quickly unstable complex dissociates and forms a
stable complex and complex free Eriochrome black-T indicator available in sky blue colour.
[Ca2+,Mg2+ Eriochrome blck-T] + EDTA [ Ca2+,Mg2+ EDTA] + EBT
wine red (Stable and colorless) (blue)
Change of wine red colour to sky blue indicates the end point of titration. From the value of
EDTA solution consumed, the total hardness of water can be calculated in terms of CaCO3
equivalents
1.Standardisation of EDTA solution:
Procedure:
1. Rinse and fill the burette with the given EDTA solution.
2. Transfer 20ml of standard hard water sample into a clean conical flask.

3. Add 1ml of pH=10 buffer (NH4Cl+NH4OH buffer) solution and 1 or 2 drops of EBT
indicator. Solution turns to wine red colour.
4. Titrate with EDTA solution till wine red colour changes to sky blue. This is the end
point.
5. Repeat the titration until two consecutive readings coincide.
Volume of Burette reading (ml)

standard hard Volume of EDTA rundown
S.No.
water sample Initial Final (V2ml)
(v1ml)
V1N1 = V2N2
V1= Volume of standard hard water =20ml
N1= Normality of standard hard water =0.02N
V2= Volume of given EDTA solution=ml
N2= Normality of given EDTA solution=?
V1 N1
N2=
V2
=
2. Determination of Total Hardness of the given water sample
1. Fill the burette with the EDTA solution.
2. Transfer 20ml of the given water sample into a clean conical flask.
3. Add 1ml of pH=10 buffer solution and 1 or 2 drops of EBT indicator. Solution
turns to wine red colour
4. Titrate with EDTA solution till wine red colour changes to sky blue. This is
the end point.
5. Repeat the titration until two consecutive readings coincide.

Volume of Burette reading (ml)

standard hard Volume of EDTA rundown
S.No. water sample Initial Final (V2ml)
(V3ml)
V3 N3 = V2 N2
V3= Volume of given water sample =20ml
N3= Normality of given water sample =?
V2= Volume of EDTA solution run down=ml
N2= Normality of given EDTA solution=.N
V2 N 2
N3=
V3
=
Total degree of hardness of the given water

sample in terms of CaCO3 equivalents = Normality(N3) 50 1000
= . ppm
Result:
Total degree of hardness of the given water sample is .mg /l(or) ppm

Expt.No:7
Date:
PH-METRIC TITRATION: DETERMINATION OF CONCENTRATION OF HCl
USING GLASS ELECTRODE
Aim: To determine the concentration of unknown HCl by using 0.1N NaOH solution pH
metrically.
Apparatus: pH meter, electrode, beaker, pipette, burette.
Chemicals required: Hydrochloric acid (HCl), 0.1N sodium hydroxide (NaOH). Buffer
solutions of pH = 4 and 7.
Theory: All acids dissociate in aqueous solution to yield H+ ions. Some acids like HCl,
H2SO4, HNO3 etc. are completely ionized in aqueous medium where as CH3COOH, HCOOH
etc. ionize to a small extent only. The former is known as strong and the later as weak acid.
pH of any solution is defined as (log [H+]) and has values between 014. pH < 7 indicate
acidic solution, pH > 7 indicate basic solution and pH = 7 means neutral solution.
The pH of a solution can be measured accurately with the help of a pH meter. Measurement
of pH is employed to monitor the cause of acid-base titration. The pH values of the solution
at different stages of acidbase neutralization are determined and plotted against the volume
of alkali added. On adding a base to an acid, the pH rises slowly in the initial stages as the
concentration of H+ ion decreases gradually. But, at the equivalence point, it increases rapidly
as at the equivalent point H+ ion concentration is very small. Then it flattens out after the end
point. The end point of the titration can be detected where the pH value changes most rapidly.
Procedure: Switch on the instrument and wait for 1015 minutes so that machine gets
warmed up. Prepare the buffer solution by adding buffer tablets of pH = 4 and pH = 7 in 100
mL of water separately. Wash the electrode with distilled water and calibrate the pH meter as
per the instruction manual.
Clean the electrode with distilled water and wipe it with a tissue paper or filter paper. Take
20 mL of HCl solution in a 100 mL beaker and immerse the electrode in it. 0.1N NaOH
solution is filled in the burette . The reading shown on the scale of pH meter is pH value of
the HCl solution. Add NaOH solution drop wise from the burette (maximum 1mL at a time),
shake the solution well and note the corresponding pH values. Near the end point, the acid is
neutralized and there will a sharp increase in pH values. Further addition of even 0.01 mL of
NaOH, increase the pH value to about 910.
Plot a graph between pH and volume of NaOH added and find out the volume of NaOH
required (V2 mL) for complete neutralization of HCl from the graph.
V1N1=V2N2
Normality of HCl (N1) = (V2N2/20) (N)
Result: The concentration of the unknown HCl is ________(N)
Precautions: i) Electrodes must be immersed in the solution properly and sufficient time
to be allowed for the electrodes to obtain the temperature of the solution.
i) pH meter should be calibrated before the experiment.
i) Magnetic stirrer may be used or the solution be stirred mechanically from time to
time during pH metric titration.

Expt.No:8
Date:
DETERMINATION OF pH OF THE GIVEN WATER SAMPLE
Aim: To determine the pH of the given water sample using pH meter.

Apparatus: Digital pH meter, combined electrode, beakers.
Chemicals required: Standard buffer solution (pH =4; pH =7), distilled water, water
sample.
Theory: pH is defined as the negative logarithm of the H+ ion concentration.
pH = -log[H+]
where H+ is the concentration of hydrogen ion expressed in moles/litre
pH value indicates whether a solution is acidic or neutral or basic.
If pH is between 0 to 7, it indicates acidic solution.
If pH is in between 7to 14, it indicates basic solution.
If pH is exactly 7, it indicates neutral solution.
pH is determined by using pH meter which contains glass electrode which is
sensitive to H+ ions.
Preparation of Buffers:
i) Dissolve a pH =4 buffer tablet in 100ml distilled water. It indicates the standard solution of
pH =4
ii) Dissolve a pH=7 buffer tablet in 100ml distilled water. It indicates the standard solution of
pH =7
Procedure:
Calibration of pH meter:
i) Set the temperature knob to buffer solution temperature.
ii) Dip the electrode in buffer solution of pH =7.
iii) Set the display value to pH =7 by turning CAL knob.
iv) Wash the electrode with distilled water and dry with the tissue paper.
v) Dip the electrode in the buffer solution of pH=4 and set the slope button to display 4.
vi) Now the instrument is ready to measure pH .
Measurement of pH:
i) Wash the electrode with the distilled water and dry with tissue paper.

ii) Dip the electrode in the sample water to be analyzed.
iii) The reading obtained is the pH value of sample.
iv) Rinse the electrode before and after measurement of each sample.
Precautions:
a) The pH electrode should be handled gently
b) The electrode should be always dipped in distilled water when not in use
Significance:
As per Indian standards the pH of the drinking water should be between 6.5-8.5 . As per
WHO standards, the pH of the drinking water should be between 7.0-8.0 .
Report: The pH of the given water sample is

Expt.No:9
Date:
DETERMINATION OF CONDUCTIVITY OF WATER SAMPLE
Aim: To determine the conductivity of the given water sample by using conductivity meter.
Apparatus: Conductivity meter.
Reagent: Standard electrical conductivity solution.
Standard solution is prepared by dissolving 0.7456grams of KCl in 1 litre distilled
water. It will have 1413 mhos/cm as conductance.
Theory: Conductivity is the capacity of the water to carry an electrical current.
Conductivity is proportional to the concentration of dissolved solids(ions) in the
solution.
Procedure:
Calibration of electrical conductivity meter:
(i) Adjust cal till the display reads 1000.
(ii) Set the Range switch to the proper range for the standard solution.
(iii) Change the cond/cell constant switch position to cell constant position.
(iv)Wash the electrode with distilled water and dry with tissue paper. Immerse the electrode
in standard solution.
(v) Adjust the cell constant present control on the rear panel till the instrument reads 1. The
conductivity of the solution is1413s/cm.
Measurement of conductivity:
(i) Wash the electrode with distilled water and dry with tissue paper.
(ii) Dip the electrode in 50ml sample for which conductivity is to be measured.
The reading indicated on the meter is the conductivity of the sample.
(iv) Rinse the electrode before and after measurement of conductivity of each sample.
Significance: Conductivity increases as the dissolved ionic species in water increases.
According to Indian standards, the conductivity should be inbetween 5-50mS/m.
Report: The conductivity of the given water sample is

Expt.No:10
Date:
CONDUCTOMETRIC TITRATION BETWEEN STRONG ACID AND

STRONG BASE
Aim: To determine the amount of the given HCl present in the given one litre solution by
using 0.1N NaOH solution conductometrically.
Apparatus required: Conductometer, Conductivity cell, Magnetic stirrer/ Glass stirrer,
beaker, burette and pipette.
Chemicals required: NaOH solution, HCl solution and distilled water
Principle: According to Kohlrauschs law, the electrical conductance of a solution depends
upon the number and mobility of ions.For the titration of a strong acid like HCl against a
strong base like NaOH, before the NaOH solution is added, the acid solution has a high
conductance due to the highly mobile hydrogen ion. As alkali solution is added the hydrogen
ions are removed due to combination with the hydroxyl ions forming feebly ionized water
(H2O) molecules and their place is taken by the much slower moving Na+ ions.
+ + ( )
Consequently the conductance of the solution decreases and continues to decrease on adding
sodium hydroxide solution until equivalence point is reached. Any further addition of alkali
means increase of Na+ and fast moving hydroxyl ions and thus the conductance begins to
increase. If we plot the conductance measured against the volume of NaOH added, the point
of intersection will give the neutralization point.
Significance:
Titrations involving coloured liquids are difficult to be performed using ordinary indicators.
But these can be easily carried out by conductometric titration method. Moreover,
conductometric titration can be performed accurately even with dilute solutions
Procedure:
1. Wash the conductivity cell thoroughly with distilled water and calibrate the
instrument to its cell constant vaue.
2. Take 20 ml of the given HCl solution whose strength is to be determined in a 100 ml
beaker.

3. Clamp the conductivity cell in the beaker containing the acid solution.
4. Set the function switch to Cond. position.
5. Fill the NaOH solution in the burette.
6. Note down the conductance from the conductometer.
7. Keep on adding NaOH from the burette, 1mL at a time.
8. Stir the solution with magnetic stirrer or a glass rod and measure the conductance.
Graph: The values of observed conductance are plotted along Y axis against the volume of
NaOH added along the X axis.
The point of intersection gives the amount of NaOH required for neutralization of the HCl.

Observations and calculations:
Volume of NaOH
S.No. consumed Conductance (C)
v (ml)
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
N1V1 = N2V2
Volume of unknown HCl solution taken (V1) = 20ml
Normality of HCl(N1)=?
Volume of NaOH at end point (from graph) =.V2 ml
Normality of NaOH(N2)=0.1N
N1= 0.1V2/20
Amount of HCl present in given one litre solution = Normality X gram equivalent wt. of HCl
= N1X 36.5
= g/L
Result:
The amount of HCl present in the given one litre solution = . g.
Expt.No:11
Date:
DETERMINATION OF TURBIDITY OF WATER SAMPLE
Aim: To determine the Turbidity of the given water sample using Turbidity meter.
Apparatus: Nephelometer.
Reagents:
Solution-1: Dissolve 1g of Hydrazine sulphate in 100ml distilled water.
Solution-2: Dissolve 10g of Hexamethylene tetramine in 100ml of distilled water.
Solution-3: Mix 5ml of solution-1 and 5ml of solution-2 in a 100ml volumetric flask. Allow
to stand for 24hrs. Dilute it to 100ml. Now the solution has a known turbidity of 400NTU.
From this stock solution, dilution is carried out to obtain lower
concentrations of 100, 40, 20 and 10 NTU.
Theory: Turbidity is a measure of cloudiness. Turbidity is the property of water because of
which it offers resistance to passage of light. It is caused by suspended solids, living or dead
micro-organisms etc.
The turbidity is measured from the amount of light scattered by the sample taking a
reference with standard turbidity suspension.
Procedure: Calibration of Nephelometer:
i) Select the appropriate range
ii) Insert the test tube( cuvette) with distilled water into cell holder and cover with light
shield.
iii) Adjust zero button to get zero an the display
iv) Take the standard solution of 100 NTU in the test tube and adjust calibration as 100
Measurement of Turbidity:
i) Rinse the test tube before and after measurement of each sample with distilled water and
dry it with a tissue paper.
ii) Take unknown sample of water in the test tube upto the mark indicated on it and place it
in the holder. The display directly gives the turbidity in NTU.
Significance: As per WHO standards, the turbidity of drinking water should be less than 5
NTU.
Report: The turbidity of the given water sample is .NTU

Expt.No:12
Date:
ESTIMATION OF TOTAL DISSOLVED SALTS IN WATER SAMPLE
Aim: To estimate the amount of total dissolved salts present in the given water sample.
Apparatus: China dish, analytical balance, measuring jar, hot air oven, water bath,
dessicator.
Principle: Water may contain dissolved salts like bicarbonates, chlorides, sulphates of
calcium, magnesium, sodium, potassium, iron etc.
The total dissolved salts in a water sample is estimated by evaporating in a
weighed dish and drying it at a constant temperature of 103C to 105C. The increase in
weight over that of the empty dish represents the total dissolved salts.
Procedure:
1. Take a clean and dry china dish, weigh it (W1).
2. Take 50ml of the given water sample with the help of measuring jar into the china
dish.
3. Evaporate the water to drying on a steam bath.
4. Keep the dish in hot air oven at 103C to remove the residual water.
5. Cool the dish in a desiccator to room temperature.
6. Then weigh the dish along with the residue (W2).
Observations and calculations:

W1 = Weight of the empty china dish =
W2 = Weight of the dish along with the residual =
V = Volume of water taken = 50 ml.
W2 W1
Total dissolved salts = 10 6 ppm
V
Significance:
Many dissolved salts cause displeasing taste, colour.
Estimation of total dissolved salts is useful to determine whether the water is useful for
agriculture , industrial purpose or not. In industries the use of water with high amount of salts
will lead to scaling, corrosion in boiler.
Result: The total dissolved salts present in the given water sample is

Expt.No:13
Date:
PREPARATION OF PHENOL- FORMALDEHYDE RESIN

Aim: To prepare Phenol- Formaldehyde resin and calculate the yield of the product.
Apparatus: Beaker, Glass rod, Funnel
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.
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 and weighed.
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 amount of Phenol Formaldehyde resin prepared= . grams

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GUDLAVALLERU ENGINEERING COLLEGE

(An Autonomous Institute Affiliated to JNTUK, Kakinada)

I B.TECH. R14 REGULATION

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 1

1) Practice experiment-Determination of the amount of HCl using standard Na2CO3.

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 2

INTRODUCTION TO CHEMISTRY LAB

Analytical chemistry is mainly divided into two.

Quantitative chemical analysis is further divided into two types.

Terms used in Volumetric Analysis:

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 3

No. of gm. equivalents . of Solute

Weight of Solute 1000

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 4

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 5

Working of acid base indicator:

Example Colour change pH range

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 6

Working of indicator in Complexometric titration:

EBT + M2+ (Ca2+, Mg2+) (EBT) M2+

(EBT) M2+ + EDTA (EDTA) M 2+ + EBT

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 7

K2CrO4 + 2AgNO3 2KNO3 + Ag2CrO4

Working of indicator in Redox Titrations:

A. Redox titrations Using Colored Titrant

6 Fe+2 + 14 H+ + Cr2O7-2 6 Fe+3 + 2 Cr+3 + 7 H2O

5 Fe+2 + MnO4- + 8H+ 5 Fe+3 + Mn+2 + 4 H2O

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 8

ESTIMATION OF HYDROCHLORIC ACID

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 9

Observations & Calculations:

Amount of HCl present in 1 liter = Normality x Gram molecular weight of HCl.

Result: 1) The normality of the given HCl (N1) = N

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 10

OH- + H+ H2O ------- 1

CO32- + H+ HCO3- ------- 2

HCO3- + H+ H2CO3 H2O+CO2 ------ 3

Titre value Conc.of H 2 SO4 50 1000

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 12

Volume of water Burette reading (ml) Volume of H2SO4 Solution

Volume of water Burette reading (ml) Volume of H2SO4Solution

Total alkalinity of the given water sample = ppm

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 13

DETERMINATION OF ACIDITY OF WATER SAMPLE

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 14

Observations and Calculations:

Determination of Partial Acidity:

Volume of water Burette reading (ml) Volume of NaOH Solution

Titre value conc.of NaOH 50 1000

(B)Titration of water sample using Phenolphthalein indicator (Total Acidity)

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 15

Observations and Calculations:

Determination of Total Acidity:

Volume of water Burette reading (ml) Volume of NaOH Solution

Total or Phenolphthalein acidity in terms of

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 16

DETERMINATION OF FERROUS IRON BY PERMANGANOMETRIC

Wt of oxalic acid transferred to 250ml volumetric flask= g

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 17

Burette readings Volume of

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 18

Observations & Calculations:

P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 19