R.V.

COLLEGE OF ENGINEERING
(An Autonomous Institution under VTU, Belagavi)
DEPARTMENT OF CHEMISTRY
STUDY MATERIAL - TABLE OF CONTENTS

EXP. NO. TITLE OF THE EXPERIMENT PAGE NO.

VOLUMETRIC ANALYSIS & PREPARATION
1. Determination of total hardness of water 1
2. Estimation of percentage of Copper in Brass by Iodometric 3
titration
3. Estimation of Iron in the given sample of Haematite ore 5
solution by Redox titration
4. Determination of Chemical Oxygen Demand (COD) of the given 7
industrial waste water sample (Self-learning experiment)
5. Determination of Dissolved Oxygen in the given water sample 9
by Winkler’s method
6. Preparation of Polystyrene by Bulk Polymerization method 11
7. Preparation of ZnO by Solution Combustion method 12

INSTRUMENTAL METHODS OF ANALYSIS

8. Determination of pKa of a weak acid using pH meter 13
9. Potentiometric titration – Estimation of FAS using standard 14
K2Cr2O7 solution. (Self-learning experiment)
10. Colorimetric estimation of Copper 16
11. Conductometric estimation of HCl using standard NaOH 18
solution
12. Determination of Viscosity Coefficient of a given liquid using 20
Ostwald’s Viscometer (density of the liquid to be given)
13. Flame Photometric estimation of Sodium in the given saline 21
solution
14. Determination of relative and Kinematic Viscosities of given 22
lubricating oil at different temperatures using Redwood
Viscometer
15. To find Tg of polymer using DSC 23
VOLUMETRIC ANALYSIS & PREPARATION and repeat the titration to get concordant
values.
EXPERIMENT NO – 1
Structure of compounds:
Aim:
Determination of total hardness of water by NaOOC CH2 H2C COONa
Complexometic titration
:N CH2 CH2 N:
Description: HOOC CH2 H2C COOH
Part-A: Preparation of standard EDTA solution:
Weigh the Weighing Bottle containing disodium
Disodium salt of EDTA
salt of EDTA (dissolves fast and completely in
OH
water) accurately and transfer the salt onto the
funnel placed on a 100 cm3 volumetric flask. Weigh N
N
the Bottle again. The difference between the two OH
weights will give the amount of EDTA transferred. SO3H
Add about 2 cm3 of Ammonia followed by water.
Dissolve the salt by adding about 20-30 cm3 of de- NO2
ionized water. Make up the solution to the mark
EBT indicator
and shake well for uniform concentration.

Part-B: Estimation of hardness of water:

Pipette out 25 cm3 of the given sample of hard
water into a clean conical flask. Add 3 cm3 NH3-
NH4CI buffer followed by a pinch of Eriochrome
black-T indicator. Titrate this against EDTA taken
in a burette till the colour changes from wine red
to pure blue. Note down the burette reading
Metal Complex of EDTA

VIVA QUESTIONS
1 What is Hard water?
2 How are the waters classified based on the degree of Hardness?
3 How is Hardness of water caused?
4 How temporary hardness is removed?
5 How do you express the total Hardness of water?
6 What is EDTA?
7 Write the structural formula for EDTA.
8 Why is disodium salt of EDTA preferred to EDTA?
9 Why is Ammonia solution added while preparing EDTA solution?
10 2.0746 g of EDTA was dissolved in 100 cm3 of water. What is the molar concentration of EDTA?
11 What is buffer solution?
12 Why is Ammonia-Ammonium Chloride buffer added?
13 What is the pH of the buffer used? How is it prepared?
14 Why is the indicator Eriochrome Black (EBT) shows wine red color at the beginning and blue color at the
end?
15 Name a metal ion sensitive indicator.
16 Why is the titration involving EDTA carried out slowly towards the end point?
17 Why is the degree of Hardness expressed in terms of CaCO3?
18 What is the application of Hardness data in environmental engineering practice?

2
19 How do you explain the color change of solution at the end point of titration?

Observation and Calculation:

Part-A: Preparation of standard EDTA solution

Weight of the Weighing Bottle + EDTA = g

Weight of the Weighing Bottle = g

Weight of the EDTA salt transferred = g

Weight of EDTA dissolved in 100 cm3 x 10

Molarity of EDTA solution = ----------------------------------------------------------
Gram molecular weight of EDTA salt (372.24)

Part-B: Estimation of hardness of water

Burette readings(in cm3) Trial-I Trial-II Trail-III

Final
Initial
Volume of EDTA run down

Part-C: Calculation

1000 cm3 of 1M EDTA = 100 g of CaCO3

Therefore ‘V’ cm3 of ‘X’ M EDTA = 100 x V x X g of CaCO3

1000

= Y grams of CaCO3

25 cm3 of hard water has hardness equivalent to ‘Y’ g of CaCO3

Therefore 106 cm3 of hard water has hardness equivalent to Y x 106 g of CaCO3
25

3
EXPERIMENT NO – 2 drop until a pale blue precipitate is obtained.
Dissolve the precipitate by adding dil. Acetic acid
Aim: drop by drop, followed by ¼ tt of Acetic acid and 1
Estimation of percentage of Copper in Brass by tt of 10% KI solution. Add a test tube of distilled
Iodometric titration water. Swirl the conical flask thoroughly for about
30 seconds. Titrate the liberated iodine against
Description: standard Sodiumthiosulphate solution taken in the
Part-A: Preparation of Brass solution burette until the solution becomes pale yellow or
Weigh exactly the given sample of Brass into a cream colored. Add about 2 cm3 of freshly
clean 250 cm3 conical flask. Add Conc. Nitric acid prepared starch solution as an indicator. Continue
drop by drop until the Brass dissolves completely. the titration by adding Sodiumthiosulphate
Add 2 tt of distilled water and about 1 g of Urea. solution strictly drop by drop until the dark blue
Boil for about 1 minute to destroy oxides of coloration disappears, leaving behind a white ppt.
Nitrogen. Cool the mixture. Repeat Part-A and B to conduct a duplicate.
Calculate the percentage of Copper present in the
Part-B: Estimation of Copper in Brass solution Brass samples.
Add 1 tt of distilled water to the solution obtained
in part-A. Add Ammonium Hydroxide drop by

VIVA QUESTIONS

1 What are the constituents of Brass?

2 How is Brass solution prepared?
3 What is the purpose of adding Urea?
4 What are Iodometric titrations?
5 Why is Ammonium Hydroxide added to the Brass solution?
6 What is the bluish white precipitate formed after adding Ammonia solution?
7 Why is the solution acidified with Acetic acid after the addition of Ammonium Hydroxide?
8 Why is Acetic acid added?
9 How is librated Iodine estimated?
10 What is the reaction that occurs between iodine and Sodiumthiosulphate?
11 Write the reaction between acidified Brass solution and Potassium Iodide.
12 Why is starch indicator added towards the end point?
13 What is the white precipitate produced at the end point?

4
Observation and Calculation:

Part-A: Preparation of Brass solution

Brass sample- 1 Brass sample –2

Weight of Brass + Weighing Bottle g g

Weight of empty Weighing Bottle g g

Weight of the Brass taken g g

Part-B: Estimation of Copper in Brass solution

Burette readings(in cm3) Trial-I Trial-II

Final

Initial

Volume of Na2S2O3 run down

Part-C: Calculation

Normality of sodium thiosulphate =‘Y’

Volume of sodium thiosulphate =‘X’ cm3

1000 cm3 1N sodium thiosulphate = 63.54g of copper

Therefore ‘X’ cm3 of ‘Y’ N sodium thiosulphate = 63.54 x X x Y g of copper

1000
= ‘A’ g of Cu

Weight of brass taken = ‘W’ g

‘W’ g of brass contains ‘A’ g of copper

Therefore 100 g brass contains Ax100 g of copper

W
= ‘B’ g Copper

5
EXPERIMENT NO – 3 Chloride in excess. Add 2 tt of demonized water
and cool the solution to room temperature,
Aim: followed by 3 cm3 of Mercuric Chloride at a
Estimation of Iron in the given sample of stretch. A silky white precipitate is formed. Reject
Haematite ore solution by Redox titration the contents of the flask and repeat the
experiment if no precipitate or greyish
Description: precipitate is formed.
Part - A: Preparation of Potassium Dichromate Titrate the solution against standard Potassium
solution Dichromate taken in the burette, using
Weigh accurately the given Potassium Potassium Ferricyanide as an external indicator.
Dichromate crystals and transfer onto the funnel In the beginning, take out a drop of the reaction
placed on a 100 cm3 volumetric flask. Dissolve by mixture using a clean glass rod and mix it with a
adding deionised water and make it up to the drop of the indicator arranged on paraffined
mark. Shake well to get uniform concentration. paper. The colour of the drop of indicator
changes to blue. Take out a drop of the reaction
Part - B: Estimation of Iron mixture after every addition of K2Cr2O7 and mix it
Pipette out 25 cm3 of the given Haematite with a fresh drop of the indicator. Appearance of
solution into a clean conical flask. Add 1/4 test blue or green colour indicates that the end point
tube of concentrated Hydrochloric acid. Heat the is not reached. At the end point, a drop of the
solution nearly to boiling. Add Stannous Chloride reaction mixture fails to give either blue or green
drop by drop to the hot solution until the solution colouration. Note down the burette reading and
becomes colourless. Add 2-3 drops of Stannous repeat the experiment for concordant values.

VIVA QUESTIONS

1 What is the main constitutes of Haematite ore?

2 In what form does Iron exist in Haematite?
3 What is the oxidation number of Iron in Haematite?
4 Give the others form of Iron ore.
5 What is the role of Stannous Chloride?
6 Why is Mercuric Chloride added and at a stretch?
7 What happens when the excess of Stannous Chloride is not removed?
8 What is the indicator used?
9 Why the color of the indicator drop remains the same at the end point?
10 Name any two oxidizing and reducing agents used in the experiment.
11 What is the reaction that occurs during the titration?
12 Write down the equations for the
a. Reactions between hot acidified ore solution and Stannous Chloride.
b. Addition of saturated mercuric Chloride to the solution in a.
c. Addition of Potassium Dichromate to the solution obtained in b.
13 Why is it necessary to add only very small excess of Stannous Chloride during the reduction of Fe3+ to
Fe2+?
14 Why grey ppt. is obtained some time?
15 Why Stannous Chloride is added while the solution is hot?

6
Observation and Calculation:

Part-A: Preparation of Potassium Dichromate solution

Weight of K2Cr2O7 + Weighing Bottle g

Weight of empty Weighing Bottle g
Weight of the K2Cr2O7 transferred g

Normality of K2Cr2O7 = Weight of K2Cr2O7 crystals dissolved in

Gram equivalent weight of K2Cr2O7 (49.03)

Part-B: Estimation of Iron

Burette readings(in cm3) Trial-I Trial-II Trail-III

Final
Initial
Volume of K2Cr2O7 run down

Part-C: Calculation

1000 cm3 of 1N K2Cr2O7 = 1 equivalent of iron

= 55.85 g of Iron

Therefore ‘Y’ cm3 of ‘x’ N K2Cr2O7 = g of iron = ‘Z’ g of iron.

25cm3 of Haematite ore solution contains ‘Z’ g of iron

250cm3 of Haematite ore solution contains ’10xZ’g of iron

Weight of Haematite ore dissolved in 250cm3 of the solution = 'W'g

‘W’ g of haematite ore contains ’10 xZ’ g of iron.

Therefore, 100g of haematite ore contains = g of iron = ‘B’ g of iron

7
EXPERIMENT NO – 4

Aim:
Determination of Chemical Oxygen Demand (COD) of the given industrial waste water sample

VIVA QUESTIONS

1 What is chemical Oxygen demand?

2 What are the constituents which increase the COD of sewage?
3 What general group of organic compounds is not oxidized in the COD test?
4 What is the role of Silver Sulphate?
5 What is the role of Mercuric Sulphate?
6 Explain the role of acidified Potassium Dichromate.
7 What are the products formed after COD analysis?
8 Why is Sulphuric acid added during the preparation of standard FAS solution?
9 Why can’t we use Nitric acid instead of dilute Sulfuric acid?
10 What is the composition of Ferroin?
11 What is the unit of COD?
12 Mention a few application of COD test in environmental engineering practice.
13 What is the limitation of COD?
14 What conclusion can be drawn from the COD measurement?

Observation and Calculation:

Part-A: Preparation of FAS solution

Weight of Weighing Bottle + FAS crystals g

Weight of Weighing Bottle

g
Weight of the FAS crystals transferred
g

Normality of FAS = Weight of FAS

Gram mol wt of FAS (392.14)

Part – B: Back Titration

8
 Burette readings(in cm3) Trial-I Trial-II Trail-III
Final
Initial
Volume of FAS run down

Part-C: Blank titration

Burette readings(in cm3) Trial-I Trial-II Trail-III

Final
Initial
Volume of FAS run down

Part-D: Calculation

Blank titre value = ‘X cm3

Back titre value = ‘Y’ cm3

Amount of dichromate (in terms of FAS) that has reacted with water sample = (X – Y) cm3.

1000 cm3 of 1N FAS solution = 1 equivalent of oxygen = 8 g of oxygen.

(X-Y) cm3 of ‘Z’ N FAS solution = g of oxygen = ‘A’ g of oxygen

25 cm3 of waste water requires ‘A’ g of oxygen

Therefore, 1000 cm3 of waste water requires = g of oxygen = ‘B’ g of oxygen

= ‘C’ mg of oxygen

9
EXPERIMENT NO – 5 add 6.0 cm3 of conc. H2SO4 and stopper the Bottle
and invert it several times, till the precipitate
Aim: dissolves completely. Iodine is liberated.
Determination of Dissolved Oxygen in the given
water sample by Winkler’s method Pipette out 50 cm3 of the reaction mixture into a
conical flask. Add 2.0 cm3 of freshly prepared
Description: starch indicator to it. Titrate the solution
Estimation of Dissolved Oxygen immediately against standardized Sodium-
Transfer 900 cm3 of the water sample to BOD thiosulphate till the colour changes from blue to
Bottle. Add about 6.0 cm3 of alkali Iodide-Azide colourless.
reagent by means of pipette (Keep the tip of the
pipette well below the surface of the solution).
Pipette out 6.0 cm3 of 48% MnS04 solution and
add it to the BOD Bottle. Stopper the Bottle and
remove the bubbles if formed and mix the
contents of the Bottle by gently inverting it a few
times. Allow the precipitate to settle down. Now

VIVA QUESTIONS

1. What is meant by Dissolved Oxygen?

2. What is the importance of dissolved Oxygen in of water?
3. Differentiate between dissolved Oxygen and COD?
4. Explain the principle involved in the Winkler's method.
5. What are Iodometric titrations?
6. What is the function of Sodium Azide in the estimation of water?
7. Upon what factors does dissolution of Oxygen in water depend?
8. Write down the reaction taking place when
(i) MnSO4 and alkaline Iodide-Azide is added to water.
(ii) Conc. H2SO4 is added to the above mixture
(iii) Iodine reacts with Sodiumthiosulphate.
9. How does the presence of NO-2 affect the DO results?
10. What is the effect of oxidisable impurities on the dissolution of Oxygen?
11. When do you say the sample of water is polluted badly?
12. Justify: 1000 cm3 of IN Sodiumthiosulphate is equivalent to 8 g of Oxygen.
13. How do you prepare 2 dm3 of 0.0246 N Sodiumthiosulphate?
14. The reaction is carried out in a BOD Bottle and not in a conical flask. Why?
15. Define BOD and COD of water

10
Observation and Calculation:

Part-A: Estimation of Dissolved Oxygen

Burette reading(in cm3) Trial - I Trial - II Trial - III

Final reading
Initial reading
Volume of Sodiumthiosulphate
rundown in cm3

Part-B: Calculation

Normality of Na2S2O3 solution = Y

50 cm3 of reaction mixture (49 cm3 of water sample) requires X cm3 of Y N Na2S2O3 solution.

1000 cm3of 1.0 N Na2S2O3= 8.0 g of Oxygen

1.0 cm3 of 1.0 N Na2S2O3 = 8.0 mg of Oxygen

X cm3 of 'Y' N Na2S2O3= 8.0 x X x Y = Z mg of oxygen

49 cm3 of water sample contains ‘Z’ mg of Oxygen

1000 cm3 of water sample contains mg of oxygen = ‘A’ mg of Oxygen = A ppm

11
EXPERIMENT NO – 6

Aim:
Preparation of Polystyrene by Bulk Description:
Polymerization method
About 30 ml of styrene monomer is freed from
stabilizer by washing three times with 10 ml of 1%
Chemicals Required: NaOH solution followed by three washings (20ml
Styrene, Polyvinyl Alcohol (PVA-suspending each) with distilled water. The monomer is then
agent), Benzoyl Peroxide (initiator), medium dried over anhydrous CaCl2.
(water), 1 % NaOH solution.
A Mixture of 50 ml of distilled water and 1 g of
Apparatus Required: PVA is taken in a 100 ml round bottom flask and
100 ml three necked round-bottom flask, placed on a hot plate at 80±2 °C.To the washed 10
thermometer, dropping funnel, Nitrogen gas ml of Styrene, 0.5 g of benzoyl peroxide (BPO) is
cylinder, hot plate cum magnetic stirrer and added. The Styrene containing Benzoyl- Peroxide
water cooled condenser. is added into the round bottom flask by means of
a dropping funnel over a period of 5 hour. The
prepared Polystyrene (PS) pearls or beads are
filtered off, washed with 2% HCl and water, and
then dried. Note down the appearance and yield
of Polystyrene.

VIVA QUESTIONS

1. Pearl or bead shaped products are obtained in Suspension Polymerization? Give reasons.
2. Explain Suspension Polymerization Process?
3. What type of initiators are used in Suspension Polymerization?
4. Give two advantages of Suspension Polymerization technique?
5. Give two uses of Polystyrene?
6. Give the names of two more initiators used in Polymerization process
7. Write the mechanism of Polymerization in the present case
8. What is a free radical and what is its use in Polymerization?

12
EXPERIMENT NO – 7

Aim: Wt of Wt of
Preparation of ZnO by Solution Combustion Urea X Valency MgNO3 X Val
=
method Mol wt of Urea Mol Wt of of MgNO3
of Urea MgNO3
Chemicals Required:
Zinc nitrate (Zn(NO3)2.6H2O, (Mol. Wt=297.46) Wt of Urea = (5x10x60)/(297.46x6) g
any organic fuel (say Urea; NH2CONH2; Mol. Wt = = 1.68 g
60) and distilled water.
Description:
Apparatus Required: Weigh exactly 5.0 g of Magnesium Nitrate and
High Temperature Furnace, 250 ml Borosil glass 1.95 g of Urea (1:1 stochiometry) in 250 ml beaker
beaker, Tong, Spatula, Weighing balance, and dissolve the salts by adding minimum
Magnetic stirrer. quantity of distilled water and stirring on a
magnetic stirrer for 10 min. The uniformly
Calculation of fuel: dissolved redox mixture is kept in a pre-heated
furnace maintained at 500 ºC. The redox solution
The valency of = 2(0) + 4(+1)+1(+4)+1(-2) undergoes evaporation and finally results in
Urea (N2H4CO) =6 viscous-gel containing uniformly mixed
The valency of = 1(+2) + 2(0)+ 6(-2)+6(0) Magnesium Nitrate and Urea. After some time it
Zn(NO3)2.6H2O = 10 catches fire with the liberation of gases and heat
energy, finally results in highly porous, white
powder of nano MgO.
The amount of Urea for 5.0 g of Zn(NO3)2 is
calculated as follows. VIVA QUESTIONS

1.What is the formula for the calculation of

amount of fuel?
2.What is the principle behind Solution
Combustion method?
3.What are the advantages of Solution
Combustion method?

13
INSTRUMENTAL METHODS OF ANALYSIS Continue adding 0.2 cm3 of NaOH & measure the
pH regularly after each addition until the increase
EXPERIMENT NO – 8 in pH is comparatively large. Take a few more
reading by adding 0.2 cm3 of NaOH.
Aim: Determine the pKa of the given weak acid from
Determination of pKa of a weak acid using pH the two graphs:
meter
(i) against volume of NaOH added.
Description:
(ii) pH against volume of NaOH added.
Pipette out 50 cm3 of the given weak acid (Acetic
Fig. 2
acid) into a clean 250 cm3 beaker. Insert glass
electrode - calomel electrode assembly into it and
connect it to pH meter. Measure the pH of the x
acid. Fill the burette with the given Sodium-
x
Hydroxide. In the beginning add 0.2 cm3 of NaOH x
at a time and stir the mixture. Measure the pH.
Fig. 1 pKa
x pH x Half Equivalence Point [x/2]
x
x
x
x
x
x Volume of NaOH in cm3
x
∆pH x Equivalence Point
x
∆V x
x x

Volume of NaOH in cm3

Equivalence point = ‘x’ cm3

Half Equivalence point = ‘x/2’ cm3
pH Corresponding to half equivalence point = ‘y’
= pKa
VIVA QUESTIONS
1. Define pKa of a weak acid.
2. pKa values of two acids are 2.8 and 3.2. Which one of these acids is stronger?
3. Why should we compute the pKa values of a weak acid?
4. Define pKa of a weak acid in terms of pH of the solution
5. Account for the following:
a) pH of the medium changes enormously at its equivalence point.
b) At half equivalence point, pH is equal to pKa.
6. Write down Henderson-Hasselbalch equation.
7. pKa values of Acetic acid and Formic acid are 4.7 and 3.7 respectively at a given temperature. Which one
of the two acids is stronger?
8. Henderson-Hasselbalch equation is holds good for buffer of weak acid and its salt with strong base. How
do would you justify the use of this equation in the experiment?
9. What is a buffer solution? Give any two examples.
10. What are the applications of Henderson-Hasselbalch equation?
11. Find out the ratio in which the acid and its salt are to be dissolved in 1 dm3 such that the resultant buffer
would offer a PH of 5.95. Given pKa = 4.0.
12. 1.0 mole of sodium acetate and 0.5 mole of Acetic acid were dissolved in 1 dm3 of water. Calculate the pH
of the buffer. Given, dissociation constant of Acetic acid at 298 K is 10-5
13. Why half equivalence point is taken into account for assigning pKa?

14
EXPERIMENT NO– 9 VIVA QUESTIONS
1 What is a Potentiometer titration?
Aim: 2 Give the principle of Potentiometer titration.
Estimation of Iron present in 1750 cm3 solution 3 What are the electrodes used in Potentiometer
of FAS using Potentiometer. Given, the titration?
normality of K2Cr2O7 solution is 0.0489N 4 What is determining factor in the oxidation-
reduction reaction?
5 What is an indicator electrode?
6 What is the reaction that occurring between FAS
and Potassium Dichromate?
7 What are the advantages of Potentiometric
titration?

15
Calculation:

Volume of K2Cr207 required for the reaction = cm3 (from graph)

NFAS =

Amount of Iron presented in 1000 cm3 of its = NFAS x Gram equivalent weight of Iron
solution

16
EXPERIMENT NO– 10 by plotting absorbance against volume of Copper
Sulphate taken. Using the calibration curve, find
Aim: out the unknown volume of Copper Sulphate
Estimation of Copper present in a given Copper solution given and calculate the amount of
Sulphate solution, using Colorimeter. Amount of Copper present in it.
Copper Sulphate pentahydrate in 100 cm3 of
solution is 55 mg

Description:
Transfer 2, 4, 6, 8 and 10 cm3 of given Copper

Absorbance (a.u)
x
Sulphate solution into different 25 cm3 volumetric
x
flask from a burette. Add 2.5 cm3 of Ammonia to
all the flasks and makeup all the solutions up to
x
the mark using distilled water. Stopper the flasks
Volume of unknown
shake well to get uniform concentration.
x solution in cm3
Prepare a blank solution by taking 2.5 cm3 of
Ammonia in another 25 cm3 volumetric flask. x

Make up that solution also up to the mark using

distilled water and shake well. To the given
unknown solution also add 2.5 cm3 of Ammonia, Volume of CuSO4 in cm 3
make it up to the mark and shake well. After 10
minutes, set the instrument to zero reading using
blank solution and measure the absorbance of all
solutions, by using 620 nm filter of a Colorimeter.
Note down the optical density of all solutions and
tabulate the readings. Draw a calibration curve
VIVA QUESTIONS

1 What is Colorimetry?
2 What forms the basis for Colorimetric determination?
3 What is photoelectric Colorimeter?
4 What are filters? Why are they used?
5 What is wave length?
6 What is frequency?
7 Why is estimation of Copper done at 620 nm wave length?
8 What is wave number?
9 State Beer’s law.
10 State Lambert’s law.
11 State Beer-Lambert’s law.
12 Upon what factors the absorbance of a solution depends?
13 What is calibration curve?
14 What is meant by transmittance?
15 Why a filter of 620 nm is used in the estimation of Copper?
16 Mention a few important criteria for satisfactory Colorimetric analysis.
17 Mention a few advantages of Photoelectric Colorimetric determination.
18 What is Blank solution?
19 What is the basic requirement of a compound for its estimation by Colorimetric method?
20 Why is Ammonia added? Why is that same amount of Ammonia added?

17
Calculation:

From the graph,

Volume of CuSO4 corresponds to optical density of unknown solution (test solution) = Z cm3

Weight of copper sulphate pentahydrate present in 100 cm3 of the given solution = ‘X’ mg

Weight of CuSO4.5H2O in 1 cm3 of its solution = X/100 mg =…………………… = ‘Y’ mg

Weight of copper present in 1 cm3 of its solution ‘Y’ x 63.54

249.54

Weight of copper present in Z cm3 of its solution =

18
 NaOH solution into the beaker and shake well.
Note down the conductance. Note down the
EXPERIMENT NO– 11 conductance by adding 0.2 cm3 of NaOH each
time to the beaker. Conductance decreases in
Aim: the beginning starts increasing after a certain
Estimation of Hydrochloric acid present in 1.5 addition of NaOH. Take around 8-10 readings on
dm3 of HCl solution using Conductometer. Given, the increasing side. Draw a graph of conductance
the normality of NaOH solution is 0.05N against volume of NaOH added. The point of
minimum conductance (intersecting point of the
Description: lines) is called the Equivalence point and it
Pipette out 50 cm3of acid into a clean 200 cm3 corresponds to complete neutralization of HCl.
beaker. Dip the conductivity cell in the acid, such Calculate the normality and amount of HCl
that the two Platinum electrodes are immersed present in 1000 cm3 of its solution.
completely. The cell is connected to the
conductivity bridge. Measure the conductance.
Take the given NaOH solution in a burette rinsed
with the same solution. Rundown 0.2 cm3 of

VIVA QUESTIONS

1 State Ohm’s law.

2 What is conductance?
3 What is the unit of conductance?
4 Name the SI unit of conductance.
5 Mention the different types of conductivities.
6 Which of the above conductivity measured during Conductometric titration?
7 What is specific conductivity?
8 What is equivalent conductivity?
9 What is molar conductivity?
10 What is a cell?
11 Define cell constant
12 Describe a conductivity cell.
13 What is the principle involved in Conductometric titration?
14 How is the accuracy of the method determined?
15 Explain the graph obtained in case of Conductometric titration involving acid mixture and NaOH.
16 What are the advantages of Conductometric titration over visual or potentiometric titration?
17 How do you account for the decrease in the conductivity at the beginning of the titration?
18 How would you account for the increase in the conductivity after the end point?
19 The second line in the graph is not as steep as the first. Explain.

19
Calculation:

From the graph, equivalence point corresponds to Volume of NaOH = cm3

(NV) HCl = (NV) NaOH

NHCI = (NV) NaOH

VHC1

Amount of HCI present in 1000 cm3 of its solution = NHCI x Gram equivalent weight of HCI (36.5 g)

20
 Ƞl = tl dl Ƞw
tw dw
EXPERIMENT NO– 12
If Laboratory temperature [T] K
Aim:
At ‘T’ K density of water = dw
Determination of Viscosity Coefficient of a given
At ‘T’ K density of liquid = dl
liquid using Ostwald’s viscometer
AT ‘T ’K viscosity of water =
At ‘T’ K viscosity of liquid =
Description:
Take a clean and dry viscometer. Fix it vertically VIVA QUESTIONS
to a stand. Using graduated pipette, transfer
known volume (say 10 cm3) of the given liquid 1 What is Viscosity Coefficient of a liquid?
into the viscometer. Then it is placed in a 2 What is density of a liquid?
thermostat (Water Bath) such that its big bulb is 3 What is specific gravity?
completely immersed in water. Suck the liquid 4 How are specific gravity and density related?
above the upper mark of the small bulb of the 5 What is SI unit of Viscosity Coefficient?
viscometer. Allow it to flow through the capillary. 6 What are the factors that affect the viscosity
When the liquid crosses the upper mark of the of a liquid?
small bulb, start a stop watch and when the liquid 7 How does the viscosity vary with
crosses the lower mark, stop the watch. Note temperature?
down the time of flow in seconds. 8 Why is acetone used for cleaning viscometer?
9 Why do you require laboratory temperature
Repeat the experiment 3-4 times and calculate for viscosity determination?
the average time of flow. Remove the liquid from 10 How is the viscosity of liquid related to its
the viscometer, clean well with acetone and dry it mobility?
in oven. Cool the viscometer to room 11 What is fluidity of a liquid?
temperature. Similarly, measure the time of flow
for water by taking the same volume. Calculate
average time of flow for water. Note down the
room temperature. Knowing the density,
viscosity of water and density of the given liquid,
viscosity of the liquid can be calculated.
Calculation:

Laboratory temperature [T] = oC = K

At ‘T’ K density of water = dw =
At ‘T’ K density of liquid = dl =
AT ‘T ’K viscosity of water = =
At ‘T’ K viscosity of liquid = =

Ƞl = tl dl Ƞw
tw dw
(1 milli poise = 10-4Nsm-2)

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EXPERIMENT NO– 13

Aim:
Estimation of Sodium present in a given NaCl
solution, using Flame Photometer. Amount of Graph
NaCl present in 100 cm3 of the solution is 2.5 g

Description: x
Flamephotometer reading

Transfer 2, 4, 6, 8 and 10 cm3 of standard Sodium

solution into different 25 cm3 volumetric flasks
x
from the burette. Make up all the solutions using x
double distilled water. Stopper the flasks and
shake well to get uniform concentration. To the x Unknown Volume
given unknown solution, add double distilled
x
water and shake well. Switch on the instrument;
turn the gas supply on and light the gas at the
burner. Adjust the air supply from the Volume of Na Solution in cm3
compressor to 10 lbs/sq inch using pressure
regulator knob. Place the sodium filter (589 nm) VIVA QUESTIONS
in position. Now dip the capillary tube in a cell 1. What is meant by atomic emission?
containing double distilled water. The stream of 2. What is Flame Photometry?
air atomized as a fine mist draws up the liquid. 3. What are alkali and alkaline earth metals?
Regulate the gas supply so that the colour of the 4. What are the various events that occur when
flame completely turns to blue. Adjust the flame solution containing metal atom ions
photometer to zero by means of zero control atomized through a flame?
knob. Feed the various sodium solutions 5. What are different components of a Flame
prepared, through the flame one by one including Photometer?
the unknown solution. Note down the flame 6. Why the analysis of Sodium is advantageous
photometer readings. Plot a graph of flame is Flame Photometry?
photometer readings against the volume of the 7. What is the role of filter in Flame
solution get the calibration curve. Using the curve Photometry?
obtained find out the volume of the unknown 8. What are the errors that occur in Flame
solution containing sodium and calculate the Photometry?
amount of Sodium in it. 9. What are the factors that influence this
experiment?

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 10. Name the fuel and oxidant used in this
experiment

Calculation:

From the graph, Volume of NaCl corresponds to Flame Photometer Reading of unknown solution (test solution)
= Z cm3

Weight of Sodium Chloride present in 100 cm3 of the given solution = mg

58.5 g of NaCl contains 23 g of Na.

Therefore, 1 cm3 of the given stock solution contains = = ‘A’g of Na

Z cm3 of the given stock solution contains = (A x Z ) g of Na

the oil to collect in the flask. Repeat the experiment

to get more readings.
EXPERIMENT NO– 14
VIVA QUESTIONS
Aim: 1. What is Viscosity?
Determination of relative and Kinematic Viscosities 2. What are different types of viscosity explain
of given lubricating oil at different temperatures them and write the units?
using Redwood Viscometer 3. What are factors effecting viscosity?
4. Mention some applications where viscosity
Description: is considered?
Clean the viscometer cup properly with the help of 5. Relation between density and viscosity?
suitable solvent e.g. CCl4, ether, petroleum spirit or 6. Which constructional feature of viscometer
benzene and dry it to remove any traces of solvent. varies with the viscosity of oil?
Level the viscometer with the help of leveling screws
and fill the outer bath with water for determining the
viscosity at 80 oC and below. Place the ball valve on
the jet to close it and pour the test oil into the cup
up to the tip of indicator. Place a clean dry
Kohlrausch flask immediately below and directly in
line with discharging jet. Insert a clean thermometer
and a stirrer in the cup and cover it with a lid. Heat
the water filled in the bath slowly with constant
stirring. When the oil in the cup attains a desired
temperature, stop the heating. Lift the ball valve and
start the stop watch, oil from the jet flows into the
flask. Stop the stop watch when lower meniscus of
the oil reaches the 50 ml mark on the neck of
receiving flask. Record the time taken for 50 ml of

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 Observation & Calculation:

Laboratory temperature = ………………...0C

Density of given liquid =………………………g/cc

Sl.No. Temperature Kinematic Density(ρ) Dynamic (or

In (˚C) Viscosity(Redwood (Kg/m3) absolute) Viscosity
Seconds)(v) (Redwood Seconds)
(µ=v * ρ)
1

EXPERIMENT NO– 15

Aim: The glass transition results in a kink in the heat

To find Tg of Polymer using DSC versus temperature plot due to the change in heat
capacity (A). In a plot of heat flow versus
Procedure:
temperature it is a gradual transition that occurs
Sample preparation
over a range of temperatures (B). The glass transition
A sample of 1‐4 mg of polymer sample is placed in a
temperature is taken to be the middle of the sloped
40 µl aluminum pan. Adapt the sample size to your
region.
pan size, if different. The polymer sample should
cover the bottom of the pan. The filled pan is
crimped and locked with Aluminium lid. DSC
Instrument is kept on for 30 minutes to attain the VIVA QUESTIONS
required temperature. The pan containing sample is
placed in the heating chamber with extreme care. 1. What is Glass transition temperature?
2. What is the significance of Tg?
Give the required inputs like heating rate, sample
3. What are factors effecting Tg?
weight, cooling time etc in the software. Run the
DSC machine and get the heat versus temperature 4. What is the principle of this experiment?
graph. The proper interpretation of the obtained 5. Why Glass transition temperature is in range?
graph will give you the glass transition temperature 6. Explain the interpretation of Graph A and B
of the sample measured.

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