Department of Applied Chemistry

Delhi Technological University

PRACTICALS (PRS 15%)

Objective: To make the student aware about the practical aspects of theory, improve their
analytical knowledge and develop ability to do work patiently.

List of Chemistry Experiments for B. Tech. 1st year students

(At least 10 experiments should be performed by the students)
1. To determine the strength of commercial hydrochloric acid, 10 ml of which have
been dissolved per liter of the given solution using sodium carbonate solution.
2. To determine the strength of Sodium hydroxide and Sodium carbonate from given
water sample using methyl orange and phenolphthalein as indicator. Given
standard N/40 Sodium carbonate to standardize HCl solution.
3. To determine the amount of permanent, temporary and total hardness of given
water sample using standard N/50 disodium salt of EDTA solution.
4. To determine the strength of free chlorine in given water sample. Given standard
N/40 copper sulphate (CuSO4) solution to standardize sodium thiosulphate
solution.
5. To determine the concentration of dissolved oxygen from the given water sample
using standard N/40 Na2S2O3 solution.
6. To analyze and interpret the given IR spectrum 1.
7. To analyze and interpret the given IR spectrum 2.
8. To determine the total alkalinity of given water sample using methyl orange as
indicator. Given standard N/40 Sodium carbonate to standardize HCl solution.
9. To determine the structure of an unknown compound A using Spectroscopic data.
10. To determine the structure of an unknown compound B using Spectroscopic data.

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Experiment No. 1:
To determine the strength of commercial hydrochloric acid, 10 ml of which have been
dissolved per litre of the given solution.
Apparatus required: Burette, pipette, conical flasks, stand, clamps, funnel etc.
Chemicals required: Sodium carbonate solution, HCl solution, methyl orange solution.
Theory: Commercial HCl is an aqueous solution of HCl gas. In order to determine the
strength of HCl, it is titrated against aqueous sodium carbonate solution. This is an
example of neutralization titration.
Methyl orange is used as an indicator during the titration. It changes colour from yellow
to red at the end point.
Reactions: HCl + Na2CO3 NaHCO3 + NaCl
NaHCO3 + HCl NaCl + H2O + CO2
Ionically: CO3-2 + H+ HCO3-
HCO3- + H+ H2O + CO2
End point: Yellow to red (acid solution in the burette).

NaO3S N N N(CH3)2

Methyl Orange
Procedure:
(i) Rinse and fill the burette with given acid solution.
(ii) Remove the air bubbles and set it at zero mark.
(iii) Pipette out 20 mL of the standard Na2CO3 solution into the titration flask and add
2 or 3 drops of methyl-orange.
(iv) Titrate with the HCl to a sharp colour change i.e., till red colour is obtained.
(v) Repeat the titration with every 20 mL of the Na2CO3 solution until three
concordant readings are obtained.

Observations:
Volume of Na2CO3 solution taken for each titration = 20 mL
Burette readings: Titration of Na2CO3 vs HCl

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Table: Titration of Na2CO3 vs HCl

S. No. Initial Reading Final Reading Vol. of HCl

Calculations:
Normality of Na2CO3 solution = NNa2CO3
To calculate normality of dil HCl solution, apply normality equation
NHCl x VHCl = NNa2CO3  VNa2CO3
or NHCl = NNa2CO3  VNa2CO3 / VHCl
= NNa2CO3  20 / VHCl
Strength of dil HCl solution = NHCl x 36.5 g/L (strength = Normality  Eq. wt.)
Since, commercial HCl was diluted 100 times (10 mL in 1000 mL), the strength of
commercial HCl can be obtained by multiplying the strength of dil. HCl by 100.
Hence, strength of commercial HCl = NHCl  36.5  100 g/L
Result:
Strength of commercial HCl is …………………. g/L
Precautions:
a) Shake the titration flask continuously during adding the solution from the burette.
b) Keep your eye in level with the liquid surface while taking the burette reading or
while reading the pipette or measuring flask etc.
c) Always read lower meniscus in case of colourless solution.

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Experiment No. 2
To determine the strength of Sodium hydroxide (NaOH) and Sodium carbonate (Na2CO3)
from given water sample. Given standard N/40 Sodium carbonate to standardize given
HCl solution.
Apparatus required: Burette, pipette, conical flask, funnel, conical flask, measuring
cylinders.
Material required: Sodium carbonate (N/40) solution, HCl solution, Phenolphthalein
(P), Methyl orange (M) and water sample.
Theory
The ionic equations involved for this reaction are:
(i) OH- + H+ H2O Phenolphthalein
(ii) CO3-2 + H+ HCO3-
(iii) HCO3- + H+ H2O + CO2 Methyl orange

The titration is based upon the specific pH range for each indicator. The
phenolphthalein indicator gives pink colour in pH range 8.2 – 10 while methyl orange
gives pink colour in pH range 4.4 – 3.0. It has been observed that the presence of sodium
hydroxide and sodium carbonate always provide a pH higher than 8.2 to the solution.
Initially when standard hydrochloric acid is added, the OH- ions are first converted to
H2O and then CO3-2 ions are converted to HCO3-. When first two steps [(i) and (ii)]
completed the pH of solution becomes less than 8.2 and the pink colour of
phenolphthalein disappears. At this point, methyl orange is added as indicator to find the
complete neutralization. On addition of further acid, the HCO3- ions are converted to CO2
and H2O. It means step (iii) is completed. When all HCO3- ions are used up the pH of
solution becomes less than 4.4 instantaneously. At this point methyl orange gives pink
colour.

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Procedure:
1. Standardization of given HCl solution
(i) Take 10 mL of standard Na2CO3 with the help of pipette into a conical flask. Add
1-2 drops of methyl orange.
(ii) Run the acid solution from the burette into conical flask drop wise with constant
shaking of solution. Find the end point when light yellow colour solution turns
pink. Note volume of acid used. Repeat this step 4-5 times till you get at least two
concordant readings.
II. Titration of given water sample with HCl solution
(i) Pipette out 10 mL of given water sample into a conical flask. Add 2-3 drops of
phenolphthalein indicator. The solution turns pink.
(ii) Add HCl solution from burette into the conical flask with constant shaking till the
pink colour disappears. Note the reading on the burette (V1).
(iii) After discolouration, add 1-2 drops of methyl orange into the solution.
(iv) Titrate now again with acid till yellow coloured solution turns pink again. Note
the volume of acid used (V2). Repeat the steps to get concordant readings.

Observation Table: Standardization of given HCl solution

S.No. Volume of Burette Readings Volume of Concordant
Na2CO3 HCl used reading (Vo)
taken (mL) Initial Final (mL) (mL)

Observation Table: Titration of given water sample with HCl solution

S.No. Volume of Burette Readings Volume of HCl Concordant
Sample taken (mL) used (mL) reading (Vo)
(mL) (mL)
Initial Final
P M P M

V1 V3 = P = ….(V1)

V2-V1 M = …. (V3)

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Calculations
Normality of given HCl solution (NHCl) = (NNa2CO3 × V Na2CO3)/VHCl
V1 = Volume of HCl when whole of NaOH and half of carbonate is neutralized
 [OH-] + ½[CO32-] and V3  ½[CO32-]
Hence, Volume of HCl required for the neutralization of NaOH = V1-V3
Volume of HCl required for the neutralization of Na2CO3 = 2V3
Normality of NaOH in given solution (NNaOH) = (NHCl × V1-V3)/10
Normality of Na2CO3 in given solution (NNa2CO3) = (NHCl × 2V3)/10
Strength of NaOH in given solution = NNaOH × Equivalent wt of NaOH g/L
Strength of Na2CO3 in given solution = NNa2CO3 × Equivalent wt of Na2CO3 g/L

Result:
Strength of NaOH in given solution = ………………. g/L
Strength of Na2CO3 in given solution = ……………….. g/L

Precautions:
(i) Before starting the experiment, the glass apparatus must be perfectly cleaned.
(ii) For each titration, the initial reading of burette should always be the same.
(iii) Always read lower meniscus of solution level in burette.
(iv) Near the end point, add acid solution dropwise and after addition of each drop, see
the colour against white background.
(v) Do not blow last drop of solution from pipette. Just tap the tip of pipette to the
walls of the flask.

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Experiment No. 3
To determine the amount of permanent, temporary and total hardness of given water
sample using standard N/50 EDTA solution.
Apparatus Required: Standard flasks, burette, conical flasks, pipette, etc.
Chemicals Required: Water, EDTA solution, Eriochrome black T, buffer.
Theory: Water that doesn’t produce lather with soap solutions rather produces white
precipitate or scum is known as hard water. Hardness of water is due to the presence of
calcium and magnesium salts in the form of bicarbonate, chloride and sulphate in water.
There are two types of hardness present in water: temporary hardness and permanent
hardness. Temporary hardness can be removed by boiling the water or by the addition of
lime (or calcium hydroxide).
The amount of permanent, temporary and total hardness of water is easily
determined by complexometric titration using disodium salt of EDTA solution.
Eriochrome black T (EBT) is used as indicator.

EBT

HOOCCH2 CH2COOH

N CH2 CH2 N

HOOCCH2 EDTA CH2COOH

Procedure:
Total Hardness of the Water Sample
1. Pipette 20 mL of the water sample into a 250 mL conical flask. Add 2-3 mL of pH
10 ammonical buffer and 1 drop of EBT indicator. You will get a wine red color
solution.

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2. Titrate the water sample with EDTA solution until the color changes from wine red
to blue. Record the volume.
3. Repeat this two more times till you get concordant readings.

Permanent Hardness
1. Transfer a 100 mL water sample into a 250 mL beaker. Gently boil the water for 30
minutes. Allow the boiled water to cool to room temperature.
4. Filter the water directly into a clean 100 mL volumetric flask. Fill the volumetric
flask to the mark with distilled water.
5. Pipet 20 mL of the filtered sample into a flask and add 2-3 mL of pH 10 ammonical
buffer and 1 drop of EBT indicator.
6. Titrate the water sample with EDTA solution until the color changes from wine red
to blue. Record the volume.
7. Repeat this two more times till you get concordant readings.
Observation Table Titration of given water sample against EDTA solution for total
hardness
S. No. Initial burette Final burette Volume of given Na2EDTA solution
reading = V1 mL reading = V2 mL used = (V2-V1) mL

Observation Table
Titration of given water sample against EDTA solution for permanent hardness
S. No. Initial burette Final burette Volume of standardized EDTA solution
reading = V1 mL reading = V2 mL used = (V2-V1) mL

Calculations:
The hardness can be calculated using the normality equation:
Nwater  Vwater = NEDTA  VEDTA
NEDTA = Normality of Na2EDTA solution = N/50
VEDTA = Volume of Na2EDTA solution used = From observation table.
Vwater = Volume of the given water sample to be analyzed = 10 mL
Substituting these values in the normality equation, we can calculate the normality of the
given water sample.

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Total Hardness or hardness of water is calculated with respect to the CaCO3 only. Thus,
hardness of given water sample is Nwater × Eq. Wt of CaCO3 = …..g/L
= Nwater × Eq. Wt of CaCO3  1000 = mg/L or ppm
For permanent hardness, repeat the calculation taking volume of Na2EDTA solution used
from observation table.
Result:
(i) Total Hardness = …….. g/L or ppm
(ii) Permanent Hardness = …….. g/L or ppm
(iii) Temporary Hardness = Total hardness – Permanent hardness = …… g/L or ppm.
Precautions:
(i) Before starting the experiment, the glass apparatus must be perfectly cleaned.
(ii) Always read lower meniscus of solution level in burette.
(iii) Near the end point, add EDTA solution drop wise and after addition of each drop,
see the colour change.
(v) Do not blow last drop of solution from pipette. Just tap the tip of pipette to the
walls of the flask.

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Experiment No. 4
To determine the strength of free chlorine in given water sample. Given standard N/40
copper sulphate (CuSO4) solution to standardize sodium thiosulfate solution.
Apparatus required: Burette, Pipette, Measuring flask, glass rod
Reagents required: Potassium iodide solution (10%), N/40 Hypo solution (Na2S2O3),
starch solution (freshly prepared).
Theory: Chlorine is widely used for disinfection of potable and municipal water supplied
to remove bacteria, fungus and other pathogenic micro–organisms, and for
deodourization, since it is a powerful oxidizing agent and is cheaply available.
Chlorination is done with the help of bleaching powder or chlorine gas or chlorine
dissolved in water in the form of concentrated solution or with chloramines. The
sterilizing action of chlorine is supposed to be due to its reaction with water producing
hypochlorous acid and nascent oxygen both of which have powerful germicidal
properties.
The principle involved in the estimation of free chlorine in water is that when a
measured quantity is treated with excess of potassium iodide, the free chlorine present in
the water oxidizes the corresponding amount of potassium iodide to iodine. The liberated
iodine is estimated by titrating against standard hypo solution, using starch as indicator.
Cl2 + 2KI 2KCl + I2
I2 + 2Na2S2O3 Na2S4O6 + 2NaI
Sodium thiosulphate Sodium tetrathionate
I2 + Starch indicator Blue colour

Procedure:
Part I: Standardization of hypo solution with given copper sulphate solution
(i) Take 10 ml of given copper sulphate solution (CuSO4) from pipette in conical flask.
(ii) Add 1 ml of potassium iodide (KI) solution and titrate with the hypo solution till faint
yellow colour develops. At this point, add 1-2 drop of starch as indicator. The solution
will turn blue in colour. Titrate further with hypo to colourless as end point. Note the
concordant volume of hypo solution as V mL.

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Part II: Titration of given water sample with hypo solution

(i) Take 10 ml of given water sample from pipette in a conical flask.
(ii) Add 1 ml of potassium iodide (KI) solution and titrate with the hypo solution till
faint yellow colour develops. At this point, add 1-2 drop of starch as indicator.
The solution will turn blue in colour. Titrate further with hypo to colourless as end
point. Note the concordant volume of hypo solution as V mL.
Observations
Table: Titration of hypo solution versus given CuSO4 solution
S.No. Volume of Burette Readings Volume of Concordant
CuSO4 hypo used reading (V)
solution (mL) Initial Final (mL) (mL)

Table: Titration of hypo solution versus given CuSO4 solution

S. No. Volume of Burette Readings Volume of Concordant
water hypo used reading (V)
sample (mL) Initial Final (mL) (mL)

Calculations
Part I: Normality of CuSO4 solution (N1) = N/40
Volume of CuSO4 solution (V1) = 10 ml
Normality of hypo solution (N2) = ?
Volume of hypo solution (V2) = burette reading
N1 V1 = N2 V2 will give the normality of hypo solution (N2)
Part II: Volume of water sample taken for each titration (V3) = 10 mL
Normality of water sample (equivalent to dissolved chlorine) (N3) = ?
Normality of hypo solution (N2) = ?
Volume of hypo solution (V2) = burette reading
N2 V2 = N3 V3 will give the normality of water sample (N3)
Total chlorine residuals = N3 × Equivalent wt of chlorine (35.5) g/L
Convert g/L into ppm.
Result: Amount of total residual chlorine in a given sample of water = ............. ppm

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Precautions:
1. The solution being unstable should be titrated immediately after its preparation.
2. The solution should be well shaken before each aliquot is withdrawn for titration.
3. Chlorine vapours being harmful, the solution should not be sucked into the pipette
with the mouth.

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Experiment No. 5
To determine the concentration of dissolved oxygen from the given water sample using
standard N/40 Na2S2O3 solution.
Apparatus required: Burette, Pipette, Measuring flask, glass rod
Chemicals required: Potassium iodide solution (10%), N/40 Hypo solution (Na2S2O3),
starch solution (freshly prepared).
Theory:
The experiment is based on the oxidation of potassium iodide by the dissolved oxygen.
The liberated iodine is titrated against a standard sodium thiosulphate solution using
starch as final indicator. Since, oxygen dissolved in water remains present in molecular
state; it is not capable of reacting with potassium iodide. An oxygen carrier such as
manganese hydroxide is, therefore, used to bring about the reaction. Manganese
hydroxide is produced in situ by the action of potassium hydroxide and manganous
sulphate. The chemical reactions taking place are as follows:
MnSO4 + 2KOH →
Mn(OH)2 + K2SO4
2Mn(OH)2 + O2 →
2MnO(OH)2
[Basic manganese oxide]
MnO(OH)2 + H2SO4 → MnSO4 + 2H2O + [O]
2KI + H2SO4 + [O] → K2SO4 + H2O + I2
I2 + 2Na2S2O3 → 2NaI + Na2S4O6
(Sodium tetrathionate)
Procedure: Take 100 mL water sample in iodometric flask; avoiding, as far as possible,
contact with air. Immediately add 1 mL of manganous sulphate solution from the burette
and 1 mL of alkaline iodide from the other burette. Insert the stopper and shake several
times. Allow the precipitate to settle half way and mix again. Repeat this process of
shaking and settling at least three times. Add 1 mL of conc. sulphuric acid. Insert the
stopper and shake again. Allow the yellow solution to stand for 5 min. Withdraw 100 mL
of the solution. Titrate it against the standard N/40 sodium thiosulphate solution till the
colour of the solution becomes faint yellow. At this stage add a few drops of starch
solution. The colour turns to deep blue due to the formation of starch – iodide. Continue
the titration till the solution becomes colourless.

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Observations:
Volume of water for each titration = 100 mL
Volume of N/40 sodium thiosulphate solution = V mL
Calculations:
100 mL of water sample  V mL of N/40 Na2S2O3 solution
Normality = V/ 100  40
Strength = V  8 / 100  40 gm. of O2/ litre
V  8 / 100  4  1000 ppm
Amount of dissolved oxygen = .......... ppm
Result: Dissolved oxygen = ................ ppm

Precautions:
1. The solution in the iodine flask should be shaken carefully while keeping the
thumb on the lid.
2. The solution should be well shaken before each aliquot is withdrawn for titration.
3. The solution in the iodine flask should not be sucked into the pipette with the
mouth.

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Experiment No. 6 and 7

To analyze and interpret the given IR spectrum.
Requirements: IR spectrum
Theory:
The qualitative aspects of infrared spectroscopy are one of the most powerful
attributes of this diverse and versatile analytical technique. The vibrational spectrum of a
molecule is considered to be a unique physical property and is characteristic of the
molecule. The infrared spectrum can be used as a fingerprint for identification by the
comparison of the spectrum from an ‘‘unknown’’ with previously recorded reference
spectra. This is the basis of computer-based spectral searching. In the absence of a
suitable reference database, it is possible to effect a basic interpretation of the spectrum
from first principles, leading to characterization, and possibly even identification of an
unknown sample.
This first principles approach is based on the fact that structural features of the
molecule, whether they are the backbone of the molecule or the functional groups
attached to the molecule, produce characteristic and reproducible absorptions in the
spectrum. This information can indicate whether there is backbone to the structure and, if
so, whether the backbone consists of linear or branched chains. Next it is possible to
determine if there is unsaturation and/or aromatic rings in the structure. Finally, it is
possible to deduce whether specific functional groups are present.

Interpretation:
Table for Spectroscopic Data
S. No. Wave number Possible group Explanation, if any

Result:

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IR Spectra 1

IR Spectra 2

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Experiment No. 8:
To determine the total alkalinity of the given water sample using methyl orange as
indicator. Given standard N/40 Sodium carbonate to standardize HCl solution.
Apparatus required: Burette, pipette, conical flask, funnel, conical flask, measuring
cylinders.
Chemicals required: Sodium carbonate (N/40) solution, HCl solution, Methyl orange
(M) and water sample.
Theory
The ionic equations involved for this reaction are:
(iv) OH- + H+ H2O
(v) CO3-2 + H+ H2O + CO2

This is an example of neutralization titration. The titration is based upon the

specific pH range of the indicator. Methyl orange gives red colour in pH range 4.4 – 3.0.

NaO3S N N N(CH3)2

Methyl Orange
Procedure:
1. Standardization of given HCl solution
(i) Take 10 mL of standard Na2CO3 with the help of pipette into a conical flask. Add
1-2 drops of methyl orange.
(ii) Run the acid solution from the burette into conical flask drop wise with constant
shaking of solution.
(iii) Find the end point when light yellow colour solution turns red. Note volume of
acid used. Repeat the steps till you get at least two concordant readings

II. Titration of given water sample with HCl solution

(i) Pipette out 10 mL of given water sample into a conical flask. Add 2-3 drops of
methyl orange indicator.
(ii) Add HCl solution from burette into the conical flask with constant shaking.

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(iii) Titrate with acid till yellow coloured solution turns red (end point).

Observations:
Volume of Na2CO3 solution taken for each titration = 10 mL
Observation table is similar to that for Exp No 01.
Table: Burette readings for the titration of given water sample vs HCl
S. No. Initial Reading Final Reading Vol. of HCl used

Calculations:
Normality of Na2CO3 solution = NNa2CO3
Calculation of Normality of HCl is similar to Exp No 01.
To calculate normality of given water solution, apply normality equation
NHCl x VHCl = Nwater sample  Vwater sample
or Nwater sample = NHCl  VHCl / Vwater sample

Result:
Total alkalinity of the given solution (in terms of CaCO3) ………………….
Precautions:
a) Shake the titration flask continuously during adding the solution from the burette.
b) Keep your eye in level with the liquid surface while taking the burette reading or
while reading the pipette or measuring flask etc.
c) Always read lower meniscus in case of colourless solution.

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Experiment No. 9:
To determine the structure of an unknown compound A using Spectroscopic data.

Given: The Molecular Formula for the unknown compound: C9H10O

Theory:
In a modern structure analysis, the powerful spectroscopic methods of IR and NMR play
a major role. In order to determine the structure of an unknown compound, it may be
required to combine a variety of spectroscopic data.

Infra Red (IR) Spectroscopy: Infrared spectrometry is especially useful in identifying

the functional groups in unknown compounds.
1H-NMR Spectroscopy: One of the most important pieces of information in a 1H NMR
spectrum is the chemical shift of the various kinds of protons in the sample. Usually, it is
difficult or even impossible to decipher structural information from a 1H NMR spectrum
without paying close attention to the chemical shifts of the NMR peaks.

Even with NMR analysis, however, it can be useful to see if your conclusions fit
with other observations, such as those from infrared and mass spectroscopy and chemical
reactivity. For example, if your NMR spectrum suggests that the unknown may be a
carboxylic acid, the exceptionally broad OH and the sharp, intense C=O stretching
vibrations in its infrared (IR) spectrum can provide important confirming evidence.

IR Spectrum

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Observations:

Table: Spectroscopic Data

IR Spectrum NMR Spectrum

1. 1.

2. 2.

3. 3.

4. 4.

Analysis & Interpretation

Result:

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Experiment No. 10:

To determine the structure of an unknown compound B using Spectroscopic data.

Given: The Molecular Formula for the unknown compound: C8H10O2

Theory:
In a modern structure analysis, the powerful spectroscopic methods of IR and NMR play
a major role. In order to determine the structure of an unknown compound, it may be
required to combine a variety of spectroscopic data.

Infra Red (IR) Spectroscopy: Infrared spectrometry is especially useful in identifying

the functional groups in unknown compounds.
1H-NMR Spectroscopy: One of the most important pieces of information in a 1H NMR
spectrum is the chemical shift of the various kinds of protons in the sample. Usually, it is
difficult or even impossible to decipher structural information from a 1H NMR spectrum
without paying close attention to the chemical shifts of the NMR peaks.

Even with NMR analysis, however, it can be useful to see if your conclusions fit
with other observations, such as those from infrared and mass spectroscopy and chemical
reactivity. For example, if your NMR spectrum suggests that the unknown may be a
carboxylic acid, the exceptionally broad OH and the sharp, intense C=O stretching
vibrations in its infrared (IR) spectrum can provide important confirming evidence.

Mass Spectrometry: The most obvious information from a compound’s mass spectrum
is its molecular mass. The molecular ion peak is often the peak at the greatest mass in the
spectrum. In practice, however, it can be tricky to rely on this generalization, because
impurities in the spectrometer may produce small peaks of higher molecular mass. Then
it becomes difficult to know exactly what the molecular mass of your compound really is.
In some compounds, the molecular ion peak can be negligibly small because of its
extensive fragmentation in the electron beam.

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Mass Spectrum

IR Spectrum

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NMR Spectrum

Observations:
Table: Spectroscopic Data

Mass Spectrum IR Spectrum NMR Spectrum

1. 1. 1.

2. 2. 2.

3. 3. 3.

4. 4. 4.

Analysis & Interpretation

Result:

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