Chemistry Manual Sem I & Ii

CSEITQUESTIONS.BLOGSPOT.IN | CSEITQUESTIONS.BLOGSPOT.
IN
SEMESTER - I
KLNCE/Dept. of Chemistry
Page 1
CSEITQUESTIONS.BLOGSPOT.IN | CSEITQUESTIONS.BLOGSPOT.IN
LIST OF EXPERIMENTS
Expt. No.
Name of the Experiments
Page No.
1.
Determination of DO Content of water sample by

Winklers method
2.
Determination of chloride content of water sample by

argentometric method
11
3.
Determination of strength of given HCl using pH meter
17
4.
Determination of strength of acids in a mixture using

conductivity meter
25
5.
Estimation of iron content of the water sample using

spectrophotometer
31
6.
Determination of molecular weight of polyvinyl alcohol

using Ostwald viscometer
37
7.
Conductometric titration of strong acid Vs strong base
43
Page 2
TABLE OF CONTENTS
Ex. No.
Date
Marks
Signature of the
Obtained Staff with Date
Page 3
Titration I: Standardization of sodium thiosulphate
Standard potassium dichromate Vs sodium thiosulphate
S. No.
Volume of standard
potassium dichromate
(ml)
Burette reading
(ml)
Initial
Volume of sodium
thiosulphate (ml)
Final
Indicator
CALCULATION
Step 1 : Standardization of sodium thiosulphate
Volume of potassium dichromate
(V1)
= 20 ml
Strength of potassium dichromate
(N1)
= -------------N
Volume of sodium thiosulphate
(V2)
= .ml
Strength of sodium thiosulphate
(N2)
= ?
According to the law of volumetric analysis,
V1 N1
= V2 N2
N2
= V 1 N1
V2
(N2)
=..N
20 x
Page 4
Expt. No
Date
DETERMINATION OF DO CONTENT OF WATER SAMPLE BY

WINKLERS METHOD
AIM
To estimate the amount of dissolved oxygen in the given water sample by Winklers method.
Sodium thiosulphate (link solution) and a std.solution of potassium dichromate of strength
___________ N are supplied.
PRINCIPLE
Oxygen dissolves in water to an extent of 7-9 mg/lit at a temperature range of 25-35C. The
amount of dissolved oxygen in water is estimated using Winklers reagent (manganous sulphate,
alkaline potassium iodide, concentrated sulphuric acid). Water sample is collected carefully avoiding
aeration/deaeration in ground stoppered flask. Initially manganous sulphate and alkali iodide
reagents are added and the reactions occur as follows:
Mn2+
2OH-
Mn(OH)2 (White ppt)
Mn(OH)2
O2
MnO(OH)2 (Yellow brown ppt)
(DO in water)
(Basic manganic oxide)
The precipitate dissolves in concentrated sulfuric acid liberating oxygen which in turn
oxidizes potassium iodide and liberates iodine. The liberated iodine is titrated against Na2S2O3 using
starch indicator.
MnO(OH)2 + 2H2SO4
Mn(SO4)2
2H2O + [O]
2KI
+ H2SO4 + [O]
K2SO4
H2O
2Na2S2O3
+ I2
Na2S4O6
2NaI
+ I2
Page 5
Titration II: Estimation of dissolved oxygen
Std. sodium thiosulphate Vs water sample
S. No.
Volume of
water sample (ml)
Burette reading (ml)

Initial
Volume of sodium
thiosulphate (ml)
Final
Indicator
CALCULATION
Step 2 : Estimation of dissolved oxygen
Volume of sodium thiosulphate
(V1)
= ml
Strength of sodim thiosulphate
(N1)
= N
Volume of water sample
(V2)
= 100 ml
Strength of water sample
(N2)
= ?
V1 N1
= V2 N2
N2
= V 1 N1
V2
=
100 x
= ___________ N
Amount of dissolved oxygen in

one litre of given water sample
= Normality Eq. wt. of O2 1000 mg

= .N 8 1000
= mg.
Page 6
PROCEDURE
TITRATION I: STANDARDISATION OF SODIUM THIOSULPHATE

The burette is washed with water and rinsed with sodium thiosulphate solution. Then the
burette is filled with the given sodium thiosulphate solution. 20 ml of std. potassium dichromate
solution is pipetted out into a clean conical flask. To this, 5 ml conc. HCl and 5 ml 10% potassium
iodide are added. The liberated iodine is titrated against sodium thiosulphate solution. When the
solution becomes straw yellow colour, starch indicator is added and then titration is continued. The
end point of the titration is the disappearance blue colour and appearance of green colour. The titration
is repeated to get concordant values.
TITRATION II: ESTIMATION OF DISSOLVED OXYGEN

100 ml of the water sample is taken in the iodine flask, 2 ml of manganous sulphate and
2 ml of alkaline potassium iodide are added. The flask is stoppered and shaken several times for
complete mixing of reagents. The flask is left aside for some time. When half of the precipitate
settles down, the stopper is removed and 2 ml of concentrated sulphuric acid is added. The stopper is
replaced and the flask is inverted several times for complete dissolution of the precipitate. It is the
titrated against standardized sodium thiosulphate solution. Starch indicator is added when the
solution becomes light yellow. The titration is continued until the blue colour disappears. From the
titre value, the strength of dissolved oxygen is calculated and hence the amount of dissolved oxygen
in the water sample is found out.
RESULT
Amount of dissolved oxygen present in given water sample =..mg/litre
Page 7
Short Procedure
AIM
To estimate the amount of dissolved oxygen in the given water sample by Winklers method.
Sodium thiosulphate (link solution) and a std. solution of potassium dichromate are supplied.
PRINCIPLE
Mn2+
2OH-
Mn(OH)2 (White ppt)
Mn (OH)2
O2
MnO(OH)2 (Yellow brown ppt)
(DO in water)
(Basic manganic oxide)
MnO (OH)2
+ 2H2SO4
Mn(SO4)2
+ 2H2O + [O]
2KI
+ H2SO4 + [O]
K2SO4
+ H2O
2Na2S2O3
+ I2
Na2S4O6
+ 2NaI
+ I2
PROCEDURE
TITRATION I: STANDARDISATION OF SODIUM THIOSULPHATE
Burette: Sodium thiosulphate
Indicator : Starch
Pipette: 20 ml std. potassium dichromate solution
End point : Appearance of light green
Additional solution: 5ml conc.HCl + 5 ml 10% KI

Volume of K2Cr2O7 x strength of K2Cr2O7

Volume of Na2S2O3
TITRATION II: ESTIMATION OF DISSOLVED OXYGEN
Burette: Sodium thiosulphate
Indicator : Starch
Pipette: 100 ml water sample
End point : Disappearance of blue colour
Additional solution: 2 ml manganese sulphate + 2 ml alkali iodide + 2 ml conc. H2SO4

Equivalent weight of oxygen = 8
Volume of Na2S2O3 x Strength of Na2S2O3

Amount of dissolved oxygen in water sample = Normality of water sample x Eq. wt. of O2
RESULT
Amount of dissolved oxygen present in given water sample =..mg/litre
Page 8
Viva Voce Questions and Answers
1. Name the method which is used to determine DO.
Winklers method
2. How much amount of dissolved oxygen normally present in water at 25C?
7 - 9 ppm
3. What is the link solution used in the determination?
Sodium thiosulphate
4. What is meant by winklers reagent?
Winklers reagent - Manganous sulphate, alkaline potassium iodide, concentrated sulphuric
acid.
5. Name the indicator used in this estimation.
Starch
6. Define iodometry and iodimetry.
Iodometry: Iodine is liberated in the titration
Iodimetry: Iodine is used in the titration
7. What is the end point in the dissolved oxygen determination?
The end point is the disappearance of blue colour.
8. What is the equivalent weight of oxygen?
Eight
9. Name the solutions which are used to determine the dissolved oxygen in a water sample.
(i) MnSO4
(ii) NaOH
(iii) KI
(iv) conc. H2SO4
10. Write the formula that is used to calculate the amount of dissolved oxygen.
Amount of DO in one litre of tap water = 8 x N x 1000 mg/L or ppm
Page 9
Titration I: Standardization of silver nitrate

Standard sodium chloride Vs silver nitrate
S. No.
Volume of
sodium chloride (ml)

Initial
Volume of
silver nitrate
(ml)
Final
Indicator
CALCULATION
Step 1 : Standardisation of silver nitrate
Volume of sodium chloride
(V1)
= 20 ml
Strength of sodium chloride
(N1)
= .N
Volume of silver nitrate
(V2)
= ..ml
Strength of silver nitrate
(N2)
= ?

V1 N1 = V2 N2
N2 = V1 N1
V2
20 x
= .N
Page 10
Expt. No..
Date.
DETERMINATION OF CHLORIDE CONTENT OF WATER SAMPLE BY

ARGENTOMETRIC METHOD
AIM
To estimate the amount of chloride ion present in the given water sample by Mohrs method.
A std. solution of ------------- N NaCl and approximately 0.01N AgNO3 solutions are provided.
PRINCIPLE
Generally, water contains chloride ions in the form of dissolved NaCl, KCl, CaCl2 and
MgCl2. The total chloride content can be estimated by titration with standard AgNO3 solution
(Argentometric method or Mohrs method).
AgCl
+ NaNO3
(White precipitate)
Potassium chromate is used as indicator. In the presence of chromate ion, silver nitrate reacts
AgNO3
NaCl
preferentially with chloride ion forming a white precipitate of silver chloride. But at the end point in
the absence of chloride ion, silver nitrate reacts with potassium chromate giving a red precipitate of
silver chromate.
2AgNO3
K2CrO4
(Yellow)
Ag2CrO4
(Red tinge)
+ 2KNO3
When end point is reached, a light red tinged precipitate is obtained due to the formation of silver
chromate.
PROCEDURE
TITRATION I: STANDARDISATION OF SILVER NITRATE
Burette: AgNO3
Indicator : 2 drops of 5% potassium chromate
Pipette: 20 ml of Std. NaCl
End point : Appearance of pale red tinge
Page 11
Titration II: Estimation of chloride ion
Std. silver nitrate Vs water sample
S. No.
Volume of given
water sample (ml)

Initial
Final
Volume of
silver nitrate (ml)
Indicator
CALCULATION
Step - 2 : Estimation of chloride ion content
(V1)
= 20 ml
Strength of chloride ion

in the water sample
(N1)
= ?
(V2)
= ..ml
(N2)
= N

V1N1 = V2N2
N1
= V2 N2
V1
Strength of chloride ion in the given water sample
x
20
= N
Calculation of amount of chloride ion

Amount of chloride ion present in
100 ml of the given water sample
= Equivalent wt. of chloride ion Strength of chloride ion

10
=
35.5
10
= ____________ gm.
Page 12
The burette is washed with distilled water and rinsed with silver nitrate solution. Then it is
filled with same silver nitrate solution up to the zero mark. A 20 ml pipette is washed with water and
rinsed with small amount of sodium chloride solution and then 20 ml of same solution is pipetted out
into a clean conical flask. 2 drops of 5% potassium chromate solution is added as indicator. The
solution becomes yellow. It is titrated against silver nitrate taken in the burette. Near the end point
coagulation of the precipitate takes place. Silver nitrate is added in drops with constant shaking. The
end point is indicated by the appearance of pale red tinge on the precipitate. The titrations are
repeated to get concordant values and the normality of silver nitrate solution is calculated.
TITRATION II : ESTIMATION OF CHLORIDE ION

Burette
: AgNO3
Pipette
: 20 ml of given water sample
The burette is filled with same silver nitrate solution up to zero mark. The given water
sample is made up to 100 ml in standard measuring flask with distilled water. A 20 ml pipette is
washed with water and rinsed with made up water sample. 20 ml of this water sample is pipetted out
and 2 drops of 5% potassium chromate is added and titrated against AgNO3 solution. The end point
is the formation of red tinge on the precipitate. The titrations are repeated to get concordant values.
Equivalent weight of chlorine is 35.5

Equivalent weight of NaCl is 58.5
RESULT
The amount of chloride ion present in 100 ml of the given water sample = gm.
Page 13
Short Procedure
AIM
To estimate the amount of chloride ion present in the given water sample by Mohrs method.
A std. solution of NaCl and approximately 0.01N AgNO3 solutions are provided.
PRINCIPLE
AgNO3
NaCl
2AgNO3
K2CrO4
(Yellow)
AgCl
+
(White precipitate)
Ag2CrO4
(Red tinge)
NaNO3
+ 2KNO3
PROCEDURE
TITRATION I: STANDARDISATION OF SILVER NITRATE
Burette: AgNO3
Pipette: 20 ml of Std. NaCl
= Volume of sodium chloride x Strength of sodium chloride

TITRATION II: ESTIMATION OF CHLORIDE ION
Burette
: AgNO3
Pipette

Amount of chloride ion
= Volume of silver nitrate x Strength of silver nitrate

= Strength of chloride ion x Eq. Wt. of chloride ion
Equivalent weight of chlorine is 35.5

Equivalent weight of NaCl is 58.5
RESULT
The amount of chloride ion present in the given water sample = gm / litre
Page 14
1. What is the name of the method used to estimate the chloride ion in a water sample?
Mohr-s method
2. Name the link solution that is used in the determination of chloride ion.
Silver nitrate solution.
3. What is meant by argentometric method?
Water contains chloride ions in the form of dissolved NaCl, KCl, CaCl2 and MgCl2. The total
chloride content can be estimated by titration with standard AgNO3 solution (Argentometric
method or Mohrs method).
3. What is the indicator used in the determination?
Potassium chromate
4. What is the colour of the indicator in a water sample?
Yellow
5. What is the end point of titration?
Formation of red tinge precipitate (Due to the formation of Silver chromate)
6. Write the formula used to calculate the amount of chloride ion present in the water sample.
Amount of Cl- in the water sample = Equivalent weight of chloride ion x Normality
7. What kind of chlorides present in water?
NaCl, MgCl2, CaCl2.
8. Why does AgNO3 react first with chloride ions in the water and not with chromate ions?
The solubility product of Ag2CrO4 is high compared to that of AgCl, therefore AgNO3 reacts
first with chloride ions in the water and all the chlorides in solution have been precipitated as
AgCl.
9. The formation of red tinge is due to what?
It is due to the formation of silver chromate Ag2CrO4.
10. What is the equivalent weight of chloride ion?
35.5
Page 15
Titration between HCl & NaOH
Volume of HCl (V1) = ______ ml
Volume of NaOH added (ml)
pH
0
2
4
6
8
10
12
14
16
18
20
Graph I : Volume of NaOH Vs pH
Graph II : Volume of NaOH Vs pH/V
Page 16
Expt. No
Date.
DETERMINATION OF STRENGTH OF GIVEN HCl USING PH METER

AIM
To determine the strength of given HCl by using pH meter and also calculate the amount of
HCl. You are provided with a standard solution of NaOH of strength ..N.
PRINCIPLE
The pH of the solution is related to the H+ ion concentration by the following formula,
pH = -log [H+]
Measurement of pH of the solution gives the concentration of H+ ions in the solution. When
NaOH is added slowly from the burette to the solution of HCl, H+ ions are neutralized by hydroxide
ions. As a result, pH of the solution increases.
HCl + NaOH NaCl + H2O
The increase in pH values takes place until all the H+ ions are completely neutralized (up to
the end point). After the end point, further addition of NaOH increases pH sharply as there is an
excess of OH- ions.
PROCEDURE
The burette is filled with standard sodium hydroxide solution. Exactly 20 ml of the given
hydrochloric acid solution is pipetted out into a clean beaker and one test tube of distilled water is
added to it. The glass electrode is dipped in it and connected with a pH meter.
Now 2 ml of NaOH solution is added from the burette to the HCl solution taken in the beaker
and pH of the solution is noted for each addition. This process is continued until at least 5 readings
are taken after the end point. The observed pH values are plotted against the volume of NaOH
added. From the graph the end point is noted. This procedure gives the approximate end point.
Accurate end point can be determined by following the same procedure. Near the end point, the pH
values are noted for every 0.2 ml addition of NaOH.
Page 17
Titration between HCl & NaOH

Volume of NaOH (ml)
pH
pH
V (ml)
pH/V
Page 18
The end point is obtained by plotting pH Vs volume of sodium hydroxide added or pH / V Vs

volume of sodium hydroxide added. From the end point the strength of hydrochloric acid is
calculated.
Page 19
CALCULATION
Step 1 : Calculation of strength of HCl
Volume of HCl
(V1)
= 20 ml
Strength of HCl
(N1)
= ......................?
Volume of NaOH
(V2)
= ........................ (titre value from graph)
Strength of NaOH
(N2)
= .. N

V1N1
= V2N2
N1
= V2 N2
V1
Strength of given HCl
= ----- x ----20
= .................. N
Step 2 : Calculation of amount of HCl

The amount of HCl present in
1 litre of the given solution
= Normality of HCl x Equivalent wt. of HCl (36.5)
= ....................... gm.
Page 20
RESULT
Strength of given Hydrochloric acid
= .N
Amount of HCl present in 1 litre of the solution = gm.
Page 21
Short Procedure
AIM
To determine the strength of given HCl by pH meter and also calculate the amount of HCl.
You are provided with a standard solution of NaOH of strength ..N.
PRINCIPLE
pH of a solution is related to the H+ ion concentration as, pH = -log [H+]
HCl + NaOH
NaCl + H2O
PROCEDURE
Burette solution
: Sodium hydroxide solution
Pipette solution
: 20 ml of the given HCl + one test tube of distilled water
Electrode
: Glass electrode
The gradual addition of NaOH from the burette (OH- ions) increases the pH value gradually.
At the end point (sharp increase) complete neutralization takes place (i.e.) all the fast moving
H+ ions are replaced by fast moving OH- ions.
After the end point there is only free OH-ions are present. So constant increase of pH occurs.
Graph 2: Volume of NaOH Vs pH /V
Graph 1: Volume of NaOH Vs pH
pH /V
pH
Volume of NaOH (ml)

Strength of HCl
Volume of NaOH (ml)

= Volume of NaOH x Strength of NaOH
Volume of HCl
Amount of HCl = Strength of HCl x Equivalent weight of HCl (36.5)

RESULT
Strength of given hydrochloric acid
=.N
Amount of HCl present in 1 litre of the solution = gm.
Page 22
1. Define pH
pH is defined as the negative to the base 10 logarithm (log) of the H+ ion
concentration. Mathematically, it is represented as
pH = -log [H+]
2. What is the pH value of a neutral solution?
7
3. Write the pH range for (i) an acidic solution (ii) a basic solution
(i)
Acidic solution : < 7
(ii)
Basic solution : > 7
4. Write the formula for pH.

pH = -log [H+] = log 1 / [H+]
5. What is the unit for pH?
No unit. Mere number.
6. How is the pH of the solution found out?
Using pH meter, indicators or pH paper.
7. Name the electrodes used in pH metry.
Glass electrode and calomel electrode.
8. Explain why the pH value increases steeply at the end point.
At the end point, all H+ ions are neutralized and the basic hydroxide ion will be
present. Hence pH is increased.
9. What is the equivalent weight of HCl?
36.5
10. Write the formula used to calculate the amount of HCl.
Amount of HCl = Equivalent weight of HCl (36.5) x Normality of HCl
11. pH + pOH = ?
14
Page 23
Titration between HCl, CH3COOH (mixture of acids) & NaOH
Volume of HCl (V) = 40 ml
Volume of
ConducNaOH
tance
added (v)
(mho)
ml
(V+v)
V
C x(V+v)
V
(mho)
Volume
Conducof NaOH
tance
added
(mho)
(v) ml
0.5
8.5
1.5
9.5
10
2.5
10.5
11
3.5
11.5
12
4.5
12.5
13
5.5
13.5
14
6.5
14.5
15
7.5
15.5
(V+v)
V
C x(V+v)
V
(mho)
C x (V+v) /V mho
Graph
(B)
(A)
Volume of NaOH (ml)
Page 24
Expt. No
Date.
DETERMINATION OF STRENGTH OF ACIDS IN A MIXTURE USING

CONDUCTIVITY METER
AIM
To determine conductometrically the strength of given hydrochloric acid and acetic acid
present in the given mixture, by titrating with standard..N sodium hydroxide solution and
calculate the amount of each acid present in 1 litre of the solution.
PRINCIPLE
Solutions of electrolytes conduct electricity due to the presence of ions. The specific
conductance of a solution is proportional to the concentration of the ions in it. When a mixture of
HCl and CH3COOH is titrated against NaOH, hydrochloric acid, being a much stronger acid will get
neutralized first. The neutralization of acetic acid will commence only after HCl has been
completely neutralized.
H+ + Cl-
Na+ + OH-
CH3COOH(aq) + Na+(aq) + OH-aq
fast
Na+ + Cl- + H2O (l)
slow
CH3COO-(aq) + Na+(aq) + H2O(l)
A graph is drawn between volume of NaOH added and the conductance of solution. There
are two points of intersection; first one corresponds to HCl and the second one corresponds to
CH3COOH.
PROCEDURE
The burette is filled with standard sodium hydroxide solution. Exactly 40 ml of the mixture
of hydrochloric acid and acetic acid is pipetted out into a clean beaker. A glass rod is placed in the
beaker for stirring the solution. The conductivity cell is kept immersed in the solution. The
conductance of the solution is measured by connecting the terminal of conductivity cell with a
conductivity bridge. 0.5 ml of standard sodium hydroxide solution is added each time from the
burette, stirred well and the conductance of the solution is noted after each addition. Conductance
decreases gradually due to the neutralization of hydrochloric acid, it reaches the first end point and
after that the conductance increases till it reaches the second end point. Further addition of sodium
hydroxide steeply increases the conductance value.
Page 25
CALCULAION
Step-1: Strength of HCl
Volume of HCl (acid mixture)
(V1)
= 40 ml
Strength of HCl
(N1)
= .............. ?
Volume of NaOH
(V2)
= V2 = ........... (A) ml (Ist titre value from graph)
Strength of NaOH
(N2)
= ____ N

V1N1 = V2N2
N1
Strength of HCl
= V2 N2
V1
x
40
= .................. N
Amount of HCl
The amount of HCl present in
= Strength of HCl x Eq.wt.of HCl (36.5)

= ................. N x 36.5
= ................... gms
Step 2 : Strength of CH3COOH

Volume of CH3COOH (acid mixture) ( V1) = 40 ml
Strength of CH3COOH
(N1) =
.............. ?
Volume of the NaOH
(V2) =
(B-A) ml (II titre value from graph)
Strength of NaOH
( N2) = ____ N

V1N1 = V2N2
N1 = V2 N2
V1
Strength of CH3COOH
x
40
= .................. N
Calculation of amount of CH3COOH

The amount of CH3COOH present in
= Normality of CH3COOH x Eq. wt. CH3COOH

= .......................... x 60
= ............................ gm.
Page 26
The values of observed conductivity or [C (V+v)/V] are plotted against volume of sodium
hydroxide added. The point of intersection at the two places gives the first and second end point
which corresponds to HCl and CH3COOH respectively. From this, the amount of HCl and
CH3COOH is calculated.
RESULT
The strength of hydrochloric acid in the mixture of acids
= ....N
The amount of HCl in 1 litre of the mixture of acids
= gm.
The strength of Acetic Acid in the mixture of acids
= ...N
The amount of CH3COOH in 1 litre of the mixture of acids = gm.
Page 27
Short Procedure
AIM
To determine conductometrically the strength of given hydrochloric acid and acetic acid in
the given mixture, by titrating with standard sodium hydroxide solution and calculate the amount of
each acid present in 1 litre of the solution.
PRINCIPLE
H+ + Cl-
Na+ + OH-
CH3COOH (aq) + Na+ (aq) + OH-aq
fast
slow
Na+ + Cl- + H2O (l)

CH3COO-(aq) + Na+(aq) + H2O(l)
PROCEDURE
C x (V+v) /V mho
Burette solution: standard sodium hydroxide solution

Pipette solution: 40 ml of the mixture of hydrochloric acid
and acetic acid
Cell: The conductivity cell
Initially the conductance is high due to the presence of fast moving H+ ions from HCl in the
(B)
mixture of acids.
(A)
NaOH is added slowly from the burette, 0.5 ml at a time. The conductance is noted for each
of NaOH(ml)
addition of NaOH. The conductance decreases for each addition, due toVolume
the replacement
of
+
+
fast moving H ions from HCl by slow moving Na ions.
When HCl is completely neutralized (end point A),the conductance increases gradually with
the gradual (0.5ml) addition of NaOH. This is due to the neutralization of CH3COOH by
NaOH.
After the neutralization of CH3COOH (end point B) the conductance increases sharply due
to presence of free OH- ions.
Strength of HCl
Volume of HCl
Amount of HCl
= Strength of HCl x Equivalent weight of HCl (36.5)
Strength of CH3COOH
Volume of CH3COOH
Amount of CH3COOH
= Strength of CH3COOH x Eq. wt. of CH3COOH (60)
RESULT
The strength of hydrochloric acid in the mixture of acids
The amount of HCl in 1 litre of the mixture of acids
The strength of Acetic Acid in the mixture of acids
The amount of CH3COOH in 1 litre of the mixture of acids
= ....N
= gm.
= ...N
= gm.
Page 28
Viva voce Questions and Answers
1. Give an example for strong acid and weak acid.
Strong acid: HCl
Weak acid: CH3COOH
2. Give an example for a strong base.
NaOH
3. Give reasons for decrease in conductance when a base is added to a mixture of acids initially.
At the beginning of the titration, the conductance of mixture of acids is due to H+
ions. When a base is added, the fast moving H+ ions are replaced by slow moving Na+ ions.
Hence, the conductance decreases.
4. Why the conductance increases linearly after the first end point?
The first end point corresponds to the neutralization of strong acid (HCl) by strong
base. After the first end point, the added base neutralizes the weak acid (CH3COOH). This
acid is feebly ionized and less amount of H+ ions are available to OH- ions for neutralization.
Hence, the conductance increases linearly.
5. Why the conductance increases sharply after the second end point when a base is added?
After the neutralization of mixture of acids, addition of base gives free OH- ions
which has high conductance and hence the conductance increases sharply..
6. Write the equivalent weights of HCl and CH3COOH
HCl
- 36.5
CH3COOH - 60
7. Write the formula used to calculate the amount of HCl and CH3COOH.
The amount of HCl = Normality x Equivalent weight of HCl (36.5)
The amount of CH3COOH = Normality x Equivalent weight of CH3COOH (60)
Page 29
Graph: Calibration curve (Absorbance Vs Concentration)
Absorbance
Concentration in ppm
TABLE I
Preparation of various concentration of Fe3+ solution
Volume of iron
solution (ml)
Volume of
HNO3 (ml)
Volume of
NH4SCN (ml)
Volume of distilled
H2O (to make equal
volume)
Concentration of
iron in ppm
Page 30
Expt. No
Date.
ESTIMATION OF IRON CONTENT OF THE WATER SAMPLE USING
SPECTROPHOTOMETER
AIM
To estimate the amount of ferric iron present in the given sample by thiocyanate method
using spectrophotometer.
PRINCIPLE
The estimation is based on Beer- Lamberts law, which states that When a beam of
monochromatic radiation is passed through a solution of an absorbing substance, the rate of decrease
of intensity of radiation with thickness of the absorbing solution is proportional to the intensity of
incident radiation as well as to the concentration of the solution. The law can be written in the form
of mathematical equation as,
Log I0 / It = cl = A
Where,
absorbance
I0
Intensity of incident light
It
Intensity of transmitted light
Concentration of solution
Thickness of the cell
Molar absorption co-efficient
Fe3+ + 6SCN-
[Fe (SCN) 6]3-
Fe3+ ions do not give any colour in solution. However a red colour can be produced, when it
reacts with a thiocyanate solution due to the formation of complex and complementary for this
colour will be in the blue region ( = 480 nm). So in the spectrophotometer, this radiation is allowed
to pass through the solution. The spectrophotometer will measure the incident radiation and the
transmitted radiation. To measure (I0), a blank solution (without Fe3+) is taken and the transmitted
light is measured, its absorbance is measured for various concentrations and a calibration graph can
be drawn with absorbance Vs concentration.
Page 31
TABLE II
Measurement of absorbance
Blank (distilled water): Zero absorbance; max = 480 nm
S. No.
Concentration
Absorbance
1ppm
0.01 N
2ppm
0.02 N
3ppm
0.03 N
4ppm
0.04 N
5ppm
0.05 N
6ppm
0.06 N
Unknown
-----
Calculation of amount of iron content

Amount of iron present in the given solution
= Normality Eq. wt. of iron 1000 ppm

= . 55.85 1000 ppm
= . ppm
Page 32
PROCEDURE
The spectrophotometer is switched on and warmed up for 10 minutes. The monochromator is
adjusted for max = 480 nm. The blank solution is kept in the cell and transmittance (I0) is measured.
Usually the instrument is calibrated for transmittance 100, for which absorbance is zero. Similarly
various known concentration of ferric iron solutions, after adding nitric acid and thiocyanate
solution, are kept in the instrument one by one and absorbance is measured in each case.
Now, the unknown solution (water sample) is treated with thiocyanate and nitric acid, kept in
the spectrophotometer and absorbance is measured. A calibration graph is drawn between
concentration and absorbance. From this, the unknown concentration is found out.
RESULT
The amount of ferric iron present in the given sample of water = ppm
Page 33
Short Procedure
AIM
To estimate the amount of ferric iron present in the given sample by thiocyanate method
using spectrophotometer.
PRINCIPLE
The estimation is based on Beer- Lambert law, which states that When a beam of
monochromatic radiation is passed through a solution of an absorbing substance, the rate of decrease
of intensity of radiation with thickness of the absorbing solution is proportional to the intensity of
incident radiation as well as to the concentration of the solution. The law can be written in the form
of mathematical equation as,
PROCEDURE
The monochromator is adjusted for = 480 nm.
The blank solution is kept in the cell and transmittance (I0) is measured.
Similarly for various known concentration of ferric iron solution, after adding nitric
acid and thiocyanate solution, the absorbance is measured.
Similarly, the absorbance for unknown solution is measured.
A calibration graph is drawn between concentration and absorbance. From this, the
unknown concentration is found out.
CALCULATION
Amount of iron present in the given solution
= Normality Eq. wt. of iron 1000 ppm
RESULT
The amount of ferric iron present in the given sample of water = ppm
Page 34

1. What is spectroscopy?
Spectroscopy is the measurement and interpretation of electromagnetic radiation
absorbed or emitted when the molecules or atoms or ions of a sample move from one allowed
energy state to another.
2. State Beer Lamberts law.
When a beam of monochromatic radiation is passed through a solution of an
absorbing substance, the rate of decrease of intensity of radiation with thickness of the
absorbing solution is proportional to the intensity of incident radiation as well as to the
concentration of the solution.
I0
Intensity of incident light
It
Intensity of transmitted light
Log I0 / It
= cl =
Concentration in moles/litre
Thickness of the cell
Absorbance or optical density
Molar absorption co-efficient
3. Write any two applications of Beer-Lamberts law

1. The concentration of colored solutions can be estimated.
2. The concentration of various industrial products can be determined.
3. The purity of chemical species can be determined.
4. Write any two reasons for the deviations from Beer-Lamberts Law.
Deviations from the law will occur when1. Monochromatic light is not used.
2. The colored solute ionized, dissociated or associated in the solution
3. Impurities are present in the solution
4. The solution undergoes polymerization.
Page 35
TABLE I
Preparation of various concentrations of polymer solution
Stock solution N1 = 1%
S. No.
Total volume V2 = 30 ml
Volume of 1% polymer solution

(stock solution) (V1 ml)
Volume of water (ml)
Concentration in % (N2)
N2 = V1N1 / V 2
1.
2.
3.
4.
5.
TABLE II
Viscosity data for a polymer / solvent
Flow time of the pure solvent (t0) = sec
S. No.
Concentration in %
(N2)
Flow time (t)

sec
(r) = t/t0
sp = r 1
sp/C = red
1.
2.
3.
4.
5.
Graph
sp/C
i
Concentration (%)
Page 36
Date
Expt.No
DETERMINATION OF MOLECULAR WEIGHT OF POLYVINYL ALCOHOL USING

OSTWALD VISCOMETER
AIM
To determine the molecular weight and degree of polymerization of the given polyvinyl
alcohol polymer solution (1%) using Ostwalds viscometer.
PRINCIPLE
Molecular weight of a polymer is nothing but the average molecular weight. This can be
determined by measuring the intrinsic viscosity (i) of a dilute polymer solution. This intrinsic
viscosity is related to the molecular weight of the polymer by the following relationship.
i
KMa (Mark - Hownik equation)
Where, i
Intrinsic viscosity
K&a
Constants for a given polymer solvent combination at a given

temperature
Average molecular weight
Degree of polymerization (Dp) provides another way of expressing the molecular weight as
follows.
Where,
Dp x m
molecular weight of the polymer
Dp
degree of polymerization
molecular weight of the monomer or the repeat unit
Important viscosity definitions:

Relative viscosity (r)
t/t0
Specific viscosity (sp)
r 1
Reduced viscosity (red) =
sp/C
Intrinsic viscosity (i)

Where,
lim sp/C
c0
Flow time for the polymer solution
t0
Flow time for the solvent
Concentration of the polymer
Page 37
CALCULATION
Mark Hownik equation is given by,
i
KMa
log i
log K + a log M
log i - log K
log M
=
a
log i - log K
= A. log
a
where, M = Molecular weight of the polymer.

Values of constants K and a for water polyvinyl alcohol system
K
a
= 4.53 x 10-4 and

= 0.64
Page 38
PROCEDURE
STEP I: Preparation of polymer solution of different concentration
Polymer solutions of different concentrations, say 0.1%, 0.2%, 0.3%, 0.4% and 0.5% are
prepared from the given polymer stock solution as shown in the table-I
STEP II: Flow time of solvent

20 ml of the solvent (water) is taken into the viscometer and is sucked through the capillary
tube up to the upper mark, without any air bubbles. Now note the flow time of the solvent to
flow from the upper mark (M1) to lower mark (M2) in the viscometer.
STEP III: Flow time of polymer solutions

The water is drained out completely and 20 ml solutions of polymer of different
concentrations are taken in the viscometer one after another by following the above procedure.
The flow time for various concentrations is determined.
(Wash and rinse the viscometer with water before taking the polymer solution of different
concentrations)
From the flow time, relative viscosity (r) can be calculated. A Graph is plotted between
sp/C and concentration (%). A straight line is obtained with an intercept called intrinsic
viscosity (i). From the value, the molecular weight of the polymer is calculated using
Mark Hownik equation.
RESULT
Molecular weight of the given polymer
=..
Degree of polymerization
=..
Page 39
Short Procedure
AIM
To determine the molecular weight and degree of polymerization of the given 1% polymer
solution (polyvinyl alcohol) using Ostwalds viscometer.
PROCEDURE
First water is taken in the viscometer upto the mark and flow time is noted in seconds.
Then Polymer solution (Poly vinyl alcohol) of different concentration are taken in the
viscometer and flow time is recorded for each concentration.
CALCULATION
By using, Mark Hownik equation, the molecular weight of the polymer is calculated.
i
=
log i =
KMa
log K + a log M
log i - log K
log M =
a
M = A.log log i - log K

a
Where, M
i
Where, i
K&a
= Molecular weight of the polymer.

= KMa (Mark - Hownik equation)
= Intrinsic viscosity
= Constants for a given polymer solvent combination at a given
temperature
M
= Average molecular weight
Degree of polymerization (Dp) = Molecular weight of the polymer
Molecular weight of the monomer (vinyl alcohol)
Graph
sp / C
i
Concentration (%)
RESULT
Molecular weight of the given polymer
Degree of polymerization
=..
=..
Page 40
1. Name the method used to determine the molecular weight of a polymer
Viscometry
2. What is the name of the viscometer used in this experiment?
Ostwalds Viscometer
3. Write Mark-Hownik equation.
i
KMa
Where,
Intrinsic viscosity
Constants for a given polymer solvent combination at a given
temperature
Average molecular weight
K&a =
M
4. What is the polymer used in this experiment?

Polyvinyl alcohol
CH 2
CH
OH
5. What are the values of K and a for water-polyvinyl alcohol system?

K = 4.53 x 10-4 and a = 0.64
6. What is the molecular weight of vinyl alcohol?
44
7. What is degree of polymerization? How is it calculated?
The number of monomer or repeat unit present in ae polymer is called
degree of polymerization, n or Dp. It is calculated as, Dp =M / m
Where, M = Average molecular weight of the polymer
m = molecular weight of the monomer
8. Write the relationship between different viscosities and flow time.
Relative viscosity (r)
t/t0
Specific viscosity (sp)
r 1 = (t/t0) - 1
Reduced viscosity (red) =
sp/C = ((t/t0) 1)/C
Intrinsic viscosity (i)
lim sp/C
c0
Flow time for the polymer solution.
Flow time for the solvent.
Concentration of the polymer.
Where,
t
t0
C
=
=
=
=
Page 41
Titration between standard HCl & NaOH
Volume of HCl (V) = 40 ml
Volume of NaOH
added (v) ml
Conductance (mho)
C x [(V+v)/V]
(mho)
0
2
4
6
8
10
12
14
16
18
20
22
24
26
28
30
32
34
36
38
40
Page 42
Expt. No..
Date
CONDUCTOMETRIC TITRATION OF STRONG ACID VS STRONG BASE

AIM
To determine the strength of given hydrochloric acid by conductometric titration against
N standard sodium hydroxide solution and calculate the amount of hydrochloric acid present
in 1 litre of the solution.
PRINCIPLE
When hydrochloric acid (H+ + Cl-) is titrated against sodium hydroxide, there is decrease in
the conductance. This is because of the replacement of fast moving H+ ions by the slow moving Na+
ions.
H+ + Cl-
+ NaOH
Na+ + Cl-
+ H2O
The decrease in the conductance continues up to the neutralization point. After all the H+ ions
are replaced, the added sodium hydroxide introduces excess of fast moving OH - ions. Hence,
conductance slowly increases after the neutralization point. A graph is drawn between the volume of
NaOH added (v) and C (V+v/V), where C is the conductance of the solution, V is the volume of HCl
taken and v is the volume of sodium hydroxide added. The end point is the exact point of
intersection of two straight lines.
PROCEDURE
The burette is filled with std. NaOH solution. Exactly 40 ml of given HCl is pipetted out into
a clean beaker. A glass rod is placed in the beaker. The conductivity cell is dipped into it. The
conductance of the solution is measured by connecting the terminals of conductivity cell with a
conductivity bridge. 2 ml of standard NaOH solution is added from the burette each time and
conductance of the solution is noted after each addition. This process is repeated until at least 5
readings are taken beyond the end point. The values of observed conductivity or C [(V+v)/V] are
plotted against the volume of NaOH added (v). The point of intersection in the graph gives the end
point. From the end point, the strength of acid is calculated and hence the amount of hydrochloric
acid in 1 litre is also calculated.
Page 43
Graph
CALCULATION
Strength of HCl
Volume of HCl
(V1)
= 40 ml
Strength of HCl
( N1)
= ................ ?
Volume of NaOH
(V2)
= ........... ...... ml (titre value)
Strength of NaOH
(N2)
= _________ N
According to the law of Volumetric analysis,

V1N1 = V2N2
Strength of HCl
Amount of HCl
Amount of HCl present in
= V2 x N2
V1
x
40
= .................N
C x (V + v ) / V mho
N1
= Normality of HCl x Equivalent weight of HCl

= .................. x 36.5
= --------------- gm.
Volume of NaOH (ml)
Page 44
RESULT
= .N
Amount of HCl present in 1 litre of the solution
= .gm.
Page 45
Short Procedure
AIM
To determine the strength of given hydrochloric acid by conductometric titration against
standard sodium hydroxide solution and calculate the amount of hydrochloric acid present in 1 litre
of the solution.
PRINCIPLE
+ NaOH
Na+ + Cl-
+ H2O
C x (V + v ) / V mho
H+ + ClPROCEDURE
Burette solution: Std. NaOH solution

Pipette solution: 40 ml of given HCl
Cell : Conductivity cell
Volume of NaOH (ml)
Initially the conductance is high due to the presence of fast moving H+ions from HCl.
NaOH is added slowly from the burette, 2 ml at a time. The conductance is noted for each
addition of NaOH. The conductance decreases for each addition, due to the replacement of
fast moving H+ ions from HCl by slow moving Na+ ions.
When the end point is reached, addition of NaOH increases the conductance.
End point is found out by plotting a graph between Volume of NaOH (X axis) and
Cx(V+v/V) (Y axis).
Strength of HCl

Volume of HCl
Amount of HCl
= Strength of HCl x Equivalent weight of HCl (36.5)
RESULT
= .N
Amount of HCl present in 1 litre of the solution
= .gm.
Page 46

1. What is conductance? Write its SI unit.
The current conducting capacity of a material is called conductance.
Its SI unit is Siemens, S.
2. What are specific conductance and equivalent conductance?
The conductance of one metre cube of an electrolyte solution is called specific
conductance and it is denoted by (kappa).
The conductance of an electrolyte solution containing one gram equivalent of the
electrolyte is known as equivalent conductance. It is denoted by (lambda).
3. How is specific conductance related with equivalent conductance?
=/V
where V is the volume of the solution containing one gram equivalent of the electrolyte.
4. Give examples for strong acid and weak acid.
Strong acid: HNO3, HCl, H2SO4
Weak acid : Acetic acid (CH3COOH), oxalic acid (C2H2O4), formic acid (HCOOH)
5. Explain why hydrochloric acid is a strong acid.
Hydrochloric acid is completely dissociated in all concentrations. Hence it is regarded
as strong acid.
HCl
H+ + Cl-
6. Explain why the strength of burette solution is always greater than the pipette solution in
conductometric titration.
We know that the dilution of the solution decreases the conductance value markedly.
Hence, burette is filled with concentrated solution to avoid dilution effect.
7. Give reasons for the decrease of conductance of an acid when a base is added initially to it.
At the beginning of the titration, the conductance of an acid is due to H+ ions. When
the base is added, the fast moving H+ ions are replaced by slow moving Na+ ions. Hence, the
conductance decreases.
8. Why the conductance increases when NaOH is added after the end point?
After the end point, further addition of NaOH results in the presence of free OH- ions,
which increases the conductance.
Page 47
9. What is the equivalent weight of (i) HCl (ii) NaOH
(i)
HCl : 36.5
(ii) NaOH : 40
10. What is the principle used to fix the end point of the titration?
When the conductance values are plotted against the volume of the burette solution,
we obtain two straight lines. The intersection of these two lines will be the end point of the
titration.
11. Write the formula that is used to calculate the amount of hydrochloric acid.
Weight of HCl per litre = Normality x Equivalent weight of HCl
= N x 36.5 g
12. What are the advantages of conductometric titrations?
1. Coloured solutions, which cannot be titrated by ordinary volumetric
methods with the help of indicators, can be successfully titrated
conductometrically.
2. The method can be employed in the case of very dilute solutions and also
for weak acids and bases.
3. No special care is necessary near the end point as it is determined
graphically.
13. What is cell constant?
Cell constant = l / a, where l is the length of the conductor and a is the area
of the electrode.
Page 48
SEMESTER - II
Page 49
LIST OF EXPERIMENTS
Expt. No.
Page No.
1.
Determination of alkalinity in water sample
53
2.
Determination of total, permanent & temporary

permanent hardness of water by EDTA method
61
3.
Estimation of copper content of the given solution by

EDTA method
71
4.
Estimation of iron content of the given solution using

potentiometer
77
5.
6.
7.
8.
Estimation of sodium present in water using

flame photometer
Corrosion experiment weight loss method
85
Conductometric precipitation titration using

BaCl2 and Na2SO4
Determination of CaO in cement
95
89
101
Page 50
TABLE OF CONTENTS
Ex. No.
Date
Marks
Signature of the
Obtained Staff with Date
Page 51
TABLE I
Titre values and different alkalinities
OH0
[P] or [M]
0
2[P] - [M]
0
Result of titration
If P = 0
If P = M
If P = 1/2M
If P > 1/2M
If P < 1/2M
CO320
0
2[P] or [M]
2[M-P]
2[P]
HCO3[M]
0
0
0
[M] 2[P]
Titration I: Standardization of hydrochloric acid

HCl Vs Std. NaOH
S. No.
Volume of sodium
hydroxide (ml)

Initial
Final
Volume of
hydrochloric acid (ml)
Indicator
CALCULATION
Strength of HCl
Volume of NaOH
(V1)
= 20 ml
Normality of NaOH
(N1)
= ________
Volume of HCl
(V2)
= ________ ml
Normality of HCl
(N2)
= ?
Strength of HCl (N2)

V1N1
= V2N2
N2
= V1N1
V2
20 x
= _______________ N
Page 52
Expt. No
Date
DETERMINATION OF ALKALINITY IN WATER SAMPLE

AIM
To determine the alkalinity of given water sample. A standard solution of N sodium
hydroxide and an unknown strength of hydrochloric acid are supplied.
PRINCIPLE
The presence of hydroxide, carbonate and bicarbonate ions mainly makes the water alkaline.
Therefore the alkalinity of a water sample is due to the presence of either one or more of the above
constituents. But hydroxide and bicarbonate ions cannot co-exist due to the following reaction.
2
OH
CO3
+ HCO3
+ H2O
The alkalinity in water may be determined by titrating the water against standard acid using
phenolphthalein and methyl orange indicators in which the following reactions take place.
a)
OH
b)
2
CO 3
+ H
+ H
H2O
HCO3
Phenolphthalein
end point (P)
The remaining half of the carbonate alkalinity and bicarbonate alkalinity are determined by
methyl orange indicator.
c) HCO3 + H+
H2O + CO2
Methyl orange end point (M)
The volume of acid consumed upto the colour change of phenolphthalein (P) shows the
completion of reactions a and b whereas that of methyl orange (M) shows the completion of
reaction c. The values (P) and (M) show the presence of alkaline constituents and their amount in
terms of volume of hydrochloric acid.
Alkalinity is expressed in terms of CaCO3 equivalent.
Page 53
Titration I: Estimation of alkalinity

Standard HCl Vs water sample
S. No.
Volume of
water sample (ml)
Volume of HCl
Phenolphthalein
Methyl orange
end point (P)
end point (M)
Concordant Value
[P]
[M]
Calculation:
From the values of [P] & [M] calculate the types of alkalinity present in the water sample using the
table 1.
Types of alkalinity
For example, if the data satisfies the condition P > M, both hydroxide & carbonate alkalinity are
present.
i)
Volume of HCl required for OH- alkalinity
=
2[P] [M]
ii)
iii)
1.
2 x---------- - ---------ml
2[M] 2[P]
2 x---------- -2 x ---------ml
(V1)
(N1)
(V2)
(N2)
=
=
=
=
------- ml
------- N
20 ml
?
N2
V1 x N1
20
`------------- N
Volume of HCl required for CO32- alkalinity
3-
HCO is not present.

Calculation of OH- alkalinity:
Volume of HCl
Strength of HCl
Due to OH- alkalinity
Strength of hydroxide alkalinity
x
20
Page 54
PROCEDURE
TITRATION I: STANDARDISATION OF HYDROCHLORIC ACID
Burette : Hydrochloric acid
Indicator: Phenolphthalein
Pipette: 20 ml of standard sodium hydroxide
End point: Just disappearance of pink colour
The burette is washed with water and rinsed with distilled water and hydrochloric acid. Then
it is filled with hydrochloric acid up to zero level mark and the initial burette reading is noted.
A 20 ml pipette is washed with water, rinsed with distilled water followed by the given
sodium hydroxide solution. Then 20 ml of sodium hydroxide solution is pipetted out into a clean
conical flask. A drop of phenolphthalein indicator is added. The solution becomes pink colour. It is
then titrated against hydrochloric acid taken in the burette. The end point is the just disappearance of
pink colour. The final burette reading is noted. Titrations are repeated for concordant values. The
readings are tabulated. From the titre value the strength of hydrochloric acid is calculated.
TITRATION II: ESTIMATION OF ALKALINITY
Indicator : 1. Phenolphthalein
2. Methyl orange
Pipette : 20 ml of given water sample
End point : 1. Just disappearance of pink colour

2. Golden yellow to pale pink colour
The burette is filled with hydrochloric acid up to zero level mark and the initial
reading is noted. A 20 ml pipette is washed with water and rinsed with the given water sample, then
exactly 20 ml of water sample is pipetted out into a clean conical flask. 2 drops of phenolphthalein
indicator are added. Pink colour is observed. The solution is titrated against the standard acid until
just disappearance of pink colour. The end point is noted (P). Then one drop of methyl orange
indicator is added to the same solution and the titration is continued against hydrochloric acid till the
appearance of pale pink colour. The final burette reading is noted (M). Titrations are repeated for
concordant values and the readings are tabulated.
Page 55
Amount of OH- content in1 lit of water sample,
in terms of CaCO3 equivalent
= strength of hydroxide alkalinity x

equivalent of CaCO3
OH- alkalinity interms of CaCO3 equivalent
= ------------------ x 50 x 103 ppm
Alkalinity due to OH- ion
= ---------------- ppm
2. Calculation of CO32- alkalinity:

Volume of HCl
(V1)
= ------- ml
Strength of HCl
(N1)
= .. N
(V2)
= 20 ml
(N2)
= ?
N2

Due to carbonate alkalinity
V1 x N1
20
Strength of carbonate alkalinity
x
20
= N
Amount of CO32- content in1 lit of water sample,

in terms of CaCO3 equivalent
= strength of carbonate alkalinity x

equivalent of CaCO3
Carbonate alkalinity in terms of

CaCO3 equivalent
= ------------------ x 50 x 103 ppm
Alkalinity due to carbonate
= ---------------- ppm
Page 56
From the values of P & M, the type of alkalinity present in the water sample is found out and
then the amount of each alkalinity is calculated in terms of CaCO3 equivalent.
RESULT
The given water sample contains the following alkalinity
Hydroxide alkalinity
= .ppm
Carbonate alkalinity
= .ppm
Bicarbonate alkalinity
= .ppm
Page 57
Short Procedure
AIM
To determine the alkalinity of given water sample. A standard solution of N sodium
hydroxide and an unknown strength of hydrochloric acid are supplied.
PRINCIPLE
Alkalinity is the ability to neutralize acid. Water may be alkaline due to the presence
of hydroxide , carbonate or bicarbonate ions. The type of alkalinity and amount can be found out by
titration with standard HCl using phenolphthalein and methyl orange indicators.
PROCEDURE: TITRATION I: STANDARDISATION OF HYDROCHLORIC ACID
Indicator: Phenolphthalein
Pipette: 20 ml of standard sodium hydroxide
Strength of HCl
End point: Just disappearance of pink colour

Volume of HCl
TITRATION II: ESTIMATION OF ALKALINITY

Indicator : 1. Phenolphthalein
2. Methyl orange
Pipette : 20 ml of given water sample
End point : 1. Just disappearance of pink colour

2. Golden yellow to pale pink colour
if the data satisfies the condition P > M, both hydroxide & carbonate alkalinity are present.
i) OH- alkalinity
Strength of OH- alkalinity
Amount of OH- alkalinity
ii) CO32- alkalinity
Strength of CO32- alkalinity
Amount of CO32-alkalinity
= 2[P] [M] (Phenolphthalein end point)

= Volume of HCl x Strength of HCl
= Strength of water sample x Eq. wt. of CaCO3 (50)
= 2[M] 2[P] (Methyl Orange end point)
= Volume of HCl x Strength of HCl
= Strength of water sample x Eq.Wt. of CaCO3(50)
RESULT
The given water sample contains the following alkalinity
Hydroxide alkalinity
= .ppm
Carbonate alkalinity
= .ppm
= .ppm
Page 58
1. What is meant by alkalinity of water?
Capacity to neutralize acid
2. What are the ions causing alkalinity?
Hydroxide, carbonate and bicarbonate ions.
3. What are the possible combinations of ions for alkalinity?
(i) OH- and CO32- (ii) HCO3- and CO324. What is the role of phenolphthalein indicator?
It is used to find the alkalinity caused by hydroxide ions and half of the carbonate ions.
5. What is the role of methyl orange indicator?
To find out the alkalinity caused by bicarbonate and other half of the carbonate ions.
6. Hydroxides and bicarbonates cannot exist together. Why?
Hydroxides and bicarbonates cannot exist together due to the following reaction.
2
OH
+ HCO3
CO3
+ H2O
7. What type of alkalinity is present if P = 0?

8. What is the burette solution used?
HCl
9. Explain why two indicators are used in the same titration?
Phenolphthalein indicator is not suitable for bicarbonate alkalinity and hence
methyl orange indicator is also used to find out bicarbonate alkalinity in the same titration.
10. How is the amount of alkalinity expressed?
The alkalinity is expressed in terms of CaCO3 equivalent and the unit is ppm or mg/L.
11. Which is strong? OH- or HCO3- ions.
OH- ions
12. What type of indicators is used in this experiment?
Acid - base neutralization indicators.
13. What are the ions responsible for alkalinity if P = M?
Only OH- ions
14. When P > 1/2M, what are the ions responsible for alkalinity?
OH- and CO32- ions
Page 59
Titration I: Standardization of EDTA
Standard hard water Vs EDTA
S. No.
Volume of standard
hard water (ml)

Initial
Volume of
EDTA (ml)
Final
Indicator
CALCULATION
Strength of EDTA
Volume of standard hard water
= 20 ml
Volume of EDTA solution consumed, V1
= ml
1ml of standard hard water contains 1mg of calcium carbonate

20 ml of standard hard water contains 20 mgs of CaCO3
20 ml of standard hard water consumes V1 ml of EDTA
i.e., V1 ml of EDTA solution
= 20 mgs of CaCO3
1ml of EDTA solution
= 20
mg of CaCO3 equivalent
V1
Page 60
Expt. No
Date.......
DETERMINATION OF TOTAL, TEMPORARY & PERMANENT HARDNESS OF

WATER SAMPLE BY EDTA METHOD
AIM
To determine the total hardness, permanent hardness and temporary hardness of the given
water sample by EDTA method. Standard hard water and a link solution of EDTA are supplied.
PRINCIPLE
Hardness
producing
Ca2+
ions
and
Mg2+
form
complexes
with
both
EDTA
(Ethylenediaminetetraacetic acid) and EBT (Eriochrome black T). But EDTA metal ion complex
is more stable than EBT metal ion complex.
Ca2+ or Mg2+ + EB
(In water)
pH 9-10
Ca EBT or Mg EBT + EDTA2-
Ca EBT or Mg EBT + 2H+

(Less stable, wine red)
pH 9-10
[Ca EDTA] 2- or [Mg EDTA] 2- + EBT

(More stable, colourless)
(Purple blue)
The end point of the titration is colour change from wine red to purple blue.
PROCEDURE
TITRATION I: STANDARDISATION OF EDTA
Burette : EDTA
Indicator : EBT
Pipette
: 20 ml std. hard water
End point : Wine red to purple blue colour
Condition: 5 ml of ammonia buffer solution

A 50 ml burette is washed with water and rinsed with EDTA. Then it is filled with EDTA solution
up to zero mark and the initial burette reading is noted. A 20 ml pipette is washed with
water and rinsed with the given std. hard water (1 ml 1 mg of CaCO3), then exactly 20 ml of std.
hard water is pipetted out into a 250 ml clean conical flask.
Page 61
Titration II: Estimation of total hardness
Given water sample Vs EDTA
Volume of given
S. No.
water sample
(ml)

Initial
Final
Volume of
EDTA
(ml)
Indicator
Calculation of the total hardness of the given water sample

Volume of hard water
= 20 ml
Volume of EDTA consumed, (V2)
= . ml
20 ml of the given hard water sample consumes
V2 ml of EDTA
1000 ml of the given hard water sample contains
20 x V21000
mg of CaCO3
V1 x 20
= 1000 V2 / V1 mg of CaCO3
=
=..ppm
Total hardness of the given sample
= ..ppm
Page 62
To this 5 ml of ammonia buffer solution (approximately half test tube) and 2 drops of EBT
indicator are added. The solution becomes wine red colour. This solution is titrated against EDTA
solution taken in the burette. End point is change of colour from wine red to purple blue. Final
burette reading is noted. The titration is repeated for concordant values. The readings are tabulated.
Let the volume of EDTA be V1 ml.
TITRATION II: ESTIMATION OF TOTAL HARDNESS
Burette : EDTA
Indicator : EBT
Pipette
End point : Wine red to purple blue
Condition : 5 ml of ammonia buffer solution

The burette is filled with the same EDTA solution up to zero mark and the initial burette
reading is noted. The pipette is washed with distilled water and rinsed with the given water sample.
Then 20 ml of water sample is pipetted out into a clean conical flask. To this 5 ml of buffer solution
and 2 drops of EBT indicator are added. The solution becomes wine red in colour. This solution is
titrated against EDTA solution taken in the burette. End point is change of colour from wine red to
purple blue. Final burette reading is noted. The titration is repeated for concordant values. The
readings are tabulated. Let this volume of EDTA be V2 ml. From the titre value V2, the total hardness
of water sample is calculated.
TITRATION III: ESTIMATION OF PERMANENT HARDNESS
Burette : EDTA
Indicator : EBT
Pipette
: 20 ml of boiled water sample

The burette is filled with EDTA up to zero mark and the initial burette reading is noted.
Page 63
Titration III: Estimation of permanent hardness
Boiled water sample Vs EDTA
S. No.
Volume of given
boiled water
sample (ml)

Initial
Volume of
EDTA (ml)
Final
Indicator
Calculation of permanent hardness

Volume of the boiled hard water
= 20 ml
Volume of the EDTA solution consumed , (V3)
=..ml (titre value)
20 ml of the boiled hard water sample consumes V3 ml of EDTA

i.e. 20 ml of boiled hard water sample contains
20 x V3
mg of CaCO3
V1
1000 ml of boiled hard water sample contains
= 20 x V3 x 1000
V1 x 20
= 1000 V3 / V1 mg of CaCO3
=
= ppm
Permanent hardness
Estimation of temporary hardness

Temporary hardness
=
=
Total hardness - Permanent hardness

-------------------- - -----------------------
= -------------ppm
Page 64
20 ml of boiled, cooled and filtered hard water sample (temporary hardness removed water
sample) is pipetted out into a clean conical flask. 5 ml of buffer solution and 2 drops of EBT are
added to it. It is titrated against EDTA. The end point is change of colour from wine red to purple
blue. Let the volume of EDTA be V3 ml. From the titre value, the permanent hardness can be
calculated.
The temporary hardness of the water sample can be found out by subtracting the value of
permanent hardness from the value of total hardness.
RESULT
Total hardness of given water sample
ppm
Permanent hardness of given water sample
. ppm
Temporary hardness of given water sample
. ppm
Page 65
Short Procedure
AIM
To determine the total hardness and also the permanent hardness of the given water sample.
Standard hard water and a link solution of EDTA are supplied.
PRINCIPLE
Ca2+ or Mg2+ + EBT
(In water)
Ca EBT or Mg EBT + EDTA2-
Ca EBT or Mg EBT + 2H+

(Less stable, wine red)
[Ca EDTA] 2- or [Mg EDTA] 2- + EBT
(More stable, colourless)
(Purple blue)
PROCEDURE
Burette : EDTA
Indicator : EBT
Pipette
: 20 ml of std. hard water

Strength of EDTA = Volume of std. hard water x Strength of std. hard water
Volume of EDTA
TITRATION II: ESTIMATION OF TOTAL HARDNESS
Burette : EDTA
Indicator : EBT
Pipette

Total hardness = Volume of EDTA for 20 ml of given hard water x 1000
Volume of EDTA for 20 ml of std. hard water
TITRATION III: ESTIMATION OF PERMANENT HARDNESS
Burette : EDTA
Indicator : EBT
Pipette
: 20 ml of boiled water sample
End point : Wine red to purple colour

Permanent hardness = Volume of EDTA for 20 ml of boiled hard water x 1000
Volume of EDTA for 20 ml of std. hard water
RESULT
Total hardness of given water sample
=
ppm
Permanent hardness of given water sample
. ppm
Temporary hardness of given water sample
. ppm
Page 66
1. What are the different sources of water?

Ocean, River, Lake, Spring, Rain water.
2. Why rain water is considered to be the purest form of natural water?
Since the rain water is free from any dissolved salt, it is considered to be the purest form of
natural water.
3. Name the impurities present in natural water.
(i) Suspended impurities (ii) Dissolved impurities (iii) Colloidal impurities
4. Define hard water.
The water which does not readily lather with soap but forms precipitate is known as hard
water.
5. What is soft water?
The water which gives lather easily with soap is called soft water.
6. What is EDTA?
EDTA is, Ethylenediaminetetraacetic acid.
7. Give the structure of EDTA
CH2 - COOH
HOOC - H2C
N - CH2 - CH2 - N
HOOC - H2C
CH2 - COOH
8. Mention the link solution that is used in the determination of hardness of water
EDTA solution
9. What are the types of hardness?
(i) Carbonate hardness (or) Temporary hardness
(ii) Non- carbonate hardness (or) Permanent hardness
10. What is temporary hardness?
Hardness caused by bicarbonates of Ca & Mg is called temporary hardness.
11. What is permanent hardness?
Hardness caused by chlorides and sulphates of Ca & Mg is called permanent hardness.
12. What happens on boiling the hard water?
If temporary hardness is present, it is removed.
Page 67
13. How hardness of water is expressed?
It is expressed in terms of CaCO3 equivalent.
14. Why CaCO3 is chosen as standard to express hardness?
Its solubility is less. Its Molecular weight is 100 and Equivalent weight is 50 which is easy
for calculation.
15. Define pH
pH of any solution is defined as
pH = -log10 aH+, where aH+ is the activity of the hydrogen ions. For dilute solutions,
activity can be replaced by concentration. i.e., pH = -log10 [H+]
16. What is the function of buffer solution?
To maintain the pH of a reaction medium.
17. What are buffer solutions?
A mixture of weak acid and its salt or weak base and its salt is known as buffer solution.
18. What are the units of hardness?
1. ppm Parts per million. It is the number of parts of hardness producing substances (in
terms of CaCO3) present per million parts of water.
2. mg/L: milligram per litre. It is the number of milligram of calcium carbonate equivalent
hardness present in 1litre of water.
3. Clarkes Degree (0Cl): It is the number of parts of CaCO3 equivalent hardness present in
70,000 parts of water. (i.e., in one gallon of water).
4. Degree of French (0Fr): It is the number of parts of CaCO3 equivalent hardness present in
105 parts of water.
The above 4 units are correlated as given below.
1 ppm = 1 ml / L = 0.07 0Cl = 0.1 0Fr
19. Why the pH of the solution is maintained between 6 to10?
Eriochrome Black - T is the metal ion indicator. This dyestuff tends to polymerize in strongly
acidic solution to a red brown product and hence the indicator is generally
used with
solution having pH greater than 6.0.
Page 68
20. Name other indicators beside Eriochrome Black T which could be used for the
determination of hardness.
Murexide (ammonium salt of purpuric acid), solochrome dark blue or calcon, Zincon and
Xylenol orange.
21. Name the different methods of determining hardness.
1. O-Hehners method
2. Soap titration method
3. EDTA method
Page 69
Titration I: Standardization of EDTA
Standard CaCO3 Vs EDTA
S. No.
Volume of standard
calcium carbonate (ml)

Initial
Final
Volume of
EDTA (ml)
Indicator
CALCULATION
Strength of EDTA
Volume of std. CaCO3 solution V1
20 ml
Strength of std. CaCO3 solution N1
-------- N
Volume of EDTA
V2
-------- ml
Strength of EDTA
N2
N2
V1 x N1
20 x
V2
Strength of EDTA
N2
--------- N
Page 70
Expt. No.
Date .
ESTIMATION OF COPPER CONTENT OF THE GIVEN SOLUTION BY

EDTA METHOD
AIM
To estimate the amount of copper present in 100 ml of the given brass solution. A standard
solution of CaCO3 of strength -------N and an approximately 0.01 M EDTA solution are provided.
PRINCIPLE
Brass is an alloy of 55% copper and 33% zinc. The purpose of alloying copper and zinc is to
improve machinability and strength. Brass may also contain small amounts of lead, tin or
aluminium.
In this method, brass is dissolved in con. HNO3, so that copper present in the brass is brought
into solution in the form of cupric ions. Then the Cu2+ ion is determined by the usual
complexometric method using EDTA.
Cu2+
+
(Copper ions)
FSB-F
[Cu-FSB-F] +
EDTA2-
[Cu-FSB-F] + 2H+
(Purple colour)
[Cu- EDTA]2(Colourless)
+ FSB-F
(Green colour)
PROCEDURE
Burette : EDTA
Indicator : EBT
Pipette
: 20 ml of std. CaCO3

The burette is washed well with distilled water and rinsed with the small amount of given
EDTA solution. It is then filled with the same solution up to the zero mark without any air bubbles.
The pipette is washed with distilled water and rinsed with the small amount of standard CaCO3
solution. 20 ml of this solution is pipetted out into a clean conical flask.
Page 71
Titration II: Estimation of copper

Standard EDTA Vs brass solution
S. No.
Volume of given
brass solution (ml)
Initial
Volume of
EDTA (ml)
Final
Indicator
CALCULATION
Strength of brass solution
Volume of EDTA
V1
---------- ml
Strength of EDTA
N1
-------N
Volume of brass solution
V2
20 ml
Strength of brass solution
N2
N2
V1 x N1
= x
V2
Strength of copper in brass solution
20
= N
Amount of copper in Brass

Amount of Cu in 100 ml of given
brass solution
strength of Cu x equivalent wt. of Cu x 100

1000
------------------ x 63.54
= gm.
10
Page 72
5 ml of ammonia buffer solution and 2 drops of EBT indicator are added. The solution turns wine
red in colour and it is then titrated against EDTA taken in the burette. The change of wine red colour
to purple blue colour is the end point. The final reading is noted. The titration is repeated to get
concordant values. From the volume of EDTA consumed, strength of EDTA solution is calculated.
TITRATION II: ESTIMATION OF COPPER
Burette : EDTA
Indicator :
Fast sulphon black - F
Pipette
End point:
Blue to green colour
: 20 ml of given brass solution

The given brass solution is made up to 100 ml in a standard measuring flask. 20 ml of this
solution is pipetted out into a clean conical flask. 5 ml of ammonia buffer solution and 3-4 drops of
fast sulphon black - F indicator are added. The solution turns blue in colour. The solution is titrated
against standard EDTA solution taken in the burette. The change of blue colour into green colour is
the end point. The titration is repeated to get concordant values.
Equivalent weight of copper = 63.54
RESULT
Strength of copper solution
= ..N
Amount of copper present in 100 ml of the given solution
= ..gm.
Page 73
Short Procedure
AIM
To estimate the amount of copper present in 100 ml of the given brass solution. A standard
solution of CaCO3 of strength -------M and an approximately 0.01 M EDTA solution are provided.
PRINCIPLE
Cu2+
+
(Copper ions)
FSB-F
[Cu-FSB-F] + 2H+
(Purple colour)
[Cu-FSB-F] +
EDTA2-
[Cu- EDTA]2(Colourless)
+ FSB-F
(Green colour)
PROCEDURE
Burette : EDTA
Indicator : EBT
Pipette
: 20 ml of std. CaCO3

Strength of EDTA
Volume of CaCO3 x Strength of CaCO3

Volume of EDTA
TITRATION II: ESTIMATION OF COPPER
Burette : EDTA
Indicator :
Fast sulphon black - F
Pipette
: 20 ml of given brass solution
End point:
Blue to green colour

Strength of copper
Amount of copper in 100 ml =
Volume of EDTA x Strength of EDTA

Volume of brass solution
Strength of copper x Eq. wt. of copper (63.54)
10
RESULT
Strength of copper solution
= ..N
Amount of copper present in 100 ml of the given solution
= ..gm.
Page 74
1. What is an alloy?
Alloy is a homogenous mixture of a metal with another metal or a metal with a non
metal or two metals with a non metal.
2. How are alloys classified?
Alloys are classified into (i) ferrous alloys (ii) non ferrous alloys
3. What is amalgam?
An alloy of mercury with a metal is called by the special name amalgam.
4. Name two ferrous alloys.
Steel, nichrome
5. Give examples for non ferrous alloys.
Brass, bronze and german silver
6. Name few alloys of copper.
Brass, bronze, solder, gun metal
7. What are the constituents present in brass?
Cu & Zn
8. What is the basic difference between brass and bronze?
Brass is an alloy of copper with zinc, whereas bronze is an alloy of copper with tin.
9. Name the metal ion indicator that is used in the estimation of copper in brass.
Fast sulphon black F (FSB - F)
10. What is the end point of the titration?
Purple colour is changed to green colour.
11. Mention the link solution that is used in the brass analysis
EDTA
12. What is the equivalent weight of copper?
63.54
14. What is the percentage of copper in brass?
From 55 60 %
15. What type of indicator does fast sulphon black-F belong to?
Metal ion indicator
Page 75
Titration I: Potassium dichromate Vs ferrous salt solution

Volume of ferrous sulphate solution = 20 ml
Volume of K2Cr2O7 added (ml)
Emf (milli volt)
0
2
4
6
8
10
12
14
16
18
20
Page 76
Expt. No
Date.
ESTIMATION OF IRON CONTENT OF THE GIVEN SOLUTION USING

POTENTIOMETER
AIM
To estimate the amount of ferrous iron in one litre of the given solution by potentiometric
titration. A standard solution of potassium dichromate of strengthN is provided.
PRINCIPLE
Potentiometric titration depends on the measurement of emf between reference electrode and
an indicator electrode. When a solution of ferrous salt is titrated with a solution of K2Cr2O7 the
following redox reaction takes place.
K2Cr2O7 + 6FeSO4 + 7H2SO4
K2SO4 + Cr2 (SO4)3 + 3Fe2 (SO4)3 + 7H2O
The ferrous ions are oxidized by Cr6+ ions. The potential slowly increases and at the end
point, there will be a sudden increase in potential. The cell is set up by connecting this redox
electrode with a calomel electrode as shown below:
Hg / Hg2Cl2(s), KCl // Fe2+,Fe3+ / Pt
The emf of the cell is measured by means of a potentiometer. The end point is obtained by
plotting the measured emf against volume of the K2Cr2O7 solution added.
PROCEDURE
Exactly 20 ml of given ferrous sulphate solution is pipetted out into a clean 100 ml beaker
and one test tube of dil. H2SO4, is added to it. A bright platinum electrode and calomel electrode are
dipped into the solution. This cell is connected to the potentiometer and the potentials are measured
for every 2 ml addition of potassium dichromate from the burette. This procedure gives the
approximate end point. Accurate end point can be determined by adding 0.2 ml K2Cr2O7 solution
near the end point. The end point is obtained by plotting emf (E) Vs volume of K2Cr2O7 or
Page 77
TABLE II
Volume of K2Cr2O7
(ml)
Emf
(mv)
E
(mv)
V
(ml)
E / V
(mv/ ml)
Page 78
E / V Vs volume of K2Cr2O7. From the end point the strength and the weight of ferrous iron
present in the whole of the given solution are calculated.
Page 79
Graph 2: volume of K2Cr2O7 Vs E/V
Graph 1: Volume of K2Cr2O7 Vs. emf
E/V
mv/ml
Emf
(mv)
Volume of K2Cr2O7 (ml)
CALCULATION
Strength of ferrous iron solution
Volume of ferrous iron solution
V1
= 20 ml
N1
= ?
Volume of K2Cr2O7,
V2
= ............. ml
Strength of K2Cr2O7,
N2
= . N
N1
= V2 x N2
= .. x ..
V1
N1
20
= ..................... N
Amount of ferrous iron

The amount of ferrous iron present
= Strength of ferrous iron x eq.wt. of iron
in 1000 ml of the solution
. N x 55.85
= ..gm.
Page 80
RESULT
The amount of ferrous iron present in one litre of the given solution =.gm.
Page 81
Short Procedure
AIM
To estimate the amount of ferrous iron in one litre of the given solution by potentiometric
titration. A standard solution of potassium dichromate of strengthN is provided.
PRINCIPLE
K2SO4 + Cr2 (SO4)3 + 3Fe2 (SO4)3 + 7H2O
PROCEDURE
Burette
: Potassium dichromate (K2Cr2O7)
Pipette
: 20 ml of ferrous sulphate
End point
: Gradually Emf increases
Condition
: One test tube of dil. H2SO4
Electrode
: Platinum electrode and calomel electrode
Strength of ferrous iron =
Volume of K2Cr2O7 x Strength of K2Cr2O7

Volume of ferrous sulphate
Amount of ferrous iron = Strength of ferrous iron x Equivalent weight ferrous iron (55.85)
Graph 1: Volume of K2Cr2O7 Vs. emf
Graph 2: volume of K2Cr2O7 Vs E/V
E/V
mv/ml
Emf
(mv)
RESULT
The amount of ferrous iron present in one litre of the given solution =.gm.
Page 82
1. Define emf.
The amount of charge produced in any material or cell is called emf.
2. What is the unit for emf?
------- Volt
3. What are the redox reactions? Give example.

The reactions in which both oxidation and reduction take place simultaneously are
called redox reactions.
K2SO4 + Cr2 (SO4)3 + 3Fe2 (SO4)3 + 7H2O
Here Fe2+ is oxidized to Fe3+ and Cr6+ is reduced to Cr3+

4. Give examples for oxidizing and reducing agents
Oxidizing agents: KMnO4, K2Cr2O7, HNO3
Reducing agents: Oxalic acid, ferrous sulphate, FAS
5. What are the two types of standard electrodes? Give example.
a. Primary reference electrode
: Eg. H2 electrode
b. Secondary reference electrode: Eg. Calomel electrode, Glass electrode,

Quinhydrone electrode
6. Name the ion which is reduced in this titration: Answer - Chromium (VI) ion (Cr6+ ion)
7. Name a reference electrode: Answer - Calomel electrode
8. Why it is said to be a reference electrode?
Its standard electrode potential value is known and from which we can measure the
potential of other electrode.
9. What is calomel? : Answer - Calomel is mercurous chloride (Hg2Cl2)
10. Define oxidation and reduction.
Loss of electrons and increase in +ve charge or decrease in ve charge oxidation
Gain of electrons and decrease in +ve charge or increase in ve charge reduction
11. What is the name of the plot E / V Vs volume?
First derivative graph and it gives accurate end point.
12. Name the electrodes used in this titration.
Platinum electrode and calomel electrode
Page 83
0.6
Absorbance
(or)
Emission
Concentration
Determination of Na+ ion in the sample water
max = 589 nm
Volume of solution
Concentration
Distilled water = Zero reading

Absorbance (or)
emission
(Standard)
(Unknown)
Page 84
Expt. No
Date.
ESTIMATION OF SODIUM PRESENT IN WATER USING
FLAME PHOTOMETER
AIM
Determine the amount of sodium present in the given water sample. A standard solution of
sodium chloride containing 100 mg of sodium per litre (1000 ppm) is provided.
PRINCIPLE
When a solution containing a metallic compound is aspirated into a flame, a vapour
containing the metal atoms will be formed. Some of these metal atoms in gaseous state, may be
raised to an energy level, which is sufficiently high to permit the emission of radiation, which is
characteristic to the metal under test. Since metals like sodium, potassium and lithium have an easily
excited flame spectrum of sufficient intensity for detection by a photocell, they are usually analysed
by flame photometer.
PROCEDURE
Exactly 2.54 g of pure dry sodium chloride is dissolved in 1 litre of distilled water. This
solution contains 1000 mg of sodium per litre. This stock solution is diluted to prepare four standard
solutions of 10, 5, 2.5 and 1 ppm sodium ions respectively.
A calibration curve is plotted, using solutions of known concentrations. The test solutions
may be suitably diluted to get readings in the range 0.1 to 0.4. The absorbance emission readings are
taken in the flame photometer for different concentrations at 589 nm wavelength. The unknown
concentration of sodium in water sample is found out with the help of the calibration curve.
Note: The amount of potassium in a given water sample may also be estimated by similar procedure
and measuring the absorbance at 766 nm.
RESULT
The amount of sodium present in the given water sample
= ppm
Page 85
Short Procedure
AIM
Determine the amount of sodium present in the given water sample. A standard solution of
sodium chloride containing 100 mg of sodium per litre (1000 ppm) is provided.
PRINCIPLE
When a solution containing a metallic compound is aspirated into a flame, a vapour
containing the metal atoms will be formed. Some of these metal atoms in gaseous state, may be
raised to an energy level, which is sufficiently high to permit the emission of radiation, which is
characteristic to the metal under test. Since metals like sodium, potassium and lithium have an easily
excited flame spectrum of sufficient intensity for detection by a photocell, they are usually analysed
by flame photometer.
PROCEDURE
A standard solution of sodium chloride is prepared.
It is diluted to four or five different concentrations.
The absorbance at 589 nm is measured in a flame photometer for various concentrations.
The absorbance is measured for unknown concentration.
A graph is plotted between absorbance and concentration.
From the graph concentration is found out.
CALCULATION
Amount of sodium = Concentration of NaCl solution x Eq. wt of sodium (23)
RESULT
The amount of sodium present in the given water sample
= ppm
Page 86

1. What is flame photometry?
It is a method in which, the intensity of the emitted light is measured when a atomized metal
is introduced in to a flame.
2. What are process involved in the estimation of sodium?
1. Evaporation
2. Vaporization
3. Dissociation
4. Thermal excitation
5. Emission
3. What are important components of flame photometry?
1. Burner
2. Mirror
3. Silts
4. Prisms
5. Detector
6. Amplifier
7. Recorder
4. What is the wavelength of the filter used in the estimation of sodium?
589 nm
5. What is the wavelength of the filter used for the estimation of potassium?
766 nm
Page 87
DETERMINATION OF RATE OF CORROSION BY WEIGHT LOSS METHOD
S. No.
Initial weight of steel

specimen (W1) gm
Final weight of
steel specimen
(W2)
Percentage of
HCl
Weight loss
(W1-W2) gm
CALCULATION
Rate of corrosion
( )
Page 88
Expt. No
Date.
CORROSION EXPERIMENT- WEIGHT LOSS METHOD
AIM
To determine the corrosion rate of mild steel specimen in HCl different concentrations at
constant temperature.
PRINCIPLE
Generally metal surfaces are covered with impurities like rust and scales. These impurities if
present at the time of coating will produce porous and discontinuous coatings. In order to get a
uniform, smooth, and adherent coating, these substances must be removed by acid cleaning (or)
pickling for which dil.HCl is used as pickling solution.
Acid cleaning is applicable to remove the scale by oxidation of metal

Fe Fe2+ + 2eDuring this process the metal ions, along with rust, get dissolved in the pickling solution. Such
dissolution is called corrosion. As the time increases the rate of corrosion also increases.
PROCEDURE
The mild steel specimens (1-5) of known dimensions are taken, washed with distilled water
and air dried. Initial weights of the specimens (1-5) are noted as W1 gm.
Similarly HCl of different concentration (3%, 6%, 9%, 12%, 15%) are prepared (called
pickling solution). Now each steel specimen is dipped in 100 ml of the above five different
concentration of HCl for 30 minutes. After that they are taken out and washed with distilled water
thoroughly and air dried. Again the specimens (1-5) are weighted and the final weights are noted as
W2 gm.
Page 89
Page 90
From the weight loss, the rate of corrosion can be calculated using the following relation.
Rate of corrosion
( )
Where W1 is the initial weight of the steel specimen (in grams)

W2 is the final weight of the steel specimen (in grams)
A is the area of the specimen in cm2
D is the density of the specimen in gm/cm3
T is the time of exposure (in hrs)
RESULT
Rate of corrosion
= --------------- .
Page 91
Short Procedure
AIM
To determine the corrosion rate of mild steel specimen in HCl of different concentrations at
constant temperature.
PRINCIPLE
Corrosion is a process of gradual destruction of metals by the chemical or
electrochemical reaction with its environment. Experimentally corrosion can be measured by dipping
a mild steel plate in a known concentration of an acid for a particular time. The rate of corrosion can
be determined with different concentration and different time.
PROCEDURE
The mild steel specimens of known dimensions are taken, washed with distilled water and air
dried. Initial weights of the specimens are noted as W1 gm.
Similarly HCl of different concentration (3%, 6%, 9%, 12%, 15%) are prepared (called
pickling solution). Now the steel specimens are dipped in 100 ml of various HCl solutions for 30
minutes. After that they are taken out and washed with distilled water thoroughly and air dried.
Again the specimens are weighted and the final weights are noted as W2 gm.
Rate of corrosion
( )
Where W1 is the initial weight of the steel specimen (in gm)

W2 is the final weight of the steel specimen (in gm)
A is the area of the specimen in cm2
D is the density of the specimen in gm/cm3
T is the time of exposure (in hrs)
RESULT
Rate of corrosion
= --------------- .
Page 92
Viva voce question and answers.
1. What is meant by corrosion?

Gradual destruction of metals by the chemical or electrochemical reaction with its
environment.
2. What is rate of corrosion?
The speed with which the metal changes into corrosion products.
3. Write the expression to calculate rate of corrosion.
Rate of corrosion
( )
W1
= Initial weight of the steel specimen
= Area of the specimen
W2
= Final weight of the steel specimen
= Time of exposure
= Density of the specimen
4. What are the types of corrosion?

1. Dry corrosion
2. Wet corrosion
5. Name some important coatings.
a) Paint b) Varnish c) Chromium coating
6. What is the equivalent weight of iron?
55.85.
7. Name of factors which influence rate of corrosion.
1. Position of the metal in emf series
2. Area of anode and cathode
3. Over voltage
4. Temperature and pH of the environment
8. What is the reaction taken place during acid cleaning.
Oxidation takes place on the metal
Fe Fe2+ + 2e9. How is the corrosion rate expressed?
1. Millimeter per year (mpy), 2. Inch per year (ipy), 3. mg per dm2 per day (mdd)
Page 93
Titration between BaCl2 Vs Na2SO4
Volume of Na2SO4 added (ml)
Conductance (mho)
0
2
4
6
8
10
12
14
16
18
20
22
24
26
28
30
32
34
36
38
40
Page 94
Expt. No
Date.
CONDUCTOMETRIC PRECIPITATION TITRATION USING
BaCl2 AND Na2SO4
AIM
To determine conductometrically the strength of given sodium sulphate solution by titrating
it with a standard solution of .N barium chloride.
PRINCIPLE
The reaction between sodium sulphate and barium chloride may be represented as,
2Na+ + SO42-
Ba2+ + 2Cl-
2Na+ + 2Cl- + BaSO4
When a solution of sodium sulphate is added to barium chloride solution, the sodium ions are
replaced by barium ions, due to the formation of BaSO4 precipitate. As a result of precipitation, the
conductance decreases. After completion of precipitation, conductance value increases due to free
SO42- ions.
PROCEDURE
Exactly 40 ml (2 x 20 ml) of barium chloride solution is pipetted out into a clean beaker. The
conductivity cell is dipped into it. The terminals of the conductivity cell are connected to a
conductivity bridge and the conductance of the solution is measured. To this solution, sodium
sulphate solution (2 ml) from a burette is added at each time.
The conductance of the solution after each addition of sodium sulphate is measured. The
conductance goes on decreasing, reaches a minimum and then increases. The values of observed
conductance are plotted against the volume of Na2SO4 added. The point of intersection of the two
lines gives the end point. From the end point, the strength of sodium sulphate can be calculated.
Page 95
CALCULATION
Strength of Na2SO4
Volume of barium chloride solution (V1)
= 40 ml
Strength of barium chloride solution (N1)
= .N
Volume of Na2SO4
(V2)
= ml (titre value from graph)
Strength of e Na2SO4
(N2)
= ?
N2
= 40 x N1
V2
= N
Conductance (mho)
Strength of Na2SO4
= 40 x ----------
Page 96
Volume of Na2SO4 (ml)
RESULT
Strength of given sodium sulphate solution = ..N
Page 97
Short Procedure
AIM
To determine conductometrically the strength of given sodium sulphate solution by titrating
it with a standard solution of .N barium chloride.
PRINCIPLE
The reaction between sodium sulphate and barium chloride may be represented as
2Na+ + SO42-
Ba2+ + 2Cl-
2Na+ + 2Cl- + BaSO4
PROCEDURE
Burette
: Sodium sulphate
Pipette
: 40ml of barium chloride
Cell
: conductivity cell
For each addition of Na2SO4 to BaCl2 solution, the conductance goes on decreasing.
At the end point, the conductance reaches the minimum and on further addition of sodium
sulphate, the conductance increases.
By plotting a graph between conductance and volume of Na2SO4, the end point can be found
out.
Strength of Na2SO4 = Volume of BaCl2 x Strength of BaCl2

Volume of Na2SO4
RESULT
Conductance (mho)
Strength of given sodium sulphate solution = ..N
Page 98
Volume of Na2SO
1. Give two examples for precipitation titration.

(i)
BaCl2 Vs Na2SO4
(ii)
AgNO3 Vs NaCl
2. Write the reaction that occur in this titration.

BaCl2 + Na2SO4 BaSO4 + 2NaCl
3. Explain why the conductance decreases when Na2SO4 is added to BaCl2 initially.
At the beginning of the titration, the conductance is due to the completely ionized
BaCl2 solution. When Na2SO4 is added, the following precipitation reaction occurs.
BaCl2 + Na2SO4 BaSO4 + 2NaCl
4. Give reasons for the increase in the conductance after the end point when Na2SO4 is added.
After the end point, the further addition of Na2SO4 results in the increase in
conductance. This is due to presence of 100% dissociated Na2SO4 solution.
5. Name the precipitate formed in this titration.
Barium sulphate
6. What is the principle involved in fixing the end point?
When the conductance values are plotted against the volume of the burette solution,
two straight lines are obtained. The intersection of these lines will be the end point of the
titration.
Page 99
DETERMINATION OF CaO IN CEMENT
Standard EDTA Vs cement solution

Burette reading
S. No.
Volume of cement
solution (ml)
Initial
(ml)
Final
(ml)
Volume of
Concordant
EDTA (ml)
value (ml)
Indicator
Patton and
Reeders
indicator
CALCULATION
Volume of EDTA
= ..ml
Strength of EDTA
= N
Volume of cement solution
= 20 ml
Strength of cement solution = .

20
Molecular weight of CaO
= 56
Equivalent weight of CaO
= 28
Weight of CaO in 1L
= Normality x Equivalent weight of CaO (28)
=___________g.
Page 100
Expt. No
Date.
DETERMINATION OF CaO IN CEMENT
AIM
Determine the amount of calcium oxide present in the given cement sample. You are
provided with . N EDTA solution.
PRINCIPLE
The general composition of Portland cement is
CaO = 60-66%, SiO3 = 17-25, Al2O3= 3-8%, Fe2O3 =2-6%, MgO = 0.1-5.5%, SO3 = 1-3%, Na2O =
0.5-1.5%.
Thus, calcium oxide is the prime constituent of cement. Excess CaO in cement reduces the
strength of cement. Lesser amount of CaO also reduces the strength of cement and result in the
quick.
PROCEDURE
A known weight of the cement sample is treated with con. HCl and the insoluble residue,
SiO2 is removed by filtration. Iron and aluminium in the filtrate are precipitated as their hydroxides
and filtered. The resulting cement solution containing calcium and magnesium is diluted to 250 ml
using distilled water in a standard flask.
Calcium of the oxide or calcium ion present in the cement solution is determined by titrating
a known volume of the cement solution with standard EDTA . The cement solution is treated with
diethyl amine to maintain the pH at 12.5. 4 N NaOH solution is added to precipitate Mg (II) present
in the cement solution as magnesium hydroxide, so that Mg (II) does not interfere in the
determination of CaO .
The solution is then titrated against standard EDTA solution using Patton and Reeders
indicator. The indicator can be used in the determination of calcium in the presence of magnesium as
the latter is the form of precipitate. The end point is the colour change from wine red to clear blue
without any reddish tinge. Glycerol is added to get a sharp end point.
Page 101
RESULT: Weight of calcium oxide in the given cement solution = ___________ gm.
Short procedure
AIM
Determine the amount of calcium oxide in the given cement sample. You are provided with
standard EDTA solution.
PRINCIPLE
Cement is a mixture of oxides of Ca, Mg, Fe, Al, Si with calcium oxide as major
constituent. The calcium in cement can be estimated by EDTA method or by oxalate method. In the
EDTA method, calcium is determined by titration with EDTA at a pH of 12.5.
PROCEDURE
A Known weight of the cement sample is treated with con,HCl and filtered.
The filtrate is made upto 250 ml standard measuring flask.
20 ml this made up solution is pipetted out into a conical flask.
Magnesium in the cement solution is precipitated as Mg(OH)2 by adding 4N NaOH.
It is titrated with standard EDTA at a pH of 12.5, using Patton and Reeder indicator.
The end point is colour change from wine red to blue.
CALCULATION
Strength of cement solution (CaO) = Volume of EDTA x Strength of EDTA
Volume of cement solution
Amount of CaO
= Strength of cement solution x Eq. Wt. of CaO (28)
RESULT
Weight of calcium oxide in the given cement solution = ___________ gm / litre.
Page 102
Page 103
1. What is cement?
Cement is a lime based building material used to bind together coarse aggregates.
2. What are the constituents of cement?
Oxides of Ca, Mg, Fe, Al, Si are the constituents.
3. How is cement solution prepared?
Accurately weighed amount of cement is warmed with moderately conc. HCl till cement
dissolves. Insoluble silica is filtered off and the filtrate is the cement.
4. What is the role of glycerol?
Glycerol is added to get the sharp end point and also to mask the magnesium ions.
5. Which is the indicator used in the determination of CaO in cement solution?
Patton and Reeders indicator is used. It gives sharp color change in the pH range 12-14.
6. What is the function of diethylamine?
It is added to maintain the pH around 12-14.
7. Why is this titration called rapid EDTA method?
The titration is called rapid EDTA method because, by this method, Ca2+ ions in cement
solution are estimated directly and quickly by using standard EDTA solution without removing the
other metal ions.
8. What are the molecular formula and molecular weight of Patton and Reeders indicator?
Molecular formula = C21 H 14 N2 O7 S
Molecular weight = 438
9. What is the role of NaOH in this titration?
Sodium hydroxide reacts with Mg2+ ions and precipitates it out in the form of Mg(OH)2 from
the cement solution.
10. What is the chemical name of Patton and Reeders indicator?
The chemical name of Patton and Reeders indicator is 2- hydroxy-1-(2-hydroxy-4-sulpholnaphthylazo)-3 naphthoic acid (HHSNNA).
Page 104

Chemistry Manual Sem I & Ii

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CSEITQUESTIONS.BLOGSPOT.IN | CSEITQUESTIONS.BLOGSPOT.

Name of the Experiments

Determination of DO Content of water sample by

Determination of chloride content of water sample by

Determination of strength of given HCl using pH meter

Determination of strength of acids in a mixture using

Estimation of iron content of the water sample using

Determination of molecular weight of polyvinyl alcohol

Conductometric titration of strong acid Vs strong base

Name of the Experiments

Strength of potassium dichromate

Volume of sodium thiosulphate

Strength of sodium thiosulphate

According to the law of volumetric analysis,

Strength of sodium thiosulphate

DETERMINATION OF DO CONTENT OF WATER SAMPLE BY

Mn(OH)2 (White ppt)

MnO(OH)2 (Yellow brown ppt)

(Basic manganic oxide)

Burette reading (ml)

Strength of sodim thiosulphate

Volume of water sample

Strength of water sample

Amount of dissolved oxygen in

= Normality Eq. wt. of O2 1000 mg

TITRATION I: STANDARDISATION OF SODIUM THIOSULPHATE

TITRATION II: ESTIMATION OF DISSOLVED OXYGEN

Mn(OH)2 (White ppt)

MnO(OH)2 (Yellow brown ppt)

(Basic manganic oxide)

Pipette: 20 ml std. potassium dichromate solution

End point : Appearance of light green

Additional solution: 5ml conc.HCl + 5 ml 10% KI

Volume of K2Cr2O7 x strength of K2Cr2O7

Pipette: 100 ml water sample

End point : Disappearance of blue colour

Additional solution: 2 ml manganese sulphate + 2 ml alkali iodide + 2 ml conc. H2SO4

Volume of Na2S2O3 x Strength of Na2S2O3

(iv) conc. H2SO4

Titration I: Standardization of silver nitrate

Burette reading (ml)

Strength of sodium chloride

Volume of silver nitrate

Strength of silver nitrate

According to the law of volumetric analysis,

Strength of silver nitrate

DETERMINATION OF CHLORIDE CONTENT OF WATER SAMPLE BY

End point : Appearance of pale red tinge

Burette reading (ml)

Strength of chloride ion

Volume of silver nitrate

Strength of silver nitrate

According to the law of volumetric analysis,

Strength of chloride ion in the given water sample

Calculation of amount of chloride ion

= Equivalent wt. of chloride ion Strength of chloride ion

TITRATION II : ESTIMATION OF CHLORIDE ION

Indicator : 2 drops of 5% potassium chromate

: 20 ml of given water sample

End point : Appearance of pale red tinge

Equivalent weight of chlorine is 35.5

Indicator : 2 drops of 5% potassium chromate

Pipette: 20 ml of Std. NaCl