BSCD291 Lab Manual

B.Tech.
CSE (DS) – 2023

Engineering Chemistry Lab (BSCD291)
Academic Session: 2023-2024 (EVEN Semester/Semester – II)
LABORATORY MANUAL
ENGINEERING CHEMISTRY LAB (BSCD291)
Table of Contents
Experiment/Lab
Page
Exercise/Activity Name of the Experiment/Activity/Exercise
Number(s)
No.
1 Determination of dissolved oxygen present in a given water sample. 2-5
To determine chloride ion in a given water sample by

2 6-9
Argentometric method (using chromate indicator solution).
3 Saponification/acid value of oil. 10-13
Determination of cell constant of a conductivity cell using 0.1M

4 14-17
KCl solution.
Conductometric titration for determination of the strength of a
5 18-22
given NaOH solution by titrating against a standard HCl solution.
pH metric titration for determination of the strength of a given
6 23-28
NaOH solution by titrating against a standard Oxalic acid solution.
7 Determination of viscosity Coefficient. 29-33
8 Thin layer chromatography. 34-37
9 Determination of the rate constant of a reaction. 38-43
10 Chemical analysis of a salt. 44-51
Mr. Akshay Kumar Dey

Assistant Professor, Department of Chemistry
Brainware University, Kolkata 1
B.Tech. CSE (DS) – 2023
EXPERIMENT NO. 1: DETERMINATION OF DISSOLVED OXYGEN PRESENT IN A GIVEN

WATER SAMPLE
1. Aim/Purpose of the Experiment: The aim of the experiment is to determine the quantity of dissolved
oxygen present in the given water sample by using Winkler’s method.
2. Learning Outcomes: After the completion of the experiment, students would be able to examine the
water testing parameter like the amount of dissolved oxygen present in water and predict the quality of
water.
3. Prerequisites: 12th level Chemistry
4. Materials/Equipment/Apparatus/Devices/Software required:
Apparatus:
BOD bottle, Burette, 250 ml conical flask, 50 ml pipette, 10 ml measuring cylinder.
Reagents:
Winkler’s A reagent, Winkler’s B reagent, Conc. H2SO4, Sodium thiosulphate solution, Starch indicator.
5. Introduction and Theory:

Oxygen remains dissolved in water. The deficiency of dissolved oxygen in water is an indicator of
several types of pollution in water. The dissolved oxygen (DO) in water is measured by Winkler’s
method. It is an Iodometric titration. A concentrated Manganous Sulphate solution (Winkler’s A) and
alkali iodide (NaOH + KI) solution (Winkler’s B) are introduced into water sample. The white
precipitate of Manganous Hydroxide [Mn(OH)2] is formed and is subsequently oxidized by dissolved
oxygen in water sample to give a brown precipitate of basic manganic oxide [MnO(OH)2]. This
manganic oxide [MnO(OH)2] is dissolved in acidic medium and liberates free iodine from the added
potassium iodide in an equivalent amount of dissolved oxygen in the water sample. The liberated iodine
is then titrated with standard 0.005(N) sodium thiosulphate solution using starch as indicator. The end
point becomes colourless from blue solution.

Working Formulae:
Let V1 = Volume of water Sample taken.
S1 = Strength of dissolved oxygen.
V2 = Volume of sodium thiosulphate solution required.
S2 = Strength of sodium thiosulphate solution.
Hence, V1 × S1 = V2 × S2
Or, S1 = (V2 × S2)/V1
Now, amount of dissolved oxygen = S1 × 8 g/lit = S1 × 8000 mg/lit = S1 × 8000 ppm.
6. Operating Procedure:
i. Fill the clean dry BOD bottle of capacity 300 ml completely with water sample avoiding as far
as possible contact with air.
ii. Add 2 ml of MnSO4 solution (Winkler`s A) and then 2 ml of alkaline KI (Winkler`s B) with two
different pipettes. The tip of the pipettes must dip below the water surface.
iii. Close the bottle with the stopper immediately and mix the solution well by inverting the bottles
3-4 times. A precipitate appears and allows the precipitate to settle down.
iv. Add 4 ml of concentrated H2SO4, close the bottle and shake till the precipitate dissolves. Allow
the solution to stand for 5 minutes.
v. Pipette out 50 ml of the solution from the BOD bottle and titrate with standard 0.005(N) Na2S2O3
solution using starch as indicator. The colour changes from blue to colourless at the end point.
Repeat the titration to get 2 or 3 concurrent readings.
7. Precautions and/or Troubleshooting:

i. It is important to prevent contamination of the sample water by atmospheric O2 during sampling,
fixation and storage.
ii. Oxygen solubility in water is temperature-dependent so temperature should be mentioned with
the obtained result.

8. Observations & Presentation of Data:
Room Temperature: ………. 0C
Table:
Volume of
sample Mean
Burette reading (ml) Strength of
No. of taken volume of DO
thiosulphate
titrations from BOD thiosulphate (ppm)
(S2) (N)
Bottle (V2 ml)
Initial Final Difference
(V1 ml)
1 50
2 50 0.005 (N)
3 50
9. Calculations & Analysis:

Strength of water sample due to dissolved O2,
S1 = (Volume of thiosulphate × strength of thiosulphate)/Volume of water sample
= (V2 × 0.005)/50
Thus, strength of DO = S1 (N) = (V2 × 0.005)/50 (N)
Amount of DO = S1 × 8 g/lit. = S1× 8000 mg/lit. = S1× 8000 ppm = ………. ppm.
10. Result & Interpretation:

The amount of dissolved oxygen present in the given water sample is ___________ ppm.
Hence, the water is suitable for drinking purpose (Limit 6.5-8 ppm).
11. Follow-up Questions:

a. What is the permissible limit of dissolved oxygen?
b. What do you mean by dissolved oxygen? How is it necessary?

c. Explain the relationship between water temperature and dissolved oxygen levels.
d. What are the potential health risks associated with low dissolved oxygen levels in drinking water
sources?
e. How agricultural practices and runoff can impact dissolved oxygen levels in nearby water bodies?
12. Extension and Follow-up Activities (if applicable):

N.A.
13. Assessments:
INTERNAL:
 Performance: 10
 Viva: 10
 Lab Report (Rough copy and practical note book): 20
14. Suggested readings:

1. Vogel's Qualitative Inorganic Analysis, G. Svehla, 7th edition, Pearson.
2. Vogel’s Text Book of Quantitative Chemical Analysis, J. Mendham, R. C. Denny, J. D. Barnes, M.
J. K. Thomas, 6th edition, Pearson.
3. Practical Physical Chemistry, S. R. Palit, S. K. De, Science Book Agency.
4. B. Sc. Honours Practical Chemistry, S, Dutta, Bharati Book Stall.

EXPERIMENT NO. 2: TO DETERMINE CHLORIDE ION IN A GIVEN WATER SAMPLE BY

ARGENTOMETRIC METHOD (USING CHROMATE INDICATOR SOLUTION)
1. Aim/Purpose of the Experiment: The aim of the experiment is to determine the chloride ion in a given
water sample by Argentometric method (using chromate indicator solution).
2. Learning Outcomes: After the competition of the experiment, students would be able to examine the
water testing parameter like the amount of chloride ion present in water and predict the quality of water.
Apparatus:
10 ml micro-burette, 100 ml conical flask, 10 ml pipette.
Reagents:
Silver nitrate (AgNO3) solution, Potassium chromate (K2CrO4) indicator.

This determination is based on precipitation titration. When AgNO3 solution is added to the water
sample in presence of K2CrO4, the chloride present in it are precipitated as AgCl. As soon as all the
chlorides are precipitated out, even a drop of AgNO3 added in excess gives a brick-red precipitate of
silver chromate. This indicates the end point.
AgNO3 + NaCl = AgCl (Curdy white ppt) + NaNO3
2 AgNO3 + K2CrO4 = Ag2CrO4 (Brick-red ppt) + 2 KNO3
Step 1: Blank titration: Take 10 ml of distilled water (used to prepare the sample) into 100 ml conical
flask. Add 5-6 drops of K2CrO4 into it and titrate the solution against (N/71) AgNO3 solution.

Step 2: Sample titration: Take 10 ml of sample water into 100 ml conical flask. Add 5-6 drops of K2CrO4
into it and titrate the solution against (N/71) AgNO3 solution till the appearance of brick-red colour.

i. A uniform sample size must be used, so that ionic concentrations needed to indicate the end
point will be constant.
ii. The pH must be in the range of 7 to 8 as silver ions are precipitated as AgOH at high pH
levels and the chromate ions are converted to Cr2O72- at low pH values.
iii. A definite amount of indicator must be used to provide a certain concentration of chromate
ions, otherwise silver chromate may form too soon or not soon enough.
iv. Caution should be made to notice indicator color change as it can varies person-to-person.
The titrant should be added drop wise and the sample shaken constantly.
v. At least three readings for each case should be taken.
Table 1: Blank titration.
Volume of
Burette reading (ml) Mean volume Strength of
No. of distilled
of AgNO3 AgNO3
titrations water
Initial Final Difference (VA ml) (SAgNO3) (N)
(V ml)
1 10
2 10 N/71
3 10

Table 2: Sample titration.

Volume of AgNO3
Burette reading (ml)
required to
Volume Mean consume the Strength Strength
No. of of water volume of chloride present of AgNO3 of water
titrations sample AgNO3 in sample water (SAgNO3) sample
(VW ml) (VB) (ml) (ml) (N) (SW) (N)
VAgNO3 =
(VB – VA)
1 10
2 10 N/71
3 10

Let volume of AgNO3 used be VAgNO3 ml and volume of water sample be VW ml.
Then, from VW × SW = VAgNO3 × SAgNO3
SW = (VB – VA)/710 (N)
So, the amount of chloride ions in the given water sample is
[(VB – VA) x 35.5 x 1000]/710 mg lit-1 (or ppm) = ………. ppm

The amount of chloride ions present in the given water sample is ………… ppm.

i. What is the permissible value of Chlorides for drinking water?
ii. What does excess of Chloride content in drinking water indicate?
iii. At the end point the change of colour is observed. What does it indicate?

N.A.

13. Assessments:
INTERNAL:
 Performance: 10
 Viva: 10


EXPERIMENT NO. 3: SAPONIFICATION/ACID VALUE OF OIL
1. Aim/Purpose of the Experiment: The aim of the experiment is to determine the acid value of a given
oil sample.
oil testing parameter like the amount of acid present in oil and evaluate the oil's suitability for various
applications in the food and industrial sectors.
Apparatus:
50 ml burette, 100 ml conical flask, 10 ml pipette.
Reagents:
Ethanol, NaOH solution, Oxalic acid solution, Phenolphthalein indicator, oil.

Sometimes the oils or fats contain free acids are expressed as acid value of the sample. The acid
value of the oil can be defined as the quantity of base expressed in milligram of potassium hydroxide
required to neutralize the free acid present in one gram of oil or fat.
A definite amount of the oil sample is dissolved in a definite volume of suitable solvent (mixture of
ethanol and diethyl ether in 1:1 ratio). The mixture is titrated with constant shaking with standard
sodium hydroxide solution using phenolphthalein as indicator.
Working Formulae:
Let the volume of NaOH solution of normality N be V ml and weight of the oil be W g.
The number of mili equivalent of alkali for neutralization of acid in W g of oil = V x N
= V x N x 56.1 mg of KOH

Where 56.1 is the equivalent weight of KOH

So, acid value = (V x N x 56.1)/W (unit less)
Step 1: Standardization of NaOH solution by standard oxalic acid solution:
Take 10 ml of supplied standard Oxalic acid (0.05 N) in a 100 ml clean conical flask and add 2-3 drops
of phenolphthalein indicator solution. Then add Sodium hydroxide solution from the burette carefully
till the whole mixture becomes pink on addition of just a drop of sodium hydroxide solution. Record
the burette reading and repeat the process at least two times for concordant values.
Step 2: Estimation of acid value of supplied oil:

Take 1 ml of the supplied oil sample in a 100 ml clean conical flask and then add about 10 ml of the
solvent (Diethyl ether and ethanol in 1:1 by volume). Shake the mixture for about 10 minutes to dissolve
the oil. Add about 20 ml of distilled water and shake the mixture shaken for 5 minutes. Then add 2-3
drops of phenolphthalein indicator. Next add Sodium hydroxide from the burette drop wise with
constant shaking till pink colour appeared which lasted for 30 seconds. Record the burette reading.

i. Reagents should be accurately standardized.
ii. The oil should be almost completely soluble to get more appropriate result.
iii. During titration the colour change at the end point should be reached by adding only one drop
of NaOH.

Table 1: Standardization of Sodium Hydroxide solution.
Volume of Mean
Strength of Strength
No. of Oxalic Burette reading (ml) volume of
Oxalic acid of NaOH
titrations acid NaOH
(S1) (N) (S2) (N)
(V1 ml) (V2 ml)
1 10
2 10 0.05 (N)
3 10
Table 2: Estimation of acid value.

Volume of Density of Mass of Burette reading (ml) Strength
Acid
oil oil oil (W) of NaOH
Initial Final Difference value
(ml) (g ml-1) (g) (S2) (N)
1 0.93 0.93

Let volume and strength of NaOH be V1 ml and S1 (N).
Volume and strength of NaOH be V2 ml and S2 (N).
Then, from V1S1 = V2S2
10 x 0.05 = V2 x S2
Or, S2 = (10 x 0.05)/V2 (N)
So, Acid value (A.V.) = (V x S2 x 56.1)/W
Where, S2 = Normality of NaOH solution (N)
V = Volume of NaOH for titration of acid (ml)
W = Weight of oil (g)


The acid value of the given oil sample is ……..

i. Define the acid value of oil and explain its significance in assessing oil quality.
ii. What is the principle behind the acid-base titration method used to determine the acid value of
oil?
iii. Discuss the factors that can influence the acid value of oil
iv. Why is it essential to standardize the potassium hydroxide (KOH) solution before performing
the acid value analysis of oil?
v. What preventive measures can be taken during oil processing and storage to minimize the
increase in acid value over time?
vi. In what industrial applications is the acid value of oil particularly important, and why?

N.A.
13. Assessments:
INTERNAL:
 Performance: 10
 Viva: 10


EXPERIMENT NO. 4: DETERMINATION OF THE CELL CONSTANT OF A CONDUCTIVITY

CELL USING 0.1(M) KCl SOLUTION
1. Aim/Purpose of the Experiment: The aim of the experiment is to determine the cell constant of a
conductivity cell using 0.1(M) KCl solution.
2. Learning Outcomes: After the competition of the experiment, students would be able to describe
conductometric titration and estimate quantitatively via application of this technique.
Apparatus:
100 ml beaker, 10 ml pipette.
Reagents:
0.1 (M) KCl solution
Equipment:
Conductivity meter

 Electricity: It is the rate at which electrical charge flows through a conductor. The unit of electricity
is Ampere (A).
 Conductor: Any substance that can conduct electricity is known as conductor.
 Resistance: It is the opposition to the flow of electricity.
𝒍
For any conductor 𝑹=𝝆
𝑨
Where l and A are the length and the area of cross section of conductor. Its unit is Ω (ohm).
 Conductance: It is the property of the conductor that allows the flow of electricity through it. It is
equal to the reciprocal of the resistance of the conductor. It is denoted by ‘G’.

For any conductor, G = (1/R)

Its unit is ohm-1 or mho or Siemen (S).
 Conductivity (Specific conductance): It is the ability of the conductor to allow the flow of
electricity through it. It is equal to the reciprocal of the resistivity of the conductor. It is denoted by
𝜿� (Greek letter ‘kappa’).
1 𝑙
For any conductor, 𝜅=( )=𝐺
𝜌 𝐴
Its unit is Siemen cm-1 (S cm-1).
 Cell constant: It is defined as the ratio of the length and the cross-sectional area of the conductor
and is denoted by (l/A). Its unit is cm-1.
Working Formulae:
The cell constant of the conductivity cell is calculated by using the formula
1 𝑙 𝑙 𝜅
𝜅 = ( ) = 𝐺 �� ⟹ �� =
𝜌 𝐴 𝐴 𝐺
Given that 𝜿(𝟎.𝟏�𝑴�𝑲𝑪𝒍�𝒔𝒐𝒍𝒖𝒕𝒊𝒐𝒏) = 1.2886 S m-1
Take a 100 ml beaker and pour 50-60 ml standard 0.1 (M) KCl solution into it. Dip the conductivity
cell into the solution, shake for about 10-15 seconds and record the conductance value of the solution.

i. Cleanliness: It should be ensured that the conductivity cell or probe is thoroughly cleaned and
free from any residues or contaminants before calibration. Residues on the electrodes can affect
the cell constant and lead to inaccurate readings.
ii. Temperature: A stable temperature should be maintained during the calibration process, as
conductivity is temperature-dependent.
iii. Calibration Solutions: High-quality calibration solutions to be used with known and traceable
conductivity values.

iv. Rinse between Solutions: The cell thoroughly to be rinsed with deionized or distilled water
between each standard solution to prevent cross-contamination and ensure accurate calibration.
Table: Determination of cell constant
Conductance (G) Conductivity (𝜅 ) Cell constant (l/A)

Sample
(mS) (S m-1) (cm-1)
0.1 (M) KCl solution 1.2886

𝜅
Cell constant = (l/A) = = ………………… cm-1
𝐺

The cell constant of the conductivity cell is ………… cm-1.

i. What is the purpose of determining the cell constant of a conductivity cell?
ii. How does temperature affect the cell constant and conductivity measurements? How can you
compensate for temperature variations?
iii. Why is a zero calibration necessary before determining the cell constant?
iv. What factors can lead to inaccurate cell constant values, and how can they be avoided?

N.A.

13. Assessments:
INTERNAL:
 Performance: 10
 Viva: 10


EXPERIMENT NO. 5: CONDUCTOMETRIC TITRATION FOR DETERMINATION OF THE

STRENGTH OF A GIVEN NaOH SOLUTION BY TITRATING AGAINST A STANDARD HCl
SOLUTION
1. Aim/Purpose of the Experiment: The aim of the experiment is to determine the strength of a given
NaOH solution by titrating against a standard HCl solution by Conductometric titration.
2. Learning Outcomes: After the competition of the experiment, students would be able to describe
conductometric titration and estimate quantitatively via application of this technique.
Apparatus:
100 ml beaker, 10 ml pipette, 10 ml micro-burette
Reagents:
NaOH solution of unknown strength, HCl solution of known strength
Equipment:
Conductivity meter

The conductance of an electrolyte solution depends on the total number of ions and their mobilities.
When a solution of a strong acid (say HCl) is taken in a beaker, it remains completely ionized. After
measuring the conductance of the solution a few drops of NaOH solution from burette is added.
Reaction takes place when fast moving H+ ions are replaced by slow moving Na+ ions, so conductance
falls. Addition of drops of NaOH solution is continued and conductance is measured for each addition.
Chemical reaction takes place up to neutralization and hence conductance gradually falls. After
neutralization, addition of NaOH only increases number of Na+ and OH- ions in the solution and hence
conductance of the solution increases with the addition of drops of NaOH. When conductance as Y-axis

is plotted against number of drops of alkali added as X-axis, two straight lines with negative and positive
slopes are obtained. The point of intersection of the two straight lines gives number of drops of alkali
needed for neutralization for the taken volume of acid. The number of drops is then converted into
volume by measuring the volume of a definite number (say 20) of drops of alkali for the same burette.
The strength of alkali is kept almost 10 times than that of acid; otherwise dilution of solution takes
place, resulting in a change in conductance.
Working Formulae:
The acid-base neutralization reaction takes place is
HCl + NaOH  H2O + NaCl
Let V1 ml of HCl solution having S1 (N) is neutralized by V2 ml of NaOH solution of strength S2 (N).
Then, V1 × S1 = V2 × S2
Or, S2 = V1 × S1/V2 (N)
So, the strength of the base (S2) = ………… (N).
 Rinse the cell a number of times with distilled water.
 Pipette out 10 ml of supplied HCl into a clean 100 ml clean beaker, dip the cell into it and add
sufficient distilled water just to dip the electrodes. Mix the solution and record the conductance
value in mS unit (it is the conductance value after adding zero drops of NaOH).
 Add 4 drops of NaOH having same size (add slowly to get same size droplets) from a micro-burette
(having capacity 10 ml) into the beaker, mix and record the conductance.
 Continue the addition of NaOH and measure the conductance after each addition.
 Take at least 6 readings beyond the end point (after a point the conductance value will increase due
to addition of NaOH).
 30 drops of alkali are allowed to fall from the same burette and the corresponding volume is
determined to find the volume of one drop of alkali.
 Plot conductance values as Y-axis against the added number of drops of alkali as X-axis in a graph.
The neutralization point is determined from the intersection of the two extrapolated straight lines.

Conductometric titration curve of HCl vs NaOH

v. Cleanliness: It should be ensured that the conductivity cell or probe is thoroughly cleaned and
free from any residues or contaminants before calibration. Residues on the electrodes can affect
the cell constant and lead to inaccurate readings.
vi. Temperature: A stable temperature should be maintained during the calibration process, as
conductivity is temperature-dependent.
vii. Calibration Solutions: High-quality calibration solutions to be used with known and traceable
conductivity values.
viii. Rinse between Solutions: The cell thoroughly to be rinsed with deionized or distilled water
between each standard solution to prevent cross-contamination and ensure accurate calibration.
Table: Recording of conductance values

No. of drops of NaOH added Conductance (mS)
0
4
8

12
16
20
…

i. 30 drops of alkali = ……….. (X) ml
Thus, 1 drop of alkali = ……….. (X/30) ml
ii. Let the no. of drops of NaOH required for the equivalent point is ………. (Y) (From the graph)
and the strength of the supplied NaOH solution is S2 (N).
Thus, the equivalence point (V2) = ……….. (X/30 × Y) ml.
iii. So, the strength of unknown supplied NaOH solution is
S2 = (V1 × S1)/V2 = ………. (N)
Where, V1 is the volume of HCl solution taken, here it is 10 ml.

The strength of the supplied unknown NaOH solution is ………. (N).
[Here, the strength of NaOH (S2) is given as 0.5 (N).]

i. How does temperature affect the conductivity of a solution during titration, and why is
temperature control important in conductometric titrations?
ii. In a conductometric titration of a weak acid (acetic acid) with a strong base (NaOH), how would
you expect the titration curve to differ from that of a strong acid (HCl) with the same base?
iii. Explain the concept of conductometric titration curves and how they can be used to identify the
equivalence point.
iv. In a conductometric titration, 25 ml of 0.1 (M) HCl is titrated against 0.1 (M) NaOH. Calculate
the volume of NaOH required to reach the equivalence point.
v. Explain the concept of an "end point" in conductometric titration and how it is determined.


N.A.
13. Assessments:
INTERNAL:
 Performance: 10
 Viva: 10


EXPERIMENT NO. 6: pH-METRIC TITRATION FOR DETERMINATION OF THE STRENGTH

OF A GIVEN NaOH SOLUTION BY TITRATING AGAINST A STANDARD OXALIC ACID
SOLUTION
1. Aim/Purpose of the Experiment: The aim of the experiment is to determine the strength of a given
NaOH solution by titrating against a standard Oxalic acid solution by pH-metric titration.
2. Learning Outcomes: After the competition of the experiment, students would be able to describe pH-
metric titration and estimate quantitatively via application of this technique.
Apparatus:
100 ml beaker, 10 ml pipette, 10 ml micro-burette
Reagents:
0.1 (N) standard Oxalic acid solution, NaOH solution of unknown strength
Equipment:
pH meter

The pH of a solution is expressed by the relation where [H+] is the molar concentration of the H+
ions in the solution. The range of pH in aqueous solution is 0 to 14. A neutral solution has a pH = 7
while acids have pH less than 7 and alkalis greater than 7.
Measurement of pH by a pH meter can be employed to monitor the course of acid base titration. On
gradual addition of an alkali (say NaOH) to an acid solution (say oxalic acid), the pH rises slowly in
the initial stage, then it rises sharply at the end point just by addition of a drop of alkali and after that it
flattens again.

A plot of pH against the number of drops of alkali is made in a graph paper and the number of drops
of alkali when there is a sharp rise in pH gives the amount of alkali for neutralization of the given
volume of acid taken.
In this pH determination a glass electrode is used. It consists of a thin membrane of a specially
prepared soft glass globe containing a dilute solution of hydrochloric acid (0.1 N HCl) in which is
immersed Ag-AgCl electrode. It is coupled with a reference electrode which is a saturated calomel
electrode.
The cell obtained is

Ag-AgCl(s) ǀ 0.1(N) HCl ǀ Glass ǀ Unknown solution ǀǀ Saturated calomel electrode
At very high pH (>10), this glass electrode loses its reversibility with H+ ions and becomes
ineffective.
Working Formulae:
Let V1 ml of acid (say Oxalic acid) solution having S1 (N) is neutralized by V2 ml of base (say
NaOH) solution of strength S2 (N).
Then, V1 × S1 = V2 × S2
Or, S2 = V1 × S1/V2 (N)
So, the strength of the base (S2) = ………… (N).
Usually the concentration of alkali is about 5-10 times that of the acid to avoid the change of pH
due to dilution.
 Calibrate the pH meter by dipping the glass electrode in a buffer solution having pH 4 in a 100 ml
beaker.
 Take 10 ml of supplied acid solution in a 100 ml beaker.
 Wash the electrode with distilled water and soak with tissue paper.
 Place the electrode in acid solution and add distilled water to immerse the electrode within the
liquid. Mix the solution well.

 Record the pH shown in the pH meter. Add two drops of NaOH from the burette, mix well and
record the pH shown by the pH meter.
 Continue the addition of NaOH and recording of pH.
 Add NaOH drop-wise near neutralizing point (pH 4.5).
 Stop addition of NaOH when there is a sharp rise in pH and then continue again.
 Take the glass electrode out of the titrating solution, wash with distilled water and keep immersed
in distilled water in another beaker.
 30 drops of alkali are allowed to fall from the same burette and the corresponding volume is
determined to find the volume of a drop of alkali.
 A graph is plotted between pH on y-axis and no. of drops of alkali added on X-axis and the number
of drops of alkali at the neutralization point is determined.
pH-metric titration curve of Oxalic acid vs NaOH

i. Clean glassware: All the glassware, including burettes, pipettes, and flasks are to be cleaned
and free from any contaminants. Residual substances from previous experiments could affect
the accuracy of the titration.
ii. Calibration: Regularly the pH meter should be calibrated using standard buffer solutions of
known pH values. This step ensures that the pH meter is giving accurate readings.

iii. Standardization of the titrant: If a strong acid or base as a titrant is used, it's crucial to
standardize it with a primary standard substance to determine its exact concentration. This step
helps in obtaining precise results.
iv. Titration speed: The titrant should be added slowly and carefully, especially near the end point.
Rapid addition can lead to overshooting the endpoint, causing errors in the titration.
Table: Recording of pH values
No. of drops of NaOH added Conductance (mS)

0
2
4
6
8
10
12
14 ~ 4.5
15
16
17
…

i. 30 drops of alkali = ……….. (X) ml
Thus, 1 drop of alkali = ……….. (X/30) ml

ii. Let the no. of drops of NaOH required for the equivalent point is ………. (Y) (From the graph)
and the strength of the supplied NaOH solution is S2 (N).
Thus, the equivalence point (V2) = ……….. (X/30 × Y) ml.
iii. So, the strength of unknown supplied NaOH solution is

S2 = (V1 × S1)/V2 = ………. (N)
Where, V1 is the volume of Oxalic acid solution taken, here it is 10 ml.

The strength of the supplied unknown NaOH solution is ………. (N).
[Here, the strength of NaOH (S2) is given as 0.5 (N).]

i. Discuss the difference between strong acid-strong base and weak acid-strong base pH metric
titrations.
ii. In a titration of a strong acid with a strong base, what will be the pH at the equivalence point?
Explain.
iii. Calculate the concentration of an unknown acid solution if 25.0 ml of 0.1 (M) NaOH is required
to neutralize 50.0 ml of the acid during titration.
iv. What are some common errors that can occur during pH metric titrations, and how can they be
identified and corrected?

N.A.
13. Assessments:
INTERNAL:
 Performance: 10
 Viva: 10



EXPERIMENT NO. 7: DETERMINATION OF VISCOSITY COEFFICIENT
1. Aim/Purpose of the Experiment: The aim of the experiment is to determine the viscosity coefficient
of a given liquid sample.
2. Learning Outcomes: After the competition of the experiment, students would be able to explain and
evaluate the liquid property like viscosity.
Apparatus:
Ostwald viscometer, 10 ml pipette, dropper, specific gravity bottle, stopwatch
Reagents:
5% sucrose solution, 10% sucrose solution, Sucrose solution of unknown strength, Distilled water

Viscosity is a property which opposes the flow of a liquid. The co-efficient of viscosity (η) is defined
as the tangential force per unit area to maintain unit difference of velocity between the two layers unit
distance apart. Its unit is dyne cm-2 sec or poise.
The viscosity coefficient (η) of a liquid is determined by measuring the time of flow of a definite
volume of liquid through the capillary of an Oswald's viscometer using Poiseuille’s equation,
𝜋𝑃𝑟 4 𝑡
𝜂=
8𝑙𝑉
Where l and r the length and radius of the capillary, respectively, t is the time of flow of V ml of
liquid and P is the driving force = ρgh.
If a liquid and water are taken separately, then
𝜼𝒍 𝑷𝒍 𝒕𝒍 𝝆𝒍 𝒈𝒉𝒕𝒍 𝝆𝒍 𝒕𝒍 𝒕𝒍
=� =� =� = �𝒔
𝜼𝒘 𝑷𝒘 𝒕𝒘 𝝆𝒘 𝒈𝒉𝒕𝒘 𝝆𝒘 𝒕𝒘 𝒕𝒘

Where, s = specific gravity of the liquid.
𝒕𝒍
So, 𝜼𝒍 = �𝒔 � × � 𝜼𝒘
𝒕𝒘
Knowing the 𝜼𝒘 , 𝜼𝒍 can be calculated. It is a relative method.

The plot of 𝜼𝒍 at various known concentration of solution against the percentage concentration of
the solution gives a straight line. By measuring the viscosity coefficient of the supplied unknown
solution, its concentration can be calculated from the graph.
Viscosity of liquids decreases with increase in temperature.
 Keep the viscometer vertically with a stand.
 Rinse the viscometer with distilled water. Introduce distilled water up to the mark on in the large
bulb.
 Using rubber tube suck the liquid in the other limb above the mark and then allow to fall. Start the
stop watch when the liquid level touches the upper mark and stop it when it touches the lower mark.
Record the time. Repeat it twice.
 Repeat the above step with the other supplied liquids.
 Determine the specific gravity of the supplied liquid with a specific gravity bottle.
 Calculate the viscosity coefficient of all the supplied liquids.
(Given the viscosity coefficient of water at 30⁰C to be 8.0 mp.)
 Plot viscosity coefficient of liquid at y-axis and its concentration on (%) as x-axis. A straight line
is obtained. Calculate the strength of the given unknown liquid from the graphical plot.

 Calibration: Before starting any viscosity measurement, make sure all the instruments involved in
the process, such as viscometers or rheometers, are properly calibrated. Calibration ensures that the
instruments provide accurate and consistent readings.

 Viscosity is highly temperature-dependent, so it is crucial to note down the temperature of the fluid
during the measurement.
 Sample preparation: The fluid sample should be free from any contaminants, bubbles, or foreign
particles that may interfere with the measurement. Properly clean and degas the sample if necessary.
Table 1: Determination of time for flow of liquids
Liquids Time of flow (sec) Average time of flow (sec)

1. ………………
Water (0%)
2. ……………… tw = …………
5% Sucrose solution 1. ………………
(liquid X1) 2. ……………… t5% = …………
10% Sucrose solution 1. ………………
(liquid X2) 2. ……………… t10% = …………
Unknown Sucrose solution 1. ………………
(liquid X3) 2. ……………… tunk = …………
Table 2: Determination of specific gravity of the liquids:
Weight of
Weight of empty Weight of empty Weight of empty
Weight of empty bottle
bottle filled with bottle filled with bottle filled with
empty bottle filled with
liquid X1 liquid X2 liquid X3
distilled water
W1 (g) = W2 (g) = W3 (g) = W4 (g) = W5 (g) =
Specific 𝑾𝟑 − � 𝑾𝟏 𝑾𝟒 − � 𝑾𝟏 𝑾𝟓 − � 𝑾𝟏
𝑺𝟓% = � 𝑺𝟏𝟎% = � 𝑺𝒖𝒏𝒌 = �
gravity of the 𝑺𝒘 = 𝟏 𝑾𝟐 − � 𝑾𝟏 𝑾𝟐 − � 𝑾𝟏 𝑾𝟐 − � 𝑾𝟏
liquids = ……... = ……... = ……...


Calculate viscosity coefficient of each liquid using the Poiseuille’s equation with the help of tables
1 and 2.
Table 3: Calculation of viscosity coefficient of different liquids:
Viscosity coefficient (η)

Liquids Equation
(mp)
Water (0%) --- 8
5% Sucrose 𝒕𝟓%
𝜼𝟓% = � 𝑺𝟓% � × � �× 𝟖
solution 𝒕𝒘 .........
10% Sucrose 𝒕𝟏𝟎%
𝜼𝟏𝟎% = � 𝑺𝟏𝟎% � × � �× 𝟖
solution 𝒕𝒘 .........
Unknown 𝒕𝒖𝒏𝒌
𝜼𝒖𝒏𝒌 = � 𝑺𝒖𝒏𝒌 � × � �× 𝟖
Sucrose solution 𝒕𝒘 .........
Table 4: Table for graph:
X-axis Y-axis
Concentration (% Solution) Viscosity coefficient (𝜼) (mp)
Water (0%) 8
5% Sucrose Solution ……….
10% Sucrose solution ……….

The viscosity coefficient of the given unknown water solution is .......... mp and its concentration is
………. % (from the graph).


i. Define viscosity and explain its significance in fluid mechanics.
ii. What are the different units used to express viscosity? How are they related to each other?
iii. Explain how temperature affects the viscosity of a fluid. Provide examples of fluids whose
viscosity changes significantly with temperature.
iv. Discuss the impact of pressure on the viscosity of a fluid. Are there any general trends or rules
that apply to all fluids?
v. A certain liquid has a viscosity of 0.02 Pa•s. Express this viscosity in poise and centipoise units.

N.A.
13. Assessments:
INTERNAL:
 Performance: 10
 Viva: 10


EXPERIMENT NO. 8: THIN LAYER CHROMATOGRAPHY
1. Aim/Purpose of the Experiment: The aim of the experiment is to separate amino acids from their
mixture using Thin Layer Chromatography (TLC) technique.
2. Learning Outcomes: After the competition of the experiment, students would be able to interpret the
principle of TLC method and apply the technique to separate amino acids.
i. Stationary phase: TLC plate
ii. Mobile phase: 1-butanol:Acetic acid:Water (4:1:5)
iii. TLC developing chamber
iv. Spraying reagent: 0.3% Ninhydrin in 95% ethanol
v. Standard amino acid solution: 10 mg solution of each of d-Alanine, l-Leucine, l-Lysine were
prepared in 5 ml ethanol and labelled them as (A), (B) and (C), respectively.
vi. Unknown sample of amino acids: Any two of the above solutions were mixed and labelled it
as unknown containing unknown amino acids (X) and (Y)
vii. Fine capillary tubes
viii. TLC reagent sprayer

 Chromatography on TLC is a solvent extraction type of process.
 The amino acids to be separated undergo partition between the TLC plate and organic solvent used
as the mobile phase.
 TLC plate acts as the stationary phase here.
 The mobile phase is a mixture of 1-butanol, acetic acid and water (4:1:5). In this solvent the amino
acids will get separated and appear as three purple colour spots corresponding to the RF value.

 The upper spot corresponds to l-Lysine, the middle spot corresponds to d-Alanine and the lower
spot corresponds to l-Leucine.
 Draw a base line at a distance of 1 cm from the lower edge of the TLC strip and put four pencil
dots at equal distance on the base line.
 Make the spot of three standard solutions with the capillary tube on three pencil dots and make the
spot of the unknown solution on the rest pencil dot. Allow the spots to dry.
 Fill the TLC chamber with 15 ml of the solvent mixture (mobile phase solvent).
 Insert the dried TLC plate into the jar in such a way that the sample spots remained downward and
the solvent touched the adsorbent layer well below the spot level.
 Allow the solvent to rise for about 8-10 cm.
 Take out the TLC plate from the jar and mark the level up to which the solvent front rise and
measure by scale from the base line.
 Allow the plate to dry.
 After drying, spray the Ninhydrin solution and dry in an air oven strongly.

 The purple spots appear depending on their respective RF values.

 Label the two spots separated from the unknown sample as X and Y.
 Find out the unknown mixture of solution by comparing the RF values with the standard solution.

 Care should be taken so that the jar becomes saturated with the solvent vapour before introducing
the TLC plate in the jar.
 The spot should be made carefully on the TLC plate with a fine capillary.
 Care must be taken so that the TLC plate does not touch the side of the vessel.
Table 1: Calculation of RF values of standard samples:

Standard samples of Distance travelled by the Distance travelled by the RF value
amino acids solute from the base line solvent from the base line (d1 / d)
(d1 cm) (d cm)
A (d-Alanine)
B (l-Lysine)
C (l-leucine)
Table 2: Calculation of RF values of unknown samples:

Standard samples of Distance travelled by the Distance travelled by the RF value
amino acids solute from the base line solvent from the base line (d1 / d)
(d1 cm) (d cm)
X
Y


The RF values of the unknown sample X is ……….. and Y is …………, which are in accordance
with the RF values of the standard amino acid samples ………… and …………, respectively.
Hence, comparing the RF values of the components in the mixture with that of the known amino
acid, it can be concluded that the mixture contains …………… and ………….. amino acids.

i. Discuss the principle behind Thin Layer Chromatography.
ii. Describe the components of a TLC plate and their functions.
iii. What are the different types of stationary phases used in TLC?
iv. Explain the factors influencing the separation of compounds in TLC.
v. How the RF value is calculated in Thin Layer Chromatography? What does it signify?
vi. Describe the significance of selecting appropriate mobile and stationary phases in TLC.

N.A.
12. Assessments:
INTERNAL:
 Performance: 10
 Viva: 10


EXPERIMENT NO. 9: DETERMINATION OF THE RATE CONSTANT OF A REACTION
1. Aim/Purpose of the Experiment: The aim of the experiment is to determine the rate constant of the
kinetics of acid catalyzed hydrolysis of ester.
rate of a chemical reaction and as well as determine the rate constant of the particular reaction.
Apparatus:
250 ml and 100 ml conical flask (one each), one 50 ml burette, 2 ml and 10 ml pipette (one each), 100
ml and 25 ml measuring cylinder (one each), watch glass, stopwatch, cold water bath.
Reagents:
Ester (Methyl acetate), acid catalyst (0.1 (N) HCl solution), alkali solution (0.01 (N) NaOH solution),
cold water, Phenolphthalein indicator.

The hydrolysis of ester catalyzed by dilute mineral acid is represented as
𝐻+
𝑅𝐶𝑂𝑂𝑅 ′ + � 𝐻2 𝑂� → � 𝑅𝐶𝑂𝑂𝐻 + 𝑅 ′ 𝑂𝐻
The rate of the reaction is written as
𝑑[𝑒𝑠𝑡𝑒𝑟]
−� = � 𝑘1 � × � 𝐶𝑒𝑠𝑡𝑒𝑟 � × � 𝐶𝐻2 𝑂 � × � 𝐶𝐻 +
𝑑𝑡
Where, 𝐶𝐻 + �is constant as 𝐻 + is a catalyst. Water is present in so large excess that 𝐶𝐻2 𝑂 also remains
unchanged. Therefore, the rate is, finally, given by
𝑑[𝑒𝑠𝑡𝑒𝑟]
−� = �𝑘� × � 𝐶𝑒𝑠𝑡𝑒𝑟
𝑑𝑡
Where, 𝑘 = � 𝑘1 � × � 𝐶𝐻2 𝑂 � × � 𝐶𝐻 + = rate constant for the hydrolysis of the given ester.

The order of the reaction is one and it is a pseudo-first order reaction. Generally, Methyl acetate or
Ethyl acetate is used as ester.
The kinetics of this reaction is studied by titrating the liberated acid with alkali and recording the
titre value with time.
The integrated rate equation for first order reactions is
1 𝑎
𝑘 = � ln
𝑡 𝑎−𝑥
Where, a = initial concentration of ester and x = concentration of ester hydrolysed after time t =
concentration of CH3COOH after time t.
Unit of k is time-1 (sec-1).
Working formulae:
We have
1 𝑎
𝑘 = � ln
𝑡 𝑎−𝑥
1 𝑎
𝑜𝑟, 𝑡 = � ln
𝑘 𝑎−𝑥
To avoid the initial concentration of ester, time difference Δt is taken. Now,

1 𝑎
𝑡1 = � ln
𝑘 𝑎 − 𝑥0
1 𝑎
𝑎𝑛𝑑, 𝑡2 = � ln
𝑘 𝑎 − 𝑥1
1 𝑎 − 𝑥0
𝑠𝑜, ∆𝑡 = � ln
𝑘 𝑎 − 𝑥1
Now, let V0, V1, V2, V3… be the volumes of alkali for definite volume of reaction mixture in t 1, t2,
t3… sec and 𝑉∞ be the volume of alkali after infinite time, i.e., when the reaction is completed.
Then, (𝑎 − 𝑥0 ) ∝ (𝑉∞ − 𝑉0 ) and (𝑎 − 𝑥1 ) ∝ (𝑉∞ − 𝑉1 ).
Hence,
1 𝑉∞ − 𝑉0
∆𝑡 = � ln
𝑘 𝑉∞ − 𝑉1

1 𝑉∞ − 𝑉0
𝑜𝑟, 𝑘 =� ln
∆𝑡 𝑉∞ − 𝑉1
1 𝑉∞ −𝑉0
Thus, in general, ∆𝑡𝑛 = � ln
𝑘 𝑉∞ −𝑉𝑛
Where, ∆𝑡𝑛 = � 𝑡𝑛+1 − � 𝑡1
𝑉∞ −𝑉0
So, ln = 𝑘�. ∆𝑡𝑛
𝑉∞ −𝑉𝑛
𝑉 −𝑉
When ln 𝑉∞−𝑉0 (as y-axis) is plotted against ∆𝑡𝑛 (as x-axis), a straight line passing through origin is
∞ 𝑛
obtained.
The gradient of the straight line gives the value of rate constant ‘k’.
 Wash the burette with distilled water and then rinse well with the supplied alkali solution. Fill the
burette with alkali solution with no air gap below the stop-cock. Adjust the level to zero mark.
 Take 100 ml of supplied acid catalyst solution in the dry 250 ml conical flask by 100 ml measuring
cylinder.
 Pour 20 ml of cold distilled water in the 100 ml conical flask and add 2-3 drops of phenolphthalein
indicator.
 Add 10 ml of supplied ester by 10 ml pipette. Start the stopwatch at the half discharge and note the
time as t1 (0 second). Stir the mixture and place it in cold water bath.
 Immediately (within 15 seconds or less if possible) take out 2 ml aliquot of the reaction mixture
and run into 100 ml the conical flask. Titrate this solution using the supplied NaOH solution till a
light pink colour is appeared. Record the titre value and mark it as V0.
 Repeat step (3). Again take out 2 ml aliquot of the reaction mixture and run it into 100 ml conical
flask. Record the half discharge time and mark it as t2 (approx. 300 seconds).
 Titrate the solution in 100 ml conical flask using the supplied NaOH solution till a light pink colour
is appeared. Record the titre value and mark it as V1.
 Take five such readings with a time-gap of approximately 5 minutes between each two readings.

 Recording of 𝑽∞ : Cover the mouth of the conical flask containing the reaction mixture by a watch
glass. Heat it in a water bath at about 60°C for about 30 minutes. Cool the mixture. Repeat step (3).
Take 2 ml aliquot of the reaction mixture and run into 100 ml the conical flask. Titrate this solution
using the supplied NaOH solution till a light pink colour is appeared. Record the titre value and
mark it as 𝑉∞ .

 Purity of all the chemicals used in the reaction should be highly purity. Impurities can introduce
variability and affect the reaction rate, leading to inaccurate results.
 A constant temperature and precise temperature to be maintained throughout the experiment. Rate
constants are highly temperature-dependent, so any fluctuations can lead to significant errors in the
measurements.
 Adequate and consistent stirring or mixing of the reaction mixture is to be continued to ensure
uniform distribution of reactants. Incomplete mixing can lead to concentration gradients that affect
the rate constant determination.
 A regular time interval should be maintained to capture the progress of the reaction accurately. Too
few data points may lead to imprecise rate constant determination.
 Multiple trials of the reaction should be performed under the same conditions to obtain an average
rate constant and reduce random errors.
Table 1: Table for calculation of rate constant:

∆𝒕𝒏 (sec) Volume of 𝑽∞ − 𝑽𝒏 𝑽∞ − 𝑽𝟎 Value of k

Time (sec) 𝐥𝐧
(𝒕𝒏+𝟏 − � 𝒕𝟏 ) NaOH (ml) (ml) 𝑽∞ − 𝑽𝒏 (sec-1)
t1 = 0 ∆𝒕𝟎 = 0 V0 = 𝑉∞ − 𝑉0 = 0
t2 = 300 ∆𝒕𝟏 = 300 V1 = 𝑉∞ − 𝑉1 =
t3 = 600 ∆𝒕𝟐 = 600 V2 = 𝑉∞ − 𝑉2 =
t4 = 900 ∆𝒕𝟑 = 900 V3 = 𝑉∞ − 𝑉3 = ……….
t5 = 1200 ∆𝒕𝟒 = 1200 V4 = 𝑉∞ − 𝑉4 =
t6 = 1500 ∆𝒕𝟓 = 1500 V5 = 𝑉∞ − 𝑉5 =
𝑡∞ --- 𝑽∞ = --- ---

∆𝑦
Slope of the line (k) =
∆𝑥
Calculate the slope by taking ∆𝑥 = � (𝑥2 − � 𝑥1 ) and the corresponding ∆𝑦 = (𝑦2 − � 𝑦1 ) values.

The value of the rate constant of the reaction is k = ____________ sec-1 (from the graph).

i. What is the rate constant of a first-order reaction if the half-life is 20 minutes? Provide the
equation relating the rate constant (k) and the half-life (t1/2) for a first-order reaction.
ii. Discuss the factors that can affect the rate constant of a chemical reaction. How would you
experimentally investigate the effect of temperature on the rate constant?
iii. Differentiate between the rate constant and the reaction rate. How are they related, if at all, in
a first-order reaction?
iv. Discuss the graphical methods used to determine the rate constant of a chemical reaction.

N.A.

13. Assessments:
INTERNAL:
 Performance: 10
 Viva: 10


EXPERIMENT NO. 10: CHEMICAL ANALYSIS OF A SALT
1. Aim/Purpose of the Experiment: The aim of the experiment is to analyze an unknown inorganic salt
qualitatively.
2. Learning Outcomes: After the competition of the experiment, students would be able to analyze
different specific properties of acidic and basic radicals and predict the composition of an inorganic salt.
Apparatus:
Test tube, Bunsen burner, Beaker, Platinum wire, etc.
Reagents:
Radical specific reagents are to be used.

Sample No.:
Physical properties:
Colour of the sample:
Odour of the sample:
Texture of the sample:
Solubility:

I. Preliminary Tests (Dry tests) for acid radicals of unknown sample:

Experiment Observation Inference
Add dilute Effervescence of colourless and odourless gas Carbonate (CO32-) may
H2SO4 to a which turns lime water milky. be present.
little dry
sample in a test (No effervescence of colourless and odourless (Carbonate (CO32-) may
tube and warm gas) be absent)
if required. Evolution of colourless gas having a smell of Sulphide (S2-) may be
rotten egg which turns Lead Acetate paper present.
black.
MS + H2SO4  MSO4 + H2S
H2S + Pb(Ac)2  PbS ↓ + 2AcOH
(No Evolution of colourless gas having a smell (Sulphide (S2-) may be

of rotten egg) absent)
Evolution of colourless gas having a smell of Sulphite (SO32-) may be
burnt Sulphur turning K2Cr2O7 paper green. present.
(No evolution of colourless gas having a smell (Sulphite (SO32-) may

of burnt Sulphur) be absent)
Smell of burnt sulphur with deposition of Thiosulphate (S2O32-)
sulphur. may be present.
(No smell of burnt sulphur with deposition of (Thiosulphate (S2O32-)

sulphur) may be absent)
Evolution of brown fumes. Nitrite (NO2-) may be
present.

(No evolution of brown fumes) (Nitrite may be absent)

Add Evolution of brown fumes. Nitrate (NO3-), Nitrite
concentrated (NO2-) may be present.
H2SO4 to a
little dry (No evolution of brown fumes) (Nitrite may be absent)
sample in a test Evolution of colourless gas with pungent smell; Chloride (Cl-) may be
tube and warm. dense white fumes when a glass rod moistened present.
with NH4OH is held at the mouth of the test
tube.
(No evolution of colourless gas with pungent Chloride (Cl-) may be

smell) absent.
Evolution of reddish brown gas. Bromide (Br-), Bromate
(BrO3-) may be present.
(No evolution of reddish brown gas) (Bromide (Br-),

Bromate (BrO3-) may
be absent.)
Evolution of violet vapour. Iodide (I-) may be
present.
(No evolution of violet vapour) (Iodide (I-) may be

absent)
Evolution of a colourless gas, turning water Fluoride (F-) may be
drop held in a glass tube waxy followed present.
by oily appearance of the test tube.
(Fluoride (F-) may be
(No evolution of gas) absent)

II. Wet tests (Confirmatory tests) for acid radicals of unknown sample:
Sample preparation: Dissolve a pinch of sample in about 50 ml of distilled water in a test

tube (for water soluble samples).
1. Take a little volume of sample solution in a test tube, A brown ring Nitrate
add almost equal volume of Ferrous Sulphate solution, appears at the (NO3-)
then add concentrated H2SO4 through the side of the junction of the present and
test tube. two layers. confirmed.
MNO3 + FeSO4  Fe2(SO4)3 + NO + MHSO4 + H2O (No brown (Nitrate is

(Fe(H2O)6)SO4+NO  (Fe(H2O)5NO)SO4+H2O ring appears) absent)
2. Take a little volume of sample in a test tube, add few A white ppt Cl- present
drops of Nitric acid and then AgNO3 solution. forms which is and
soluble in confirmed.
KCl + AgNO3  AgCl + KNO3 NH4OH
AgCl + NH4OH  Ag(NH3)2)Cl + 2H2O solution.
(Chloride is
(No white ppt) absent)
3. Take a little volume of sample in a test tube, add The solution S-2 present
Sodium Nitroprusside Solution. turns violet. and
confirmed.
Na2S + Na2[Fe(CN)5NO)]  Na4[Fe(CN)5(NOS)] (No violet (Sulphide is
colouration) absent)
4. Take a little volume of sample in a test tube, add few ml White ppt SO4-2
of HCl, then add BaCl2 solution. forms. present and
confirmed.
Na2SO4 + BaCl2  BaSO4 + 2NaCl (No white ppt) (Sulphate is
absent)

III. Preliminary Tests (Dry tests) for basic radicals of unknown sample:
i. Dry test tube heating:

Take a little First the sample becomes white, Cu salt may be present
sample in a clean then turns black.
dry test tube and (No such observation) (Cu salt may be absent)
heat first gently Yellow when hot and yellow Pb salt may be present
and then strongly when cold.
with a burner. (No such observation) (Pb salt may be absent)
Yellow when hot and white when Zn salt may be present
cold.
(No such observation) (Zn salt may be absent)
White when hot, white when Ca, Mg, Na, K, Al, Ba salts
cold. may be present.
(No such observation) (Ca, Mg, Na, K, Al, Ba salts
may be absent)
Brown residue forms. Fe salt may be present.
(No such observation) (Fe salt may be absent)
White sublimate forms. NH4+ salt may be present.
(No such observation) (NH4+ salt may be absent)
ii. Special test for NH4+:

A little sample was Colourless pungent smell, on NH4+ present and
heated with soda lime. holding a glass moistened with confirmed.
HCl white fumes appears.
(No such observation) (NH4+ salt is absent)

iii. Flame test:

A pinch of Bluish green flame Cu salt may be present
sample is Bluish white flame Pb salt may be present
taken on the Apple green flame Ba salt may be present
tip of a Brick red flame Ca salt may be present
platinum wire Dazzling golden yellow flame in naked eye Na salt may be present
and held into but becomes colourless when observed
Bunsen through double blue glass.
burner flame Violet when observed through naked eye K salt may be present
carefully. but becomes crimson red when observed
through double blue glass.
IV. Wet tests (Confirmatory tests) for basic radicals of known sample:
Sample preparation: Dissolve a pinch of sample in about 50 ml of distilled water in a test tube
(for water soluble samples).
Dissolve a small amount sample in dilute HCl

White ppt., may be Pb2+ No ppt formed.
1. Ppt dissolves on heating
but reappears on cooling. To one part of the solution, add Ammonium Hydroxide
2. Dilute the mixture, heat slowly in excess. First greenish ppt forms slowly in excess,
to dissolve, add a little KI then the whole solution becomes deep blue – Cu2+ confirmed.
solution. To the other part of the solution, add few drops of
Yellow ppt forms, concentrated HNO3 and excess NH4Cl, mix and then add
dissolves on boiling. NH4OH in excess.
Needle shaped golden ppt White or Brown ppt. No ppt formed.
2+
appears on cooling – Pb
confirmed. White ppt forms.

Boil the mixture and add To one part of the solution

NH4Cl, ppt dissolves – Al3+ dilute HCl was added, then
confirmed. NaOH was added drop wise.
White ppt forms,
Brown ppt forms. dissolves giving a colourless
Dissolve it in dilute HCl, then solution – Zn2+ confirmed.
add Potassium Ferrocyanide. To the other part, add
Blue ppt of Prussian Blue saturated solution of
forms – Fe3+ confirmed. Ammonium Carbonate.
White ppt appears – Ba2+,
Ca2+ may be present.
No ppt formed.
Add Na2HPO4 solution.

White ppt forms – Mg2+
confirmed.

 Before the wet test to be performed it should be ensured that the sample becomes completely
soluble in solvent.
 The platinum wire should be handles very cautiously, as it is very costly apparatus.
 For dry test the test tube should be clean and dry.
 To perform the dry test sample should be taken in a minimum quantity to get better result.
 Bunsen burner flame to be used very cautiously.


N.A.


Hence, the provided inorganic salt contains ___________ as an acid radical and ___________ as a basic
radical.

i. Why Zn salt is yellow when hot and white when cold?
ii. What is the chemistry of flame test?
iii. Why is conc. HCl is used in flame test?
iv. Why K2Cr2O7 paper turns green when hold over mouth of the test tube of hot Sulphite salt?
Exp. 10(A): Systematic qualitative analysis for acid radicals of a known sample.
Exp. 10(B): Systematic qualitative analysis for basic radicals of a known sample.
Exp. 10(C): Systematic qualitative analysis for acid and basic radicals of an unknown sample.
13. Assessments:
INTERNAL:
 Performance: 10
 Viva: 10



BSCD291 Lab Manual

Uploaded by

Document Information

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

BSCD291 Lab Manual

Uploaded by

Copyright:

Available Formats

B.Tech.

CSE (DS) – 2023

1 Determination of dissolved oxygen present in a given water sample. 2-5

To determine chloride ion in a given water sample by

3 Saponification/acid value of oil. 10-13

Determination of cell constant of a conductivity cell using 0.1M

7 Determination of viscosity Coefficient. 29-33

8 Thin layer chromatography. 34-37

9 Determination of the rate constant of a reaction. 38-43

10 Chemical analysis of a salt. 44-51

Mr. Akshay Kumar Dey

EXPERIMENT NO. 1: DETERMINATION OF DISSOLVED OXYGEN PRESENT IN A GIVEN

3. Prerequisites: 12th level Chemistry

5. Introduction and Theory:

Mr. Akshay Kumar Dey

7. Precautions and/or Troubleshooting:

Mr. Akshay Kumar Dey

8. Observations & Presentation of Data:

Room Temperature: ………. 0C

9. Calculations & Analysis:

10. Result & Interpretation:

11. Follow-up Questions:

Mr. Akshay Kumar Dey

12. Extension and Follow-up Activities (if applicable):

14. Suggested readings:

Mr. Akshay Kumar Dey

EXPERIMENT NO. 2: TO DETERMINE CHLORIDE ION IN A GIVEN WATER SAMPLE BY

3. Prerequisites: 12th level Chemistry

5. Introduction and Theory:

2 AgNO3 + K2CrO4 = Ag2CrO4 (Brick-red ppt) + 2 KNO3

Mr. Akshay Kumar Dey

7. Precautions and/or Troubleshooting:

8. Observations & Presentation of Data:

Room Temperature: ………. 0C

Table 1: Blank titration.

Mr. Akshay Kumar Dey

Table 2: Sample titration.

9. Calculations & Analysis:

10. Result & Interpretation:

11. Follow-up Questions:

12. Extension and Follow-up Activities (if applicable):

Mr. Akshay Kumar Dey

14. Suggested readings:

Mr. Akshay Kumar Dey

EXPERIMENT NO. 3: SAPONIFICATION/ACID VALUE OF OIL

3. Prerequisites: 12th level Chemistry

5. Introduction and Theory:

Mr. Akshay Kumar Dey

Where 56.1 is the equivalent weight of KOH

Step 2: Estimation of acid value of supplied oil:

7. Precautions and/or Troubleshooting:

8. Observations & Presentation of Data:

Room Temperature: ………. 0C

Mr. Akshay Kumar Dey

Table 1: Standardization of Sodium Hydroxide solution.

Table 2: Estimation of acid value.

9. Calculations & Analysis:

Mr. Akshay Kumar Dey

10. Result & Interpretation:

11. Follow-up Questions:

12. Extension and Follow-up Activities (if applicable):

14. Suggested readings:

Mr. Akshay Kumar Dey

EXPERIMENT NO. 4: DETERMINATION OF THE CELL CONSTANT OF A CONDUCTIVITY