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LIST OF EXPERIMENTS V+ TEAM
1. CONDUCTOMETRIC TITRATION OF STRONG ACID AND STRONG
BASE HCl vs NaOH
AIM
To determine the amount of strong acid (HCl) present in the given solution by
conductometric titration using standard NaOH of 0.1N.
PRINCIPLE
Solution of electrolytes conducts electricity due to the presence of ions. Since specific
conductance of a solution is proportional to the concentration of ions in it, conductance of the
solution is measured during titration.
When NaOH is added slowly from the burette to the solution HCl (strong
acid) gets neutralized first. Since the fast moving H+ ions are replaced by slow moving Na+
ions, decrease in conductance takes place until the end point is reached.
HCl + NaOH NaCl + H2O
When the end point is reached, addition of NaOH will cause sudden increase in the
conductance. This is due to the presence of fast moving OH ions.
MATERIALS REQUIRED
1) Conductivity bride 2) conductivity cell 3) Beaker 4) Standard NaOH 5) HCl
6) Burette, pipette, glass rod etc.,
PROCEDURE:
The burette is filled with NaOH solution up to the zero level. 50 ml of the given make
up HCl solution is pipetted out into a clean 100 ml beaker. The conductivity cell is placed in it.
The two terminals of the cell are connected with a conductivity bridge.
Now 1 ml of NaOH from the burette is added to the solution taken in the beaker,
stirred, and then conductivity is measured. This is continued up to the end point. (The
conductivity is going on decreasing up to the end point) After the end point, again NaOH is
gradually added and few more readings are noted.
Expt.No: Date:
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.
Table
HCl vs NaOH
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Volume of NaOH added (ml) Conductance (mho)
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Calculation
Step: I Calculation of Normality of HCl
Volume of HCl V1 = 50 ml
Strength of the HCl N1 = ……N.
Volume of the NaOH V2 = ----------ml (From Graph)
Strength of the NaOH N2 = -----------N
According to the law of volumetric analysis
V1N1 = V2N2
V2N2
N = -----------
V1
………....ml x……..…...N
= -------------------------------------
50
Strength of HCl = ……………..…N
CO
ND
UC
TA
NC
E
VOLUME OF NaOH
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Step : II
Calculation of amount of HCl:
The amount of HCl present in
one Litre of the given solution = ---------N x Eq.wt.of HCl (36.45)
= ……………..gms
RESULT
The amount of HCl present in 1 litre of the given solution =. …………gms.
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2. CONDUCTOMETRIC TITRATION OF MIXTURE OF ACIDS (HCl
& CH3COOH) AGAINST NaOH
AIM:
To determine the amount of a strong acid and a weak acid (HCl and CH3COOH)
present in one litre of the given mixture of acid solution by conductometric titration using
standard NaOH of ………N.
PRINCIPLE:
Solution of electrolytes conducts electricity due to the presence of ions. Since specific
conductance of a solution is proportional to the concentration of ions in it, conductance of
the solution is measured during titration.
When the sodium hydroxide is added slowly from the burette to the solution, HCL
(strong acid) gets neutralised first. Since the fast moving H+ ions are replaced by slow
moving Na+ ions decrease in conductance take place until the end point is reached
HCl + NaOH NaCl + H2O (Ist neutralisation)
After the complete neutralisation of all HCl, the neutralisation of CH3COOH starts,
CH3COOH + NaOH CH3COONa + H2O ( 2nd neutralisation)
Since CH3COONa is stronger than CH3COOH conductivity slowly increases until all
CH3COOH is completely neutralised. When the end point is reached, addition of NaOH
will cause sudden increase in the conductance. This is due to the presence of fast moving
OH – ions.
MATERIALS REQUIRED:
1) Conductivity bridge 2) Conductivity cell 3) Beaker 4) Standard M/10 NaOH 5)
Approximately N/10 HCl & CH3COOH 6) Burette, pipette, glass rod etc.,
PROCEDURE:
The burette is filled with NaOH solution upto the zero level. 20 ml of the given mixture
of acids (HCl + CH3COOH) is pipetted out into a clean 100 ml beaker. The conductivity cell is
Expt.No: Date:
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LIST OF EXPERIMENTS V+ TEAM
placed in it and then diluted to 50 ml by adding conductivity water, so that the electrodes are
well immersed in the solution. The two terminals of the cell are connected with a conductivity
bridge.
Now 1ml of NaOH from the burette is added to the solution, taken in the beaker stirred
for some time and then conductivity is measured. (The conductivity is going on decreasing
upto the end point) This process is repeated until atleast five readings are taken after the end
point (a) has been reached.
After the end point, again NaOH is gradually added, which causes increase in
conductance. The increase in conductance is observed until the end point (b) is reached.
After the second end point, sudden increase in conductance is observed on further
addition of NaOH. The reading (conductivity) is continuously measured for each addition of
NaOH and are tabulated. Now the graph is plotted between the volumes of NaOH versus
conductivity. From the graph the first end point (a) and the second end point (b) is noted. From
the end points the amount of HCl and CH3COOH present in 1 litre of the mixture of solution is
calculated.
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Table
Volume of mixture (HCl + CH3COOH) Vs NaOH
Volume of NaOH
added (ml)
Conductance (mho)
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Calculation
StepI: Calculation of normality of HCl
Volume of the mixture (HCl) V1 = 20ml
Strength of the mixture (HCl) N1 = ………N
Volume of the NaOH V2 = …….. ml (Ist titre value)
Strength of the NaOH N2 = ……… N
According to the law of volumetric analysis
V1N1 = V2N2
V2N2
N1 = _____
V1
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…..ml x ….N
= _________
20
Strength of HCl = ……..N
Step II: Calculation of amount of HCl :
The amount of HCl Present in
1000 ml of the given solution = Normality of HCl x Eq, wt Hcl
= ……..gms
Step III : Calculation of normality of CH3COOH
Volume of the mixture (CH3COOH) V1 = 20 ml
Strength of the mixture (CH3COOH) N1 = …….N
Volume of the NaOH V2 = ………ml (2nd titre value)
Normality of NaOH V2 = 0.1 N
According to the law of volumetric analysis
V1N1 = V2N2
V2N2
N1 = ____
V1
…….ml x…N
= __________
20
Normality of CH3COOH = ……..N
Step IV : Calculation of amount of CH3COOH
The amount of CH3COOH Present in = Normality of CH3COOH x eq.wt.CH3COOH
1000 ml of the given solution
= ……gms
RESULT: i) The amount of HCL present in 1 litre of the given solution ………gms
ii) The amount of CH3COOH present in 1 litre of the given solutions
……….….gms
3. CONDUCTOMETRIC PRECIPITATION TITRATION USING BaCl2
AGAINST Na2SO4
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AIM :
To determine the amount of BaCl2 present in one litre of the given solution by
conductometric titration using standard Na2SO4 of ……….N
PRINCIPLE:
Solution of electrolytes conducts electricity due to the presence of ions since specific
conductance of a solution is proportional to the concentration of ions in it, conductance of the
solution is measured during titration.
In the precipitation titration, the ions are converted to insoluble precipitate, which will
not contribute in the conductance.
When Na2SO4 is added slowly from the burette to the solution of BaCl2, BaSO4 gets
precipitated while the chloride ions remain unchanged.
[Ba2+ + 2Cl]+[2Na+ + SO24] BaSO4 + 2Na+ + 2Cl-
The Ba2+ ions in the solution are replaced by free Na+ ions. Since the mobility of Na+
ions is less that of Ba2+ ions the conductance of the solution decreases.
After the end point, when all the Ba2+ ions are replaced, further addition of Na2SO4
increases the conductance. This is due to the increase of Na+ and SO24 ions in the solution.
MATERIALS REQUIRED
1) Conductivity bride 2) conductivity cell 3) Beaker 4) Standard N/10Na2SO4 5)
Approximately N/10BaCl2 solution 6) Burette, pipette, glass rod etc.,
PROCEDURE:
The burette is filled with Na2SO4 solution upto the zero level. 20 ml of the given BaCl2
solution is pipetted out into a clean 100 ml beaker. The conductivity cell is placed in it and then
diluted to 50 ml by adding conductivity water. The two terminals of the cell are connected with
a conductivity bridge.
Now 1 ml of Na2SO4 from the burette is added to the solution taken in the beaker,
stirred, and then conductivity is measured. This is continued upto the end point. (The
conductivity is going on decreasing upto the end point) After the end point, again Na2SO4 is
gradually added and few more reading are noted.
Thus the conductivity is continuously measured for each addition of Na2SO4 and are
tabulated. Now the graph is plotted between the volume of Na2SO4 and conductivity. From the
graph end point is noted and hence amount of BaCl2 present in 1 litre is calculated.
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Table
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BaCl2 Vs Na2SO4
Volume of
Na2SO4 added
(ml)
Conductance
(mho)
Calculation
Step: I Calculation of normality of BaCl2
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Volume of BaCl2 mixture (HCL) V1 = 20 ml
Strength of the BaCl2 solution N1 = ……N.
Volume of the Na2SO4 V2 = --------ml (titre value)
Strength of the Na2SO4 N2 = --------N
According to the law of volumetric analysis
V1N1 = V2N2
V2N2
N1 = _____
V1
….ml x….N
= ___________
20
Strength of BaCl2 = ……N
Step : II Calculation of amount of BaCl2:
The amount of BaCl2 present in
Litre of the given solution = ------- x Eq.wt.of BaCl2 (122.14)
= ………..gms
RESULT:
The amount of BaCl2 present in 1 litre of the given solution = …..……gms.
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4. ESTIMATION OF FERROUS IRON BY
POTENTIOMETRIC TITRATION
AIM:
To estimate the amount of ferrous iron present in whole of the given solution by
potentiometric method. A standard solution of potassium dichromate of strength ……..N is
provided.
PRINCIPLE:
Potentiometric titrations depend on measurement of emf between reference electrode
and an indicator electrode. When a solution of ferrous iron is titrated with a solution of
potassium dichromate, the following redox reaction takes place.
6Fe24 + Cr2O7 2 + 14H 6Fe3+ + 7H2O
During this titration Fe2+, whose concentration increases, at the end point, there will be
a sharp change due to sudden removal of all Fe2+ ions.
Connecting this redox electrode with a calomel electrode as shown below sets up the
cell:
Hg,HgCl2(s) KCl // Fe2+, Fe3+, Pt
A graph between emf measured against the volume of K2Cr2O7 added is drawn and the
end point is noted from the graph.
MATERIALS REQUIRED: (i)Potentiometer (ii) pt electrode (iii) saturated calomel electrode (iv) standard K2Cr2O7
solution (v) given ferrous iron solution.
PROCEDURE:
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The given ferrous iron solution is made upto 100 ml in a standard flask. 20 ml of this
made up solution is pipetted out into a clean 100 ml beaker. About 10 ml of dil H2SO4 and 20
ml of distilled water are added in it. A platinum electrode is dipped into the solution. This
electrode is then coupled with a saturated calomel electrode and the cell is introduced into
potentiometric circuit. The std K2Cr2O7 solution is taken in the burette and added.
Titration – I First adding std. K2Cr2O7 solution in portions of 1 ml and the emf carries out a
Preliminary titration. of the cell is measured after each addition. The addition of K2Cr2O7 is
continued even after the end point and the range at which end point lies is found out by plotting
volume of K2Cr2O7 added emf (graph I).
Titration –II
Another titration is carried out by adding std. K2Cr2O7 solution in portions of 0.1 ml
near the end point and the emf of the cell is measured after each addition. The addition of
K2Cr2O7 is continued even after the end point for further 1 ml. The accurate end point is
determined by plotting E / V Vs Volume of K2Cr2O7 added (graph ∏). From the end point,
the strength of ferrous iron solution and hence its amount can be calculated.
Observations and calculations:
Figure 1 – Potentiometric titration
Step: I
Table – I
Volume of ferrous iron solution = 20 ml
Volume of K2Cr2o7
(ml) Emf (Volts)
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Graph – 1 - Graph-2
Step : II
Table – II
Volume of ferrous iron solution = 20 ml
Volume of K2Cr2O7
(ml)
Emf
(Volts)
E
(Volts)
Vml E / V volts / ml
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Step – III
Calculation of normality of ferrous iron solution:
Volume of ferrous iron solution V1 = 20 ml
Normality of ferrous iron solutionN1 = --------N
Volume of K2Cr2O7 V2 = …………ml(from graph 2)
Normality of K2Cr2O7 N2 = ………..N
According to the law of volumetric analysis V1N1 = V2N2
V2 x N2
N1 = _______
20
Normality of ferrous iron solution N1 = ………….. N
RESULT:
The amount of ferrous iron present in 100 ml of the given solution is = ………gms.
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5. DETERMINATION OF STRENGTH OF HCL AGAINST NaOH BY
pH METRY
AIM:
To determine the strength of given HCL by pH metry, a standard solution of
NaOH……..N is provide.
PRINCIPLE:
Since 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+ ion is the solution.
When NaOH is added slowly of m the burette to the solution of HCL, the fast moving H+
Ions are progressively replaced by slow moving Na+ ions. As a result pH of the solution
Increases.
H+ CL- + Na+ OH- → NaCl+H2O
The increase in pH takes place until the all the H+ ions are completely neutralized
(upto the end point) after the end point, further of NaOH increases pH sharply as there
is an excess of fast moving OH- ions.
MATERIALS REQUIRED:
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1pH meter 2) Glass electrode 3) Beaker 4) Standard n/10 NaOH
5) Approximately N/10 HCI 6) Burette, Pipette, Glass rod etc.,
PROCEDURE:
The burette is filled with std. NaOH Solution. Exactly 20m of the given HCL
Solution is pipetted out into a clean beaker. It is then diluted to 20 ml by adding distilled
Water. The glass electrode is dipped in it and connected with a pH meter.
Now NaOH solution is gradually added form the burette to the HCL solution taken
In the beaker and pH of the solution is noted each addition. This process is continued
Until atleast 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.
Table : I
Volume of HCL Vs NaOH
Volume of NaOH
ml
pH
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Table :
Volume of NaOH Vs pH / V
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Volume of
NaOH ml pH
pH V (ml) pH/ /v
Calculation
Step: I Calculation of Strength of HCL
Volume of HCL V1 = 20 ml
Strength of the HCL N1 = ………N
Volume of the NaOH V2 = ……… (titre value)
Strength of the NaOH N2 = --------- N
According to the law of volumetric analysis
V1N1 = V2N2
V2N2
N1 = _____
V1
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…. X……N
= ____________
20
Strength of HCL present in 1 litre of the given solution = …………. N
Step :II Calculation of amount of HCL :
The amount of HCL Present in
1000ml of the given solution = …… N x Eq.wt.of HCL (36.45)
= ……….. gms
RESULT:
1. Strength of the given HCL solution = ………………N
2. Amount of HCl present in 1 litter of the solution = ………………gms
6. DETERMINATION OF WATER OF CRYSTALLIZATION OF A
CRYSTALLINE SALT (CuSO4)
AIM:
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7. DETERMINATION OF THE IRON CONTENT BY
SPECTROPHOTOMETRY
AIM:
To determine the amount of iron content of an unknown solution by spectrophotometry.
PRINCIPLE :
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Spectrophotometer is an instrument used to measure the intensity of the light absorbed
by a substance. The relationship between absorbance (A) and the concentration of the solution
(C) is given by Beer - Lambert’s law.
Io
log __ = A = ECX
I
Where
Io = Intensity of incident light
I = Intensity of transmitted light
E = Molar absorption co-efficient
X = Thickness of the cell
C = Concentration of the solution
From the equation it is seen that, the absorbance (A) is directly proportional to the
molar concentration and thickness of the cell.
In the determination of iron, ferrous iron solution is acidified with HNO3 to convert
Fe2+ into Fe3+. Fe3+ ions does not give any colour in solution. But, it gives red colour when it
reacts with potassium thiocyanate (KSCN) (or) Ammonium thiocyanate (NH4SCN) solution.
Fe3+ 6KSCN [Fe(SCN)6]
3- + 6K+
red colour complex
This complex has maximum absorption in the region = 480 nm. A calibration curve is drawn
by measuring the absorbance of known solution. Then the absorbance of unknown solution is
measured, using which the concentration can be determined from the calibration curve.
MATERIAL REQUIRED:
1) Spectrophotometer 2) Ferrous ammounium sulphate 3) HNO3 4) 25 ml standard
flask 5 Nos. 6) Graduate pipette 7) Potassium thiocyanate (or) Ammonium
thiocyanate.
PROCEDURE :
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1.Preparation of stock Fe3+ iron solution
A stock solution of Fe3+ is prepared by dissolving 0.0838 gms of ferrous ammonium
sulphate with 1 ml of con. HNO3 in 1 litre of distilled water.
From the stock solution, various concentrations are prepared as shown in table I
1. Determination of iron content
The spectrophotometer is switched on and warmed up for 10 minutes. The monochromater is
adjusted for = 480 nm
The blank solution (distilled water ) is kept in the cell and the absorbance is measured
for which the absorbance is zero and transmittance is 100.
Now the absorbance of all the standard solutions are similarly measured. Also the
absorbance of unknown solution is measured.
The calibration graph is drawn between the concentration and absorbance from which
the concentration of unknown solution is measured.
Table I : Preparation of various concentration of Fe3+ solution
Volume of iron
solution
Volume of
HNO3
Volume of
KCN3
Concentration of Iron
ppm
2
4
6
8
Unknown
3
3
3
3
3
5
5
5
5
5
2 ppm
4 ppm
6 ppm
8 ppm
-
1 ml of stock solution = 1 ppm of iron
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Calibration curve (absorbance Vs concentration)
Table II: Measurement of absorbance
Blank (distilled water) : zero absorbance
Concentration
ppm
Absorbance
2 ppm
4 ppm
6 ppm
8 ppm
Unknown
RESULT:
Amount of iron present in the solution = ……..ppm
CONCENTRATION
AB
SO
RB
AN
CE
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