21 Scheme Chemistry Lab Manual
21 Scheme Chemistry Lab Manual
21 Scheme Chemistry Lab Manual
Name:
Section:
Batch:
Branch:
USN:
Vision: “To be recognized as a premier technical and management institution promoting extensive
education fostering research, innovation and entrepreneurial attitude"
Mission:
collaborative learning.
-sd-
Principal
DEPARTMENT OF CHEMISTRY
MAHARAJA INSTITUTE OF TECHNOLOGY MYSORE
VISION:
Dept. of Chemistry, MIT, Mysore 3
Foster technologically relevant chemical education in engineering
applications to bring about excellence in research and innovation.
MISSION:
To endow relevant knowledge in chemical science with eminent teaching
and demonstration.
-sd-
HOD
DO’s:
DONT’s:
Do not walk around in the lab unnecessarily.
Do not go out of the lab without permission.
Do not eat, smoke or drink in the laboratory.
Do not walk barefoot in the laboratory.
Never do unauthorized experiment.
Never taste any chemicals.
Do not use any equipment or chemicals unless you are trained and
approved as a user by your supervisor.
GENERAL INSTRUCTIONS
CONTENTS OF EXPERIMENTS
Sl. Date Part – A Marks
No INSTRUMENTAL ANALYSIS
Dept. of Chemistry, MIT, Mysore 8
.
Part – B
VOLUMETRIC ANALYSIS
INSTRUMENTAL
EXPERIMENTS
PART - A
Dept. of Chemistry, MIT, Mysore 10
Capillary Tube
Fig. Viscometer
PART - A
INSTRUMENTAL EXPERIMENTS
h d g r4t
8V l
Where h is the coefficient of viscosity of the liquid, V = volume of the
liquid, r = radius of the tube, 1 = length of the tube, P is the pressure
difference between the two ends of the tube, h = height of the capillary tube,
d = density of the liquid, and g = gravitational force. If equal volumes of two
different liquids are allowed to flow through the same tube under identical
w t d
w w
conditions, then, L tLd L
ηw t L d L
hL = t w dw
Liquid Number =
ηw t L d L
hL = t w d w =______________________
= ...................milli poise
RESULT:
The viscosity co – efficient of given liquid = ________ milli poise
Dept. of Chemistry, MIT, Mysore 13
and is inversely proportional to the temperature (T), i.e. h α 1/ T. Hence
the measurements are carried out at constant temperature.
PROCEDURE:
1. Transfer the known volume (say 15 ml) of the given organic liquid taken
in a burette into the viscometer. Suck the organic liquid above the upper
mark ‘A’ in the viscometer and allow it to flow freely through a capillary.
Start the stop clock when the liquid level just crosses the upper mark ‘A’
and stop it when the liquid level just crosses the lower mark ‘B’ in the
viscometer. Note down the time of flow of liquid in seconds (t l) and repeat
the experiment to get agreeing values.
2. Pour out the organic liquid and rinse the viscometer in acetone again.
Dry it in an electric oven and fix the viscometer vertically to a stand.
4. Determine the viscosity co-efficient of the given organic liquid using the
relation,
ηw t L d L
hL = t w dw and the given values of hw, dw and dL.
Note: -Transfer the organic liquid into the bottle after the experiment is
completed and rinse the viscometer with acetone and keep it in an
electric oven.
Dept. of Chemistry, MIT, Mysore 14
OBSERVATIONS AND CALCULATIONS
Volume of
NaOH pH pH pH/V
added in ml
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
6.5
7.0
7.5
8.0
8.5
9.0
9.5
10.0
Dept. of Chemistry, MIT, Mysore 15
EXPERIMENT NO.2 Date:
THEORY:
The strength of an acid is experimentally measured by determining its
equilibrium constant or disassociation constant (Ka). Strong acids are
completely ionized in aqueous solution and hence it is impossible to
determine the disassociation constant of strong electrolytes. But in case of
weak electrolytes are partially ionized in aqueous solution and hence the
equilibrium constant of weak electrolytes can be experimentally determined.
Let us consider weak acid like formic acid, which ionizes, freely in aqueous
solution as,
ka
HCOOH (aq) + H2O (l) H3O+ (aq) + HCOO- (aq)
HCOO H O
3
\Ka = HCOOH
pKa is a modern method of expressing the strength of weak acid ,
ie., pKa = - log10 Ka
pKa value is determined by measuring the changes in pH of acid solutions at different
amount of the base added. In the titration of an acid with a base, the pH of the solution rises
gradually at first and then more rapidly. At the equivalence point there is a very sharp
increase in pH for a very small quantity of base added. Beyond the equivalence point, the pH
increases slightly on addition of base. The titration curve is obtained by plotting change in pH
against different volume of the base added and from the graph, determined the equivalence
point of an acid. The pKa value of an acid can be calculated using Henderson equation ,
Salt
pH = pKa + 1og10 Acid
At half equivalence point [salt] = [acid] and hence pH at half
equivalence point gives the pKa value of weak acid, i.e. pH = pKa .
Dept. of Chemistry, MIT, Mysore 16
Scale :
Graph No.: 2 1
pH Scale :
HEP
Volume of NaOH added in ml
RESULTS:
PROCEDURE:
Make up the given weak acid in a 100 ml standard flask to the mark
by adding distilled water and mix well for uniform concentration. Pipette out
25 ml of the given weak acid into a clean 100 ml beaker.
Connect the glass and calomel combined electrode to the pH meter
and immerse the electrode in to the acid taken in a beaker. Measure the pH
of the acid . Add 0.5 ml of sodium hydroxide solution taken in a micro
burette in to the acid, stir well and measure the pH of the acid and continue
the addition of sodium hydroxide until the sudden raise in the pH of the
acid occur. Then take few more readings and take the difference in the pH of
acid (DpH) and the volume of sodium hydroxide added (DV). Plot the graph,
DpH/DV against the volume of sodium hydroxide added (graph No.1) and
from the graph 1, determine the equivalence point of the acid. Plot the
graph, pH against the volume of sodium hydroxide added (graph No 2).
Determine the half equivalence point that gives the pKa value of weak acid
by using the graph 2.
Dept. of Chemistry, MIT, Mysore 18
OBSERVATIONS AND CALCULATIONS
added added
in ml (V ) in ml (V )
0.0 5.5
0.5 6.0
1.0 6.5
1.5 7.0
2.0 7.5
2.5 8.0
3.0 8.5
3.5 9.0
4.0 9.5
4.5 10.0
5.0
Scale :
X –axis, 1.0 cm = _______ ml of K2Cr2O7
E
Y –axis, 1.0 cm = _______ V
THEORY:
When the electrode is dipped in the solution, the potential of an
electrode depends on the concentration of the ions in the electrolyte.
Therefore determination of maximum potential can serve as an indicator in
potentiometric analysis. Determination of change of potential with
concentration gives more accurate results than volumetric analysis.
Where Ecell = emf of the cell, E°cell standard emf of the cell, n = number of
electrons involved in the reaction, [products] = concentration of the products
and [reactants] = concentration of the reactants.
Dept. of Chemistry, MIT, Mysore 20
Note:
1. Normality of K2Cr2O7 = N K2Cr2O7 = 0.1 N
2. Equivalent weight of Mohr’s salt = 392
N K Cr O7 ×V K
\ Normality of Mohr’s salt solution =
2 2 2
Cr2 O 7
V Mohr ’s salt
N Mohr’ s salt
= 25 =_____________ N
PROCEDURE:
Make up the given Mohr’s salt solution in a 100 ml standard flask to
the mark by adding distilled water and mix well for uniform concentration
Pipette out 25 ml of Mohr’s salt solution in to a clean 100 ml beaker followed
by adding one t.t. of dilute sulphuric acid and stir well using a glass rod.
Connect the platinum and calomel electrodes to the potentiometer,
and immerse the electrodes in to the Mohr’s salt solution taken in a beaker.
Measure the emf of the solution. Add 0.5 ml of potassium dichromate
solution in to the Mohr’s salt solution, stir well and measure the emf of the
solution and continue the addition of potassium dichromate added until the
sudden raise in the emf of solution occur. Then take few more readings and
take the difference in the emf of solution (DE) and the volume of potassium
dichromate added (DV). Plot the graph, DE / DV against the volume of
potassium dichromate added. From the graph, determine the volume of
potassium dichromate required to rapid increase in the emf of the solution.
Calculate the weight per liter and weight per 100 ml of Mohr’s salt.
Scale :
X –axis, 1.0 cm = _______ ml of NaOH
V1 V2
Volume of NaOH added in ml
Dept. of Chemistry, MIT, Mysore 23
EXPERIMENT NO. 5 Date:
N NaOH x V1
Normality of HCl = ----------------------------
V Acid Mixture
0.2 x
=-------------------= ------------N
50
= --------------------X 36.5
X= -----------------------g
X
Weight per 100 ml of HCl = = ------------ = ---------- g
10 10
Estimation of CH3COOH
0.2 x
=----------------= ------------N
50
Weight per liter
of CH3COOH = Y = N C H COOH X Equivalent weight of CH3COOH
3
= --------------------X 60
Y= -----------------g
Y
Weight per 100 ml of CH3COOH = = ------------ = ---------- g
10 10
RESULT:
1. Amount of HCl present in the given solution =…….………g
10 3.93 x 10 = 39.30 10 x 1 = 10
15 3.93 x 15 = 58.95 15 x 1 = 15
20 3.93 x 20 = 78.60 20 x 1 = 20
25 3.93 x 25 = 98.25 25 x 1 = 25
Calculation:
Scale:
Concentration of Cu in mg/ml
Dept. of Chemistry, MIT, Mysore 27
EXPERIMENT NO. 5 Date:
THEORY:
\ Io = I a + I t
A = log Io / It = ε ct.
C
=
\ V ml of copper sulphate = V = 1.0 1.0 = ________ml
Results:
PART - B
INSTRUCTIONS TO THE STUDENTS:
PIPETTE
1. Wash pipette with tap water and then rinse with distilled water.
2. Rinse pipette with a small quantity of the solution to be taken in
burette and discard the solution into sink.
3. During transferring solution into a clean conical flask, when all the
solution from the pipette flows out, touch the tip of the pipette to the
bottom of the flask gently.
4. Do not blow out the last drops of the liquid from the pipette.
CONICAL FLASK
1. Wash conical flask with tap water and then rinse with distilled water.
2. Do not try to drain out the water particles from the conical flask.
3. Do not rinse the conical flask with the solution to be taken in the
conical flask.
4. During the titration, place the conical flask on a glazed white tile below
the burette.
Dept. of Chemistry, MIT, Mysore 32
x 4
MEDTA = 372.24 = ____________ (a) M
Final readings
Initial readings
Volume of EDTA
run down in ml
diamine tetra acetic acid (EDTA) which form complex with Ca 2+ and Mg2+
ions. The EDTA molecule has two easily replaceable hydrogen atoms and
hence the EDTA form complex with metal ion present in water. Reaction can
hardness of the water is usually expressed in terms of ppm (ie, parts per
salt of EDTA is used as reagent for preparing the solution. The structures of
EDTA ( H4Y ) and disodium salt of EDTA (Na2H2Y) are given below.
(MV )EDTA ×
M Hard water = = = ________M
V Hard water 25
Weight of CaCO3 equivalent hardness per liter = M Hard water × Mol . wt of CaCO 3
= × 100 = _____ = a
a ×106
106 ml (1 million ml ) of hard water sample contains = ppm of CaCo 3
1000
= …………… p pm of CaCo3
Thus total hardness of the given water sample = …………… ppmof CaCo 3
PROCEDURE:
standard flask using a glass funnel. Dissolve the crystals by adding ½ t.t. of
ammonium hydroxide and little distilled water. Make up the solution to the
mark by adding distilled water and mix well for uniform concentration.
Pipette out 25ml of the given water sample into a clean conical flask
against EDTA solution taken in a burette until the wine red colour changes
to purple blue. Note down the volume of EDTA added and repeat the
REACTIONS:
x 4
MEDTA = 372.24 = ____________ (a) M
Final readings
Initial readings
Volume of EDTA
run down in ml
PROCEDURE:
(MV ) EDTA ×
M Cement =
V Cement
= 25
= ________M
= ________g =a
a
Percentage of CaO in the given cement solution = ×1 00=−−−−−−¿
W
RESULT: The Percentage of CaO present in the given cement solution = ____
Dept. of Chemistry, MIT, Mysore 39
Pipette out 25ml of the given cement solution into a clean conical
flask. Add 5ml of 1:1 glycerol, 5ml of diethyl amine and 10ml of 2N sodium
hydroxide. Add 2-3 drops of Patton- Reeder’s indicator. Shake well and
titrate this against EDTA solution taken in a burette until wine red color
changes to purple blue. Note down the volume of EDTA added and repeat
the experiment for concordant values. Calculate the percentage of calcium
oxide in the given cement solution.
REACTIONS:
Weight of FAS 4
Normality of FAS = Equivalent weight of FAS
×4
N FAS = = __________(a) N
392
Final readings
Initial readings
THEORY:
PROCEDURE:
V2 = ________=________ml
(NV )FAS ×
N Waste water =
V Waste water
= 25
= ________N
= ………….× 8× 1000 mg dm 3
= …………..mgdm 3
RESULT: The COD value of the given waste water= ______ mg of oxygen/dm 3
Dept. of Chemistry, MIT, Mysore 43
REACTIONS:
THEORY:
The chief constituents of brass alloy are copper and zinc. It also contains
small quantities of tin, lead and iron. The percentage composition of a
typical brass alloy is given below.
PROCEDURE:
(NV )Na S O ×
N Brass solution= 2 2
= 3
= ________N
V Brass solution 25
= ________g =a
a
Percentage of copper in the given brass solution = ×100
W
= __________________
= ________
II Estimation of copper:
Pipette out 25 ml of brass solution into a clean conical flask and add
dilute ammonium hydroxide drop by drop until bluish white precipitate is
formed. Dissolve the ppt. by adding dilute acetic acid drop by drop and then
add 1/ 4 t.t. of acetic acid in excess. Add one t.t. of 10% potassium iodide
solution and shake well. Titrate the liberated iodine against standard
sodium thiosulphate solution taken in a burette using starch as indicator
towards the end point. (Add starch when brown solution changes to whitish
yellow). Disappearance of blue colour is the end point. Note down the
volume of hypo added and repeat the experiment for concordant values.
Calculate the percentage of copper in the given sample of brass.
REACTIONS:
heat
Cu + 4 HNO3 Cu (NO3)2 + 2 H2O + 2 NO2
(Reddish brown)
Weight of K 2 Cr2 O 7 4
x4
__________(a) N
N K2Cr2O7 = 49
THEORY:
Rust contains mainly hydrated ferric oxide (Fe 2O3. n H2O). The
solution of rust is made by dissolving the sample of rust in dilute HCl. The
resultant clear solution contains ferric chloride (FeCl 3). The ferric ions (Fe3+)
present in rust solution are redused to ferrous ions(Fe 2+) by adding stannous
chloride(SnCl2) under hot condition in the presence of HCl. The excess
stannous chloride is removed by the addition of mercuric chloride (HgCl 2)
solution. The resulting solution having ferrous ions is titrated against
standard potassium dichromate using potassium ferricyanide as an external
indicator.
PROCEDURE:
(NV ) K 2 Cr 2O 7 ×
N Rust soln= = = ________
V Rust soln 25
×55.85
= = ……... g = a
4
a
Percentage of iron in the given rust solution = ×100=−−−−−−¿
W
= _________
RESULT: The Percentage of iron present in the given rust solution =…….
Dept. of Chemistry, MIT, Mysore 52
b) Estimation of iron:
Pipette out 25ml of the rust solution into a clean conical flask. Add ¼
t.t of concentrated hydrochloric acid and heat the solution nearly to boiling.
Add stannous chloride drop by drop taken in a separate burette till yellow
color solution becomes colorless and then add 2-3 drops of stannous
chloride in excess. Cool the solution to lab temperature then add one t.t of
distilled water and add 10ml of saturated mercuric chloride at once. Shake
well and a silky white precipitate is formed. (If no ppt or black ppt is formed,
reject and repeat the experiment). Then titrate this solution against
standard potassium dichromate solution taken in a burette, using
potassium ferricyanide as an external indicator. The end point is failure to
observe blue color when one drop of the titrated mixture is brought in
contact with a drop of the indicator placed on paraffin paper. Note down the
volume of potassium dichromate added and repeat the experiment for
concordant values. Calculate the percentage of iron in the given sample of
rust solution.
REACTIONS:
heat
Fe2O3 + 6HCl 2FeCl3 + 3 H2O
(Rust) [Ferric chloride)
SCHEME OF VALUATION
DESCRIPTION Part-A Part-B Max. marks
Procedure write up 08 07 15
Conduction 26 26 52
Calculation, graph 09 09 18
works and Result
Viva- Voice 07 08 15
Part A
Potentiometry, Colorimetry Pka and Viscosity Conductometry
and Flame Photometry
Error (cm3) Marks Error (cm3) Marks Error (cm3) Marks
±0.5 13 + 13 ±5 13 + 13 ±0.5 13 + 13
±0.5 to 0.6 11 + 11 ±5.1 to 6 11 + 11 ±0.51 to 0.6 11 + 11
±0.6 to 0.7 9+9 ±6.1 to 7 9+9 ±0.61 to 0.7 9+9
±0.7 to 0.8 7+7 ±7.1 to 8 7+7 ±0.71 to 0.8 7+7
±0.8 to 1.0 5+5 ±8.1 to 10 5+5 ±0.81 to 1.0 5+5
DEMONSTRATION EXPERIMENTS
(For CIE)
25
Flame photometric reading
20
15
10
5
a
0
0 5 10 15 20 25
Volume of sodium solution
= x 100 ppm
50
= ----------- ppm
THEORY:
Flame photometry is an atomic emission technique used for the
salts is sprayed into the flame, electrons in the metal ions of the vapour gain
thermal energy and get excited from lower energy level E1 to higher energy
return to the ground state by emitting radiations (En – E1 = h) which are
as K, Ca, Li, etc is based on the fact that these elements impart
characteristic colors to the Bunsen flame and the brightness of the flame
these elements. It is simple and rapid method for the estimation of alkali
particular element is placed between the flame and the detector. The sample
Radiation from the resulting flame is collected by the lens and allowed to
radiation of the element under determination to the photo cell. The output
= x 100 ppm
50
= ----------- ppm
Result:
The amount of sodium present in the given test solution is----------- ppm
The amount of potassium present in the given test solution is----------- ppm
Procedure:
Dept. of Chemistry, MIT, Mysore 58
Result:
The amount of sodium present in the given test solution is----------- ppm
The amount of potassium present in the given test solution is----------- ppm
Dept. of Chemistry, MIT, Mysore 59
OBSERVATION AND CALCULATION
X 10
= 287.6
= ………………..
Dept. of Chemistry, MIT, Mysore 60
DEMONSTRATION EXPERIMENT NO. 2 Date:
THEORY:
PROCEDURE:
Outcome:
VIVA QUESTIONS
Part-A
1. What is weak acid?
2. What is pKa of a weak acid?
3. Define pH.
4. What is Ka?
5. How are pH and pKa related?
6. What are the electrodes used in the measurement of pH for the determination of pKa?
7. Why half equivalent point is taking for calculating pKa value of weak acid?
8. What is viscosity?
9. What is viscosity coefficient of a liquid?
10. What is the SI unit of viscosity coefficient?
11. How does the viscosity vary with temperature?
12. Write the expression used to calculate the viscosity coefficient of liquid.
13. Why is the same volume of water and liquid used in the determination of viscosity?
coefficient of liquid?
14. Which reference electrode is used in the determination of ferrous ammonium sulphate
potentiometrically?
15. What is meant by transmittance?
16. What is absorbance?
17. Define Bear – Lambert’s law.
18. What is the relation between absorbance and concentration?
19. What is a blank solution?
20. Which compound of copper is responsible for the deep blue color in the colorimetric
determination of copper?
21. Why is ammonia added to copper sulphate solution in the colorimetric determination of
copper?
22. Why is the estimation of copper done at 620 nm wavelengths?
23. What is the wave length used in the colorimetric determination of iron?
24. Why is potassium thiocyanate solution added to ferric alum solution in the colorimetric
determination of iron?
25. Which compound of iron is responsible for the red color in the colorimetric
determination of iron?
26. What is conductance?
27. What is the unit for conductance?
28. What is emf of the cell?
29. What is cell constant? Mention its unit.
30. Why is conductance of HCI decreases on adding NaOH before the end point?
31. Why is the conductance of HCI increases on adding NaOH after the end point?
32. What is an electrolyte?
33. What are types of electrolyte? And give example for each?
Part-B
1. What is an acid and base?
2. What is meant by titration?
3. What is end point?
4. What is a standard solution?
5. What is standardization?
6. What is estimation?
7. Define normality.
8. Define molarity.
10. What is an indicator? And mention the different types of indicators.
11. What is an oxidation and reduction?
12. What is an oxidising and reducing agents?
13. What is an hard water?
14. How is hardness of water caused?
Dept. of Chemistry, MIT, Mysore 62
15. What are the types of hard water?
16. What are the causes of temporary and permanent hardness of water?
17. How is temporary and permanent hardness of water removed?
18. How do you express the total hardness of water?
19. Name the metal ion indicator.
20. What is EDTA?
21. What are buffer solutions?
22. Mention types of buffer solutions.
23. Why is ammonia-sodium chloride buffer solution is added in the determination of total
hardness of water?
24. What is the end point in the determination of total hardness of water?
25. What are the constituents of cement?
26. Which indicator used in the determination of CaO in cement solution?
27. Why the diethylamine and glycerol added to the cement solution?
28. What is an ore?
29. What is the main constituent of haematite ore?
30. What is the role of stannous chloride in the determination of iron in haematite ore
solution?
31. Why is mercuric chloride added in the determination of iron in haematite ore solution?
32. What happens when the excess of stannous chloride is not removed in the
determination iron in haematite ore solution?
33. What is the indicator used in the determination of iron in haematite ore solution?
34. Whyis potassium ferricyanide cannot be used as an internal indicator in the analysis of
haematite ore?
35. What is the colour of K3[Fe(CN6] with ferrous ion?
36. Why is the colour of the indicator drop remains the same at the end point in the
determination of iron in haematite ore?
37. What is an alloy?
38. What are the constituents of brass?
39. How is a brass solution prepared?
40. What is the purpose of adding urea to the brass solution?
41. Why is ammonium hydroxide added to the brass solution in the determination of copper?
42. Why is acetic acid added to the brass solution in the determination of copper?
43. Why is KI added to the brass solution although copper is present in brass solution?
44. Why is the blue solution of brass turns brown upon the addition of KI solution?
45. Why is starch indicator added towards the endpoint in iodometric titrations?
46. What is the white precipitate left at the end point in the determination of copper in
brass?
47. What is hypo?
48. What is Mohr’s salt?
49. What are the salts present in Mohr’s salt?
50. Why is sulphuric acid added during the preparation of Mohr’s salt solution?
51. What is a hydrolysis?
52. What is chemical oxygen demand (COD)?
53. What is biological oxygen demand (BOD)?
54. What is the role of silver sulphate in the determination of COD?
55. What is role mercuric sulphate in the determination COD?
56. What is the indicator used in COD experiment?
57. What is the colour change at the end point in the determination of COD?
58. Why COD value always greater then BOD value.
Dept. of Chemistry, MIT, Mysore 63