Experiment- Date:

Department of Chemistry
Name: Branch:
Registration Number: Duration: 90 min.
Standardization of EDTA
Requirements
Reagents and solutions: Standard hard water (0.01M or 1000ppm), EDTA solution, EBT
indicator, and NH3-NH4Cl buffer solution.
Apparatus: Burette, pipette, conical flask, standard flask and burette stand.
Procedure:
Titration I - Standardization of EDTA
To the given EDTA solution in a 100 mL standard volumetric flask, add distill water up to the
mark to make up the volume of 100 mL. Use this solution as titrant (burette solution).
Subsequently pipette out 20 mL of the standard hard water (0.01M) into a clean 250 mL
conical flask. Add approximate 2mL of ammonia buffer (NH 4OH – NH4Cl) solution to
maintain the pH around 10. Add 1-2 drops of Eriochrome Black – T (EBT) indicator and
titrate the solution against EDTA solution taken in the burette. The end point is change of
color from wine red to steel blue. Repeat the titration for concordant titre values. Let ‘V 1’ be
the volume of EDTA consumed.
Table:

Volume of standard Burette reading (mL) Volume of EDTA

S. No.
hard water (mL) Initial Final (V1, mL)

Concordant titre value

Calculation:

20mL of standard hard water = mL of EDTA

 20 x 1mg of CaCO3 = mL of EDTA
 1mL of EDTA = (20/V1) mg of CaCO3 eqvt.
= mg of CaCO3 eqvt.
Experiment- Date:

Or
Concentration of EDTA:
M1V1 = M2V2
EDTA CaCO3
M1 (Molarity of EDTA) xV1 (volume of EDTA consumed) = M2 (Molarity of CaCO3) x V2 (volume of Std. Hard water)
M1= M2xV2/V1
M1= 0.01 X 20/V1
CaCO3 equivalent
1L of 1M of EDTA = 100 gm equivalent of CaCO3
1L of 0.01 X 20/V1 EDTA = 100X0.01X20/V1 gm= 20/V1 gm equivalent of CaCO3
1ml of 0.01 X 20/V1 EDTA = 20/V1 mg equivalent of CaCO3

Evaluation of result
Sample Experimental Actual Value Percentage of Marks awarded
number value error (EDTA strength)
<5%-(Full)
>5 and <10 (-1)
>10 and <20 (-2)

Problem:
The following is data obtained on analysis of a sample water collected VIT Bhopal tap water. 50
mL of sample of hard water consumed 15 mL of EDTA. The same sample water when titrated
after boiling consumed 10 mL of EDTA. 50 mL of 0.02 M standard CaCO3 consumed 20 mL of
EDTA. Calculate the temporary, permanent and total hardness of the water sample in ppm units.
Experiment- Date:

Department of Chemistry
Name: Branch:
Registration Number: Duration: 90 min.

HARDNESS OF WATER - BY EDTA METHOD DETEMINATION OF

TOTAL HARDNESS
Aim
To determine the total hardness of the given water sample using Standard Hard Water (0.01M)
and EBT as an indicator by complexometric titration (EDTA Method).
Principle:
Hardness of water is due to the presence of calcium and magnesium salts in water. Ehtylene
diamine tetraacetic acid (EDTA) forms complexes with a large number of cations including
Ca2+ and Mg2+ ions depending upon pH of the solution. Hence, it is possible to determine the
total hardness of water using EDTA solution. EDTA in the form of its sodium salt (H 2Y2-) is
more often used in place of EDTA in complexometric titration for estimation of metal ions
because pure EDTA (H4Y) is sparingly soluble in water. EDTA has six binding sites (the four
carboxylate groups and the two amino groups) providing six pairs of electrons. The resulting
metal-ligand complex, in which EDTA forms a cage-like structure around the metal ion, is very
stable at specific pH. All metal-EDTA complexes have a 1:1 stoichiometry. The H 2Y2- form
complexes with metal ions as follows.
M + H2Y2- → MY2- + 2H+ ……… (1)
where, M is Ca2+ and Mg2+ present in water. Reaction (1) can be carried out quantitatively at pH
of 10 using Eriochrome Black T (EBT) indicator. EBT forms a wine-red complex with M 2+ ions
which is relatively less stable than the metal-EDTA complex. On titration EDTA first reacts
with free M2+ ions and then with the metal-EBT indicator complex. The end point of the
reaction is change of colour from wine red to steel blue.
Requirements
Reagents and solutions: Standard hard water (0.01M or 1000ppm), EDTA solution, EBT
indicator, hard water sample and NH3-NH4Cl buffer solution.
Apparatus: Burette, pipette, conical flask, standard flask and burette stand.
Experiment- Date:

Procedure
Titration I - Standardization of EDTA

Makeup the volume of given EDTA solution in the standard volumetric flask to 100 mL and
use this solution as titrant (burette solution). Subsequently pipette out 20 mL of the standard
calcium ion solution (0.01M) into a clean 250 mL conical flask. Add 2-3mL of ammonia
buffer (NH4OH – NH4Cl) solution to maintain the pH around 10. Add three drops of
Eriochrome Black – T (EBT) indicator and titrate the solution against EDTA solution taken in
the burette. The end point is change of color from wine red to steel blue. Repeat the titration
for concordant titre values. Let ‘V1’ be the volume of EDTA consumed.

Titration II - Estimation of total hardness

Pipette out 20 mL of the given sample or tap water into a clean conical flask. Add 2-3mL of
ammonia buffer (NH4OH – NH4Cl) solution and three drops of Eriochrome Black–T (EBT)
indicator. Titrate this mixture against standardized EDTA solution taken in the burette. The
end point is the change of color from wine red to steel blue. Repeat the titration for concordant
titre value. Let ‘V2’ be the volume of EDTA consumed.
OBSERVATION AND CALCULATION
Titration I - Standardization of EDTA
Burette: EDTA solution
Conical Flask: 20 mL of Standard hard water (SHW) + 2-3 mL buffer solution + 2 drops of
EBT
End point: wine-red to steel blue.

Volume of standard Burette reading (mL) Volume of EDTA

S. No.
hard water (mL) Initial Final (V1, mL)

Concordant titre value

20mL of standard hard water = mL of EDTA

 20 x 1mg of CaCO3 = mL of EDTA
 1mL of EDTA = (20/V1) mg of CaCO3 eqvt.
= mg of CaCO3 eqvt.
Titration II - Estimation of total hardness
Experiment- Date:

Burette: standardized EDTA solution

Conical Flask: 20 mL of HW + one test tube buffer solution + 2 drops of EBT

S. No. Volume of Standard Burette reading (mL) Volume of EDTA

hard water (mL) Initial Final (V2, mL)

Concordant titre value

20mL of given hard water = mL of EDTA

= V2 X 20/V1 mg of CaCO3 eqvt.
V2 X 20 X 1000
1000mL of given hard = mg of CaCO3 eqvt
V1 X 20
V2 X 1000
Total Hardness = mg / L
V1
Result:

The total hardness is present in the given sample hard water: ppm
Evaluation of result
Sample Experimental Actual Value Percentage of Marks awarded
number value error (EDTA strength)

Space for Calculations

Experiment- Date:

Department of Chemistry
Name: Branch:
Registration Number: Duration: 90 min.
ESTIMATION OF TYPES OF ALKALINITY IN WASTE WATER
SAMPLE
Aim

To determine the extent and type of alkalinity present in the given water sample.

Principle:

Alkalinity in water is due to the presence of OH -, CO32- and HCO3- ions. The alkalinity of a

given sample of water can be obtained by neutralizing the above mentioned ions with standard

HCl. Titrating the given sample of water to a pH of 8.3 or till the pink color which appears on

addition of Phenolphthalein indicator) disappears which will indicate the complete

neutralization of OH- ions and half of CO32- ions (CO32- will get converted to HCO 3-). Titrating

the same sample of water at a pH of 4.4 or till a sharp color change from yellow to orange of

methyl orange indicator will indicate the total alkalinity i.e. the amount of OH -, CO32- and

HCO3- present in the given sample

OH- and HCO3- ions cannot exist in water together because they combine instantaneously to

form CO32- ions.

It is for this reason, the three ions OH-, CO32- and HCO3- cannot exist together.
Experiment- Date:

Requirements

Reagents and solutions:

Hydrochloric acid (0.1N), water sample, methyl orange and phenolphthalein indicator
solutions.
Apparatus: Burette, pipette, conical flask, standard flask and burette stand
Procedure
Titration I: Estimation of Alkalinity
To the given water sample in a 100 mL standard volumetric flask, add distill water up to the
mark to make up the volume of 100 mL. Pipette out 20 mL of the given water sample into a
clean 250 mL conical flask. To this add 2 drops of phenolphthalein indicator and titrate the
solution against HCl taken in the burette. The end point is disappearance of pink colour. The
corresponding burette reading is noted and it is denoted as phenolphthalein end point [P].
To the same solution, add two drops of methyl orange indicator and continue the titration. The
end point is color change from pale yellow to orange. This end point indicates complete
neutralization of alkalinity present in water sample and is known as methyl orange end point
[T]. Repeat the titration for concordant titre values.
OBSERVATION AND CALCULATION
Titration : Estimation of Alkalinity
Concordant
Burette reading (mL)
value (mL)
Volume
Final
of Water
S. No.
Sample
Initial At At [P] [T]
(mL)
phenolphthalein methyl orange
end point [P] end point [T]
1

Concordant titre value

Phenolphthalein alkalinity (mg/L) as CaCO3

[P] mL of HCl X Normality of HCl X 50 X 1000

= -------------------------------------------------------------------
Volume of water sample taken

= _________________ ppm [P]

Experiment- Date:

Methyl orange alkalinity (mg/L) as CaCO3 (Total alkalinity)

[T] mL of HCl X Normality of HCl X 50 X 1000

= -----------------------------------------------------------------
Volume of water sample taken

= __________________ ppm [T]

ALKALINITY TABLE:

Volume of p Alkalinity due to

and m (mL) OH- CO32- HCO3-

[p] = 0 0 0 [M]

[p] = [m] [M] 0 0

[p] = ½ [m] 0 2[P] 0

[p] > ½[m] 2[P] - [M] 2[M] - 2[P] 0

[p] < ½[m] 0 2[P] [M] – 2[P]

Result
The given water sample contains _________ and _______________ ions.

Amount of ___________________ alkalinity = __________________ ppm

Amount of ___________________ alkalinity = __________________ ppm

Total alkalinity or methyl orange alkalinity of the water sample = __________ppm

Evaluation of result

Sample Experimental Actual Value Percentage of Marks awarded

number value error

Space for Calculations

Experiment- Date:

Department of Chemistry
Name: Branch:
Registration Number: Duration: 90 min.
ESTIMATION OF COPPER IN AN ALLOY BY IODOMETRY
Aim: To estimate the amount of copper present in the given solution.
Principle:
The experiment is based on the reaction between iodine and sodium thiosulphate. Copper
sulphate liberate equal amount of iodine from KI solution in a weakly acidic medium as
follows.
CuSO4 + 2KI CuI2 + K2SO4

2CuI2 Cu2I2 + I2
The liberated iodine is titrated against sodium thiosulphate using starch indicator until the blue
colour disappears.

Requirements
Reagents and solutions:
standard solution of 0.01 N copper sulphate, ammonium hydroxide, KI, dilute acetic acid,
starch and an approximately 0.01N sodium thiosulphate.
Apparatus
Burette, pipette, conical flask, standard flask and burette stand
Procedure:
Titration I: Standardisation of Sodium thiosulphate
Pipette out 20ml of standard copper sulphate solution into a clean conical flask. Add
ammonium hydroxide drop by drop till a pale blue precipitate is formed. Dissolve the
precipitate by adding a slight excess of dil. acetic acid. Then add 10ml of 10% KI solution and
titrate the liberated iodine against sodium thiosulphate solution taken in the burette. When the
solution turns straw yellow, add 1ml of freshly prepared starch as indicator and continue the
titration. The end point is the disappearance of blue colour and appearance of dirty white
solution. Repeat the titration for concordant value. Calculate the normality of sodium
thiosulphate by using the normality of copper.
Experiment- Date:

Titration II: Estimation of Copper

To the given alloy sample in a 100 mL standard volumetric flask, add distill water up to the
mark to make up the volume of 100 mL. Pipette out 20ml of this solution into a clean conical
flask. Add ammonium hydroxide drop by drop till a pale blue precipitate is formed. Dissolve
the precipitate by adding a slight excess of acetic acid. Then add 10ml of 10% of KI solution
and titrate the liberated iodine against standardised sodium thiosulphate solution taken in the
burette. When the solution becomes straw yellow, add 1ml of freshly prepared starch as
indicator and continue the titration. The end point is the disappearance of blue colour and
appearance of dirty white solution. Repeat the titration for concordant value. Calculate the
normality of copper solution by using the normality of sodium thiosulphate and estimate the
amount of copper present in the whole of the given solution.
OBSERVATION AND CALCULATIONS

Titration I: Standardisation of sodium thiosulphate

Volume of Std CuSO4 Burette reading (ml) Volume of

S. No. (ml) Initial Final Sodium Thio
Sulphate
(ml)

Calculation :

Volume of Std CuSO4 =

Normality of Std CuSO4 =

Volume of Sodium Thio Sulphate =

Normality of Sodium Thio Sulphate = ------------------N.

Experiment- Date:

Titration II : Estimation of Copper

Volume of Unknown Burette reading (ml) Volume of Sodium
S. No. CuSO4 Initial Final Thio sulphate(ml)
(ml)

Calculation :

Volume of Sodium Thio Sulphate =

Normality of Sodium Thio Sulphate =

Volume of Unknown CuSO4 =

Normality of Unknown CuSO4 = ----------------------N

The amount of copper present in the whole of given solution = (Normality x Eq.Wt)/10

= ---------------------g.

Result:

The amount of copper present in the whole of the given solution = g.

Evaluation of result

Sample Experimental Actual Value Percentage of Marks awarded

number value error

Space for Calculations

Experiment- Date:

Department of Chemistry
Name: Branch:
Registration Number: Duration: 90 min.
ESTIMATION OF FERROUS ION BY CERIMETRY

Aim: To estimate the amount of ferrous ion present in the whole of the given solution
Principle:
Ceric ions oxidise ferrous ions in acid medium according to the equation,
Ce+4 + Fe+ 2 →Ce 3+ + Fe+3
The ceric ammonium sulphate solution of approximately known strength is standardized
against standard FAS.
For the above titrations, redox indicator ferroin can be used. Ferroin is a complex formed
between Fe(II) ion and 1,10-phenanthroline, [Fe(Phen)3]+2. The reduced form of indicator has
an intense red colour, whereas oxidised iron (III) complex has a blue colour. The indicator
reaction may be written as,
[ Fe (Phen )3 ]3+ +c [ Fe (Phen )3 ]+2
Pale blue Red
When iron (II) is titrated with Ce (IV) in sulphuric acid medium, the ferroin indicator is
initially red in colour in its reduced form. At the end point, Ce (IV) oxidises it to Fe (III)
complex. The end point, is a sharp change from red to pale blue colour.
Requirements
Reagents and solutions:
A standard solution of 0.01N ferrous ammonium sulphate, sulphuric acid, Ferroin
indicator and an approximately 0.01N solution of Ceric ammonium sulphate.
Apparatus
Burette, pipette, conical flask, standard flask and burette stand
Procedure
Titration I: Standardisation of Cerium (IV) sulphate solution:
Pipette out 20ml of Ferrous ammonium sulphate solution in to a clean conical flask. Add about
20ml of 2N sulphuric acid followed by 2 drops of ferroin indicator. Titrate it against Cerium
(IV) solution taken in the burette. The end point is colour change from red to pale blue colour.
Repeat the titration to get concordant value. From the titre value, calculate the strength of
cerium (IV) solution.
Titration II: Estimation of Ferrous ion
Experiment- Date:

Make up the given ferrous ion solution to 100ml in a standard flask. Pipette out 20ml of this
solution in to a clean conical flask. Add about 20ml of 2N sulphuric acid solution and 2 drops
of ferroin indicator. Titrate it against standardised cerium (IV) solution taken in the burette.
End point is colour change from red to pale blue colour. Repeat the titration to get concordant
value. From the titre value, calculate the strength of ferrous ion and hence calculate the
amount of ferrous ion present in the given solution.

OBSERVATION AND CALCULATIONS

Titration I: Standardisation of Cerium (IV) sulphate solution:

Volume of Std FeSO4 Burette reading (ml) Volume of CAS

S. No. (ml) Initial Final (ml)

Calculation :

Volume of FeSO4 =
Normality of FeSO4 =
Volume of CAS =
Normality of CAS =--------------------N.
Titration II: Estimation of Ferrous ion

Volume of FeSO4 Burette reading (ml) Volume of

S. No. (ml) Initial Final CAS(ml)
Experiment- Date:

Calculation

Volume of CAS =

Normality of CAS =

Volume of FeSO4 =

Normality of FeSO4 = --------------------N.

The amount of Ferrous present in the whole of given solution =(Normality x Eq.Wt)/10

=----------------------g.

Result:

The amount of ferrous ion present in the whole of the given solution = ___________g.

Evaluation of result

Sample Experimental Actual Value Percentage of Marks awarded

number value error

Space for Calculations

Experiment- Date:

Department of Chemistry
Name: Branch:
Registration Number: Duration: 90 min.
DISSOLVED OXYGEN (DO) ANALYSIS IN WATER

Aim: To estimate the amount of dissolved oxygen in the given water sample

Principle:

Dissolved oxygen is an important factor in corrosion. Oxygen is poorly soluble in water. The

solubility of oxygen decreases with increase in concentration of the salt under a pressure of one

atmosphere, the solubility is less in saline water. The estimation of dissolved oxygen in water

is useful in studying corrosion effect of boiler feed water and in studying water pollution.

Dissolved oxygen is usually determined by Winkler’s method. It is based on the fact that

dissolved oxygen oxidized potassium iodide (KI) to iodine. The liberated iodine is titrated

against standard sodium thiosulphate solution using starch indicator. Since dissolved oxygen in

water is in molecular state. It as such cannot oxidize KI. Hence Manganese Hydroxide is used

as an oxygen carrier to bring about the reaction between KI and Oxygen. Manganese

hydroxide, in turn, is obtained by the action of NaOH on MnSO4.

The liberated iodine (I2) is titrated against standard sodium thiosulphate (Na 2S2O3) solution

using starch as indicator.

Experiment- Date:

Requirements

Reagents and solutions:

Sodium thiosulphate solution (0.01 M), Alkali Iodide solution: (KI + NaOH in water), conc.

H2SO4, Manganese Sulphate, starch solution as indicator

Apparatus

Burette, pipette, conical flask, standard flask and burette stand

PROCEDURE:

Titration : Estimation of dissolved oxygen

100 mL of tap water sample is taken in a conical flask, 2 mL of manganese sulphate and 2mL
of alkali iodide solution are added and shaken well for the through mixing of the reagents. The
flask is left aside for few minutes to allow the precipitate to settle down and then 10mL of
Sulphuric acid is added for the complete dissolution of the precipitate. Then it is further titrated
against standard sodium thiosulphate solution. When the solution becomes light yellow, starch
indicator is added. The end point is disappearance of bluish brown colour. The titration is
repeated twice or thrice to get the concordant value. From the titre value the strength of
dissolved oxygen is calculated and hence the amount of dissolved oxygen in the water sample
is calculated.

OBSERVATION AND CALCULATIONS

Table : Estimation of dissolved oxygen

Burette reading (mL) Volume of sodium

Volume of water sample
S. No. thiosulphate
Initial Final
(V1 / mL)
(V2 / mL)
1

Concordant value
Experiment- Date:

Calculations :

Volume of sodium thiosulphate V2 = …………………. mL

Strength of sodium thiosulphate N2 = 0.01 M

Volume of water sample taken V1= 100 mL

Strength of given water sample N1 = ?

V1N1=V2N2

V2N2
N 1=
V1

V 2 X 0.01
N 1=
100

Amount of dissolved oxygen (ppm) = normality × equivalent weight of O2×1000mg/L

of the given water sample.

= ……………….N × 8 × 1000mg/L

= ------------------ ppm.

RESULT :

Amount of dissolved oxygen in the given water sample = ………………… ppm.

Evaluation of result

Sample Experimental value Actual Percentage of Marks awarded

number Value error

Space for calculations

Experiment- Date:

Department of Chemistry
Name: Branch:
Registration Number: Duration: 90 min.
ESTIMATION OF SULPHATE IN EFFLUENT BY TDS-CONDUCTIVITY METHOD
Principle
Electrolyte solutions conduct electricity due to the presence of ions in solution. In case of
precipitation titration between BaCl2 and Na2SO4, the conductance decreases slowly due to the
replacement of Na ion by SO42- upto the equivalence point. After the equivalence point the
conductance increases rapidly due to the excess addition of BaCl 2 which remains in solution as
Ba2+ and Cl-. This makes detection of neutralization point easy from the conductance trend
plotted as a graph. This is the principle is used in the estimation of SO 42- from an effluent
sample.
Apparatus required
TDS-Conductivity bridge, conductivity cell, burette, pipette, volumetric flasks, glass rod and
100 mL beaker.
Chemicals required
BaCl2, Unknown sulphate solution, 0.01 N KCl and distilled water.
Procedure
Calibration of TDS-Conductivity meter:
Place a freshly prepared 0.01 N KCl solution (given in bottle) in a 100 mL beaker and dip the
conductivity cell in this solution and connect to the TDS-Conductivity meter. Press “CAL”
button and complete the internal calibration of the instrument.
Estimation of unknown sulphate in the given solution:
Take 40 mL of given sulphate solution in a 100 mL beaker. The conductivity cell is dipped into
the beaker and connected to TDS conductivity meter. Fill the burette with BaCl 2 solution (0.04
N). Record the conductivity of the sulphate solution as 0 th reading. Add 1 mL portion of known
concentration of BaCl2 into the beaker, stir with glass rod, wait for a stable reading and note
down the conductance. Continue the addition of BaCl 2 (1 mL each time) and note the
conductance after each addition. Continue the titration beyond the equivalence point for about
3mL. The conductance will decrease till complete precipitation of BaSO 4 and then starts
increasing on continuing the addition of BaCl2. A graph is now drawn by plotting conductance
Vs volume of BaCl2 added and the intersection point from the graph gives the volume of BaCl2
Experiment- Date:

OBSERVATION
Table. 2 Estimation of unknown sulphate solution
Sl No Volume of Conductance Remark
BaCl2 in mL
0
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
Experiment- Date:

9.0

8.5

8.0
Conductance (mhos)

7.5

7.0

6.5

6.0

5.5 V2 mL

5.0
0 2 4 6 8 10 12 14
BaCl2 added (mL)

Figure: Model graph for TDS-Conductometric estimation of unknown sulphate sample

solution
Calculations:
Estimation of unknown sulphate:
From the second plot,
20 mL of unknown sulphate consumed V2 mL of BaCl2 for complete precipitation of sulphate.
Volume of BaCl2 V2 = …………………. mL
Strength of BaCl2 N2 = 0.04 M
Volume of sulphate solution taken V1= 40 mL
Strength of given water sample N1 = ?
V1N1=V2N2
V2N2
N 1=
V1
V 2 X 0.04 V 2
N 1= =
40 1000
Amount of sulphate (ppm) = normality × equivalent weight of SO42-×1000mg/L

V2 mg
= X 96 X 1000 =V 2 X 96 PPM =PPM
1000 l
Result
Amount of sulphate present in the given sample = ……………….ppm.
Evaluation of result
Sample Experimental value Actual Percentage of Marks awarded
number Value error

Space for Calculation:

Experiment- Date:

Department of Chemistry
Name: Branch:
Registration Number: Duration: 90 min.

ESTIMATION of Fe(II) IN STEEL BY REDOX POTENTIOMETRY

Principle:
Potassium permanganate oxidizes ferrous ion (Fe 2+) to ferric ion (Fe3+) in the presence of acid
as per the reaction:
5Fe+2 → 5Fe+3 + 5e
MnO4- + 8H+ + 5e → Mn2+ + 4H2O
5Fe + MnO4- + 8H+ → 5Fe+3 + Mn2+ + 4H2O
+2

The electrode potential (oxidation potential) in the titration depends upon the concentration of
Fe2+, Fe3+ and hydrogen ions.
To avoid the effect of the change in the hydrogen ion concentration, the titration is usually
carried out in large excess of an acid.
The oxidation potential of this redox system is given by
RT Fe 3+
E=E0 + ln ( 2 + )
nF Fe
Connecting the redox electrode (Pt) with a saturated calomel electrode (SCE) completes the
necessary cell as indicated below:

HgHg2Cl2 (s), Saturated KCl  Fe3+, Fe2+Pt

(SCE)
When potassium permanganate is added Fe2+ is oxidized to Fe3+ whose concentration increases
with progressive addition of potassium permanganate. The observed EMF gradually increases.
At the end point, there will be a sharp increase due to sudden removal of all Fe 2+ ions. Plot
between EMF measured (E) Vs. Volume of potassium permanganate added and another plot
between  E / V vs. Average volume of potassium permanganate are made. The end
point of the titration is measured graphically.
Requirements

Reagents and solutions: KMnO4 solution, Steel solution, 2.0 N H2SO4.

Apparatus: Platinum electrode, Calomel electrode, Potentiometer, Volumetric flasks, Burette,

Pipette, Beakers.
Experiment- Date:

Procedure:
Calibration of Potentiometer: Switch on the potentiometer and connect the standard Weston-
Cadmium cell terminals to either channel A (move channel switch to position A) or channel B
(move the channel switch to position B). Place the electrodes into D.I. water and adjust the
standardization knob to set the value 0.00 V by using “SET ZERO” knob.
Estimation of Fe(II) in steel:
Transfer the given unknown steel [containing Fe(II)] solution into a clean 250 mL beaker. Add
20 mL dilute sulphuric acid (2.0 N) with the help of measuring cylinder. Put a small magnetic
stir bar into this mixture. Place the electrodes in the beaker and ensure that stir bar not touching
the electrode tip during stirring. Stir the solution at a slow rate (RPM) by using “STIRRER”
knob. Measure the potential at 0 mL addition of KMnO 4 solution. Then, add 1 mL aliquot of
KMnO4 solution each time from a burette to the beaker containing steel sample solution. Stir
the solution carefully and measure the EMF for each mL addition of KMnO 4 solution till the
potential shows a tendency to increase rapidly. After the abrupt change in cell EMF is
observed, continue the titration to take 5 more readings by adding 1 mL burette solution every
time. Plot a graph between ΔE/ΔV vs. average volume of KMnO4 added. Calculate the amount
of KMnO4 required (V2) for this titration from the peak point. Calculate the percentage of
Fe(II) in the given solution by calculations shown.
OBSERVATION AND CALCULATIONS

(a) Plot of EMF vs volume of KMnO4 (b) Plot of plotting ΔE/ΔV versus average

added (mL) volume of KMnO4

Experiment- Date:

Sl. Vol. of
E E/V Average
No KMnO4 EMF (Volt) V (mL)
(Volt) (Volt/mL) Volume (mL)
. ( mL)
1 0 0.5
2 1 1.5
3 2 2.5
4 3 3.5
5 4 4.5
6 5 5.5
7 6 6.5
8 7 7.5
9 8 8.5
10 9 9.5
11 10 10.5
12 11 11.5
13 12 1 ml 12.5
14 13 13.5
15 14 14.5
16 15 15.5
17 16 16.5
18 17 17.5
19 18 18.5
20 19 19.5
21 20 20.5
22 21 21.5
23 22 22.5
24 23 23.5
25 24 24.5
Experiment- Date:

Calculations:

By stoichiometry, 5 moles of Fe(II) will need 1 mole of KMnO4 for complete oxidation.
Hence,
V1 N1 =5 x V2 N2,

Where, V1= Volume of Steel solution= 100 mL

N1= Strength of Iron solution
V2= Volume of KMnO4 (From graph 2)
N2= Strength of KMnO4= 0.05 M
5 XV 2 N 2
N 1=
V1

5 X V 2 X 0.05
N 1=
100

Amount of Fe(II) present in ppm = normality × equivalent weight of Fe ×1000mg/L

5 X V 2 X 0.05 X 55.85 X 1000 mg

¿
100 L

¿ 139.625 X V 2 ppm

Result
Amount of Fe (II) in the steel solution = …………………………

Evaluation of result
Sample Experimental value Actual Percentage of Marks awarded
number Value error

Space for calculations

Experiment- Date:

Department of Chemistry
Name: Branch:
Registration Number: Duration: 90 min.

COLORIMETRIC ESTIMATION OF COPPER IN BRASS

Principle: Generally, colorimeter works on Beer-Lambert law (or Beer's law) which states the
linear relationship between absorbance and concentration of an absorbing species. The general
Beer-Lambert law is usually written as:
A=Ct
Where, A is the measured absorbance,  is a wavelength-dependent absorptivity coefficient, t is
the path length, and C is the analyte concentration. When working in unit path length, the Beer-
Lambert law is written as:
A = C or A α C
So absorbance of a particular analyte depends on its concentration. After drawing calibration
graph the determination of copper concentration in brass sample can be done by colorimetry
applying Beer-Lambert law.
Solutions required
1. Known Brass Solution –10 mg/mL of Cu(II)
2. Unknown Brass solution

Procedure:
Calibration of Colorimeter: In a clean cuvette, take D.I. water up to the mark. Wipe outside
of the cuvette by using filter paper. Insert the cuvette in the sample holder of colorimeter.
Change the filter to 700 nm. Then press the “calibration” knob to set the value 0.00
Preparation of solution
Prepare test solutions as per following.
Solution 1 (2 mg/mL): Add 8 ml of D.I. water to 2 ml of known brass solution and shake well.
Take this solution in the cuvette till the mark, measure its absorbance.
Solution 2 (4 mg/mL): Add 6 ml of D.I. water to 4 ml of known brass solution and shake well.
Take this solution in the cuvette till the mark, measure its absorbance.
Solution 3 (6 mg/mL): Add 4 ml of D.I. water to 6 ml of known brass solution and shake well.
Take this solution in the cuvette till the mark, measure its absorbance.
Experiment- Date:

Solution 4 (8 mg/mL): Add 2 ml of D.I. water to 8 ml of known brass solution and shake well.
Take this solution in the cuvette till the mark, measure its absorbance.
Unknown Solution: Take this solution in the cuvette till the mark, measure its absorbance.
Draw a calibration graph taking concentration of Copper (II) as X-axis and absorbance
readings as Y-axis and a straight line that passes through the origin is obtained as shown in
Figure From the calibration plot, measure the concentration of copper (II) in the unknown
sample from its absorbance value by putting into the calibration curve.

Figure: Model calibration curve for Cu(II) estimation

Table-1: Experimental Data
S. No Concentration (mg/mL) Absorbance
1. 2
2. 4
3. 6
4. 8
5. Unknown Ni(II)

Result
Concentration of Nickel in the steel sample = ………………….. mg/mL
Evaluation of result

Sample Experimental value Actual Percentage of Marks awarded

number Value error

Space for Calculations