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Pipette
solution Std CaCl 2 20 ml hard water 20ml Boiled hard
water
Indicator EBT EBT EBT
End point Wine red to Wine red to steel Wine red to Steel
Steel blue blue blue
TITRATION I
STANDARDISATION OF EDTA
Std CaCl 2 Vs EDTA Indicator: EBT
AIM
To estimate the amount of total, temporary and permanent hardness
in the given sample of hard water. A standard solution of CaCl 2 is provided
such that 1 ml of solution is equal to 1 mg of CaCO3
PRINCIPLE
PROCEDURE
TITRATION – I
(i) STANDARDISATION OF EDTA
Pipette out 20ml of sample hard water into a clean conical flask. Add
5ml of buffer solution and 4 -5 drop of eriochrome black T indicator. Titrate
the wine red coloured solution with EDTA from the burette until the colour
steel blue appears at the end point. Repeat the titration for concordant
values. Let the titre value be V2ml.
TITRATION – III
(iii) DETERMINATION OF PERMANENT HARDNESS
Take 250ml of hard water sample in a 250ml beaker and boil gently
for about 20 minutes. Cool, filter it into a 250ml standard flask and make
the volume upto the mark. Take 20ml of this solution and proceed it in the
same way as in titration (I). The volume of EDTA consumed corresponds to
the permanent hardness of the water sample. Let the titre value be V 3ml.
Temporary hardness is calculated by subtracting permanent hardness from
total hardness.
RESULT
(i) Amount of total hardness of the given sample water = ------- ppm.
= ------------ppm
SHORT PROCEDURE:
TITRATION I TITRATION II
Standardization of Estimation of copper
CONTENTS Na2S2O3 (Std. K2Cr2O7 Vs (Std Thio Vs Alloy solution )
Na2S2O3 )
Burette solution Na2S2O3 Na2S2O3
TITRATION I
STANDARDIZATION OF Na2S2O3 WITH K2Cr2O7 SOLUTION
Std. K2Cr2O7 Vs Na2S2O3 Indicator : Starch
S.No. Volume of Burette Reading Volume of Concordant
K2Cr2O7 Initial Final Thio value (ml)
(ml) (ml)
1.
2.
3.
Strength of K2Cr2O7 ( N1 ) = N
Volume of Na2S2O3( V2 ) = ml
= ( 20 x N1 )/ V2
= N
AIM
To estimate the amount of copper present in the given sample of brass.
PRINCIPLE
Brass is an alloy with 55% copper and 33% zinc and small
amount of lead and aluminium. Brass is dissolved in con.nitric acid to convert
copper present in the alloy to cupric ions. Then copper is estimated
iodometrically by titrating the iodine that was liberated against standard sodium
thio sulphate solution using starch as indicator.
PROCEDURE
PREPARATION OF BRASS ALLOY SOLUTION
About 0.2g of the sample of brass was weighed
accurately and transferred into a clean dry 250ml beaker. To this
about 10ml of con. Nitric acid was added and allowed to boil for a
small interval of time till the alloy was dissolved. This was cooled,
diluted with water and made upto 250 ml in a standard flask.
TITRATION I
STANDARDIZATION OF Na2S2O3 WITH K2Cr2O7 SOLUTION
20ml of the standard potassium dichromate solution is
pipetted out into a conical flask. 20ml of dil.sulphuric acid and 10ml
of 10% KI are added. The liberated iodine is titrated against sodium
thio sulphate taken in the burette till the colour changes to yellowish
green. 1ml of starch is added till the colour changes from blue to
light green colour. Titration is repeated for concordancy.
TITRATION II
ESTIMATION OF COPPER
The brass solution is transferred into the 100ml standard flask and
10ml of dil sulphuric acid is added and made up to the mark using distilled
water.
20ml of the alloy solution was pipetted out into a conical flask. To
this aqueous ammonia is added in drops till a blue precipitate of Cu(OH) 2 is
formed. One or two drops of acetic acid is added to dissolve the precipitate.
To this 10ml of 10% KI is added and titrated against standard thio sulphate
using starch as indicator. The end point is the disappearance of blue colour
and appearance of green colour.
RESULT
The given sample of brass is found contain copper to ---------%
TITRATION II
ESTIMATION OF COPPER
1.
2.
3.
Volume of Na2S2O3 V1 = ml
Strength of Na2S2O3 N1 = N
= (V1x N1)/ V2
= --------- N
*200ml of sample water + 2ml of MnSO 4 + 2ml of alk. KI- Shaken for 10 mins. A
brown gelatinous precipitate will be formed. Dissolve it with minimum amount of
Con. Sulphuric acid to get a clear reddish brown solution.
TITRATION1
STANDARDISATION OF SODIUM THIO SULPHATE
=--------- N
Expt.No. 3 ESTIMATION OF DISSOLVED OXYGEN IN WATER SAMPLE
(WINKLER’S METHOD)
AIM
PRINCIPLE
Two methods are widely used to determine DO are:
Winkler’s method
DO reacts with Mn2+ ions in alkaline medium forming basic magnanic oxide
which is a brown precipitate.
MnSO4 + 2 KOH Mn(OH)2 + K2SO4
The liberated iodine is finally estimated by titration with sodium thio sulphate.
= ______ mg/L
The liberated iodine in an amount equivalent to Cr 2O72- reacts with sodium thio
sulphate .
∗ Starch is added as indicator which forms an intense blue colour weak adsorption
complex with iodine present in low concentrations. The complex gets readily
broken when thio sulphate addition is continued and hence a sharp colour change
occurs at the end-point.
PROCEDURE
20ml of std. K2Cr2O7 solution is pipetted out into a clean conical flask.
About 10ml of 10% KI solution and 20ml of dil.sulphuric acid are added. The
liberated iodine is titrated against sodium thio sulphate in the burette. When the
solution turns yellow (pale) colour, 2 to 3 drops of freshly prepared starch indicator
is added and the solution assumes intense blue colour. The addition of sodium thio
sulphate is continued till the blue colour is discharged leaving behind a pale green
colour (due to the presence of Cr3+ ions). The titration is repeated to get a
concordant value.
RESULT
TITRATION I
STANDARDISATION OF AgNO3 :
Std. NaCl Vs AgNO3 Indicator: Potassium Chromate
N2 = (V1 X N1 ) / V2
= N
AIM
To estimate the amount of chloride present in the given water sample, being
supplied with standard solution of sodium chloride of strength _________N .
PRINCIPLE
Generally water contains chloride ions (Cl – ) in the form of NaCl,
KCl,CaCl2, and MgCl2. The concentration of chloride ions more then 250 ppm is not
desirable for drinking purpose. The total chloride ions can be determined by
argentometric method ( Mohr’s Method ).
In this method Cl – ion solution is directly titrated against AgNO3 using potassium
chromate ( K2CrO4) as the indicator
AgNO3 + Cl – AgCl ↓ + NO3–
( in water ) ( white ppt )
At the end point when all the Cl – ions are removed. The yellow colour of
chromate changes into reddish brown due to the following reaction.
2AgNO3 + K2CrO4 Ag2CrO4 +2KNO3
(yellow ) ( Reddish brown )
PROCEDURE
Titration –I
Standardization of AgNO3
The burette is washed well with distilled water and rinsed with small amount
of AgNO3 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 NaCl solution 20 ml of this solution is pipetted out in
to the clean conical flask.1ml of 2% K 2CrO4 indicator solution is added and titrated
against AgNO3 solution taken in the burette. The end point is the change of colour
from yellow to reddish brown. The titration is repeated for concordant values.
Titration –II
Estimation of Chloride ion
20 ml of the given water sample is pipetted out in the clean conical flask and
1 ml of 2% K2CrO4 indicator solution is added. It is then titrated against
standardized AgNO3 solution taken in the burette. The end point is the change of
colour from yellow to reddish brown.
RESULT
Amount of chloride ion present in the given water sample = …….ppm
TITRATION II
ESTIMATION OF CHLORIDE IN WATER SAMPLE:
Std. AgNO3 Vs Water Sample Indicator: Potassium Chromate
N1 = V2 X N2
V1
= N
Amount of chloride ion present in 1 litre( 1000 ml )of the water sample
=Equivalent weight of Chloride ion X strength of chloride ion ppm
AIM
PRINCIPLE
Alkalinity in water is due to the presence of soluble hydroxides,
bicarbonates and carbonates. Alkalinity can be determined by
Potentiometric methods
Using pH meter
Titrimetry using different indicators
TITRATION : 1
STANDARDISATION OF HCl :
Std. NaOH Vs HCl Indicator: Phenolphthalein
TITRATION – II
ESTIMATION OF ALKALINITY IN WATER SAMPLE
Std.HCl Vs Water sample Indicator:1. Phenolphthalein
2. Methyl orange
S.No. Volume of Burette Reading Volume of Concordant
water Initial Final HCl value
sample (ml) (ml)
(ml)
P M P M P M P M
PROCEDURE
TITRATION – I
STANDARDISATION OF HCl
TITRATION – II
ESTIMATION OF ALKALINITY IN WATER SAMPLE
RESULT
1) The type of alkalinity present in the water sample = ------ions.
= -------------- ppm.
=-----------ppm.
Solvent used = Water
AIM
To determine the molecular weight and degree of polymerization of a
polymer by viscosity average method.
PRINCIPLE
[η]int = KMa
Where,
M = molecular weight of the polymer
K & a are constants for a particular polymer – solvent system
η = Intrinsic viscosity = [η sp/C]C=0 = [η r/C]C=0
η sp = specific viscosity = η r – 1
η r = relative viscosity = η/η 0 = t / t0
The flow time of the polymer solution (t) and that of the pure solvent (t 0)
are found experimentally and substituted to get η sp , η r and thus [η]int.
Knowing K & a, molecular weight of the polymer solution is calculated.
DP = M / m (M= mol.wt of polymer, m = mol. wt of monomer)
PROCEDURE
Graph - I
nsp/C
Concentration (g/dl)
Graph - II
lnnr/C
Concentration (g/dl)
Where X = volume of bulk solution to be taken for preparing 100ml of
0.2g/dl Polymer solution]
A well cleaned Ostwald viscometer is rinsed with water and filled with
10ml of distilled water, Water in the viscometer is sucked into the upper
bulb using a rubber bulb. The time taken for water to flow from the upper
mark to the lower mark is measured with a stop clock and noted as t0.
RESULT:
The molecular weight of the given polymer =
The degree of polymerization of the polymer =
Rough titration:
S.No Volume of Observed
. NaOH conductance
added (ml) (m mho)
Fair titration:
S.No Volume of Observed
. NaOH conductance
added (ml) (m mho)
AIM
PRINCIPLE
PROCEDURE
A conductivity cell is dipped into the beaker with HCl solution and connected to
the terminals of the conductivity bridge. About 1ml of Std NaOH is added and
stirred well for 30 seconds. The conductance is measured and the titration is
continued till five measurements after the endpoint. A graph is plotted for the
conductance values against the volume of NaOH and the endpoint range is fixed.
The above titration is repeated again and the exact endpoint is found out by
adding in increments of 0.1ml of NaOH in the end point range and continued after
endpoint upto five readings.
A graph is plotted with the conductance values against the volume of NaOH and
then the strength of the strong acid is found out.
RESULT
Rough titration:
Fair titration:
AIM
To determine the strength of strong acid and weak acid present in the
given acid mixture
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 the titration.
HCl + NaOH NaCl + H2O (I neutralization)
CH3COOH + NaOH CH3COONa + H2O (II neutralization)
When a solution of HCl is treated with NaOH the fast moving hydrogen
ions are progressively replaced by slow moving sodium ions. As a result
conductance of the solution decreases. This decrease will take place until
the first neutalisation point is reached. Further addition of alkali results in
formation of sodium acetate.
Since sodium acetate is stronger electrolyte than acetic acid,
conductivity slowly increases until all acetic acid is completely neutralized.
(II Neutalisation) This is due to the presence of fast moving OH - ions.
Anymore addition of alkali increases the conductance sharply.
PROCEDURE
The burette is filled with NaOH solution upto zero mark. The given
unknown solution (mixture of a weak & a strong acid) is transferred into a
100ml standard flask and made upto the mark with distilled water. 20ml of
the made up solution is pipetted out into a clean 100ml beaker. The
solution is diluted to 50ml using distilled water. A conductivity cell is
dipped into the solution and the terminals are connected to a conductivity
meter.
The burette solution is added to the unknown solution in the beaker in 1
ml increments, the solution is stirred using a glass rod, and the observed
conductance values are read from the meter. The conductance values show
decrease in the initial values, then gradually increases and finally shows a
steep increase. The titration hence shows two end-points (ie) I
neutralization (strong acid) & II neutralization (weak acid).
The titration is repeated with the same procedure by adding 0.1 ml
increments of the burette solution in the region of the end-point and the
conductance values are noted for all the increments. The accurate end-
point is obtained by plotting a graph between observed conductance Vs
volume of NaOH added.
RESULT
The strength of acids present in the given unknown solution are
a) Strong acid = N b) Weak acid = N
AIM
PRINCIPLE
PROCEDURE
The burette is filled with Na2SO4 solution upto the zero mark. The
given unknown solution is carefully transferred into a 100ml standard flask
using a funnel and glass rod and the solution is made upto the mark using
distilled water. 20ml of the made up solution is pipeted out into a clean
100ml beaker. The conductivity cell is placed in it and then the solution is
diluted to 50ml by adding distilled water. The conductivity cell is
connected to conductivity meter.
The titration is repeated with the same procedure. In the range of the
end point the titration is carried out by adding 0.1ml increments and the
accurate end point is obtained by plotting a graph between the observed
conductance values and the volume of sodium sulphate solution added.
RESULT
precipitation
Conductance
= ---------- g
Rough titration:
Fair titration:
S.No Volume of Emf in mVolt ∆E in mVolt ∆V in ml ∆E/∆V in
Dichromate m Volt/ml
in ml
Expt. No 10
ESTIMATION OF FERROUS ION BY POTENTIOMETRIC TITRATION.
AIM
To estimate the amount of ferrous ion present in the given solution
potentiometrically. 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.
PROCEDURE
The given Ferrous solution is made up in a 100ml standard flask. Std.
Potassium dichromate solution is filled in the burette upto the mark.
20ml of Ferrous solution is pipetted out into a 100 ml beaker. 10ml of
dil.H2SO4 and 20ml of distilled water are added. A platinum electrode and a
calomel electrode are dipped into this solution and connected to a potentiometer.
Then 1ml of potassium dichromate is added to the solution and stirred well for 30
seconds. The emf is measured and the titration is continued by adding potassium
dichromate in 1ml increments till five measurements after the end point.
A graph is drawn by plotting the emf against the volume of potassium
dichromate and the end point range is fixed.
About 20ml of Ferrous solution is pipetted out and the titration is continued by
adding 0.1ml increments of potassium dichromate in the end point range. The emf
is measured for each 0.1ml after stirring the solution well.
A graph is plotted between emf and the volume of potassium dichromate and
also a first derivative graph is plotted (ΔE/ΔV against vol. of K 2Cr2O7). The
strength of Ferrous solution and the amount of Ferrous ion present are calculated
from the end point.
RESULT
Rough titration:
ROUGH GRAPH
EMF(mV)
Volume of Potassiumdichromate
FAIR GRAPH
ΔE/ΔV
Volume of
Potassiumdichromate
= ------------ N
= g
Rough titration:
pH
ΔpH/ΔV
Eq.Pt
Volume of Volume of
NaOH(ml) NaOH(ml)
Expt.No. 11 DETERMINATION OF STRENGTH OF HCl WITH NaOH
BY pH METRY
AIM
PRINCIPLE
When all H+ ions of HCl are neutralized at the end point, addition of
NaOH causes high increase in pH because of the addition of excess OH -
ions.
PROCEDURE
The burette is washed with distilled water, rinsed with the given std.
Sodium hydroxide and filled with the same solution. Exactly 20ml of the
given HCl solution is pipetted out into a clean beaker. It is then diluted to
50ml with distilled water. A glass electrode is dipped into the solution and it
is connected to a pH meter.
Now NaOH is gradually added from the burette to HCl taken in the
beaker. pH of the solution is noted for each addition of NaOH. This
process is continued until atleast 5 readings are taken after the end point.
RESULT
(i) Strength of the given HCl solution = ---------- N
Fair titration:
Std.NaOH Vs HCl
AIM:
Determine the percentage of water of crystallization in crystalline Copper
sulphate.
PRINCIPLE:
A known weight of AR Copper sulphate crystals are heated and the weight of
anhydrous Copper sulphate is determined. From the weight loss, the percentage of
water is calculated.
PROCEDURE:
A silica crucible is heated to dull redness over a clay pipe triangle for about
15 minutes using a non luminous flame .Then it is heated strongly. After heating the
crucible is kept in a dessicator, allowed to cool for about half an hour and weighed
accurately.(W1 g)
About one gram of crystalline AR Copper sulphate is introduced in the
crucible and is again weighed accurately. (W2 g). It is then heated strongly keeping
the lid slightly tilted to one side for the water vapour to escape. Heating is
continued for half an hour. The crucible and contents are then cooled in a
desiccator and weighed. (W3 g) . The process is repeated for concordance. A
duplicate is also conducted.
RESULT:
The percentage of water of crystallization in hydrated Copper sulphate = -------
S.No. Concentration Absorbance
(N)
MODEL GRAPH
ABSORBANCE
CONCENTRATION
PRINCIPLE
When a monochromatic light passes through a homogeneous coloured
solution, a portion of incident light is reflected, a portion is absorbed and the
remaining is transmitted.
Io = Ir + Ia + It
T = I / Io = 10 -∈CI
Fe3+ ion does not give any colour in solution. However, it develops a red
colour when it reacts with KCNS solution.
I0
ELECTRICAL
SLIT
SIGNAL
SOURCE MONOCHROMATOR SAMPLE CELL DETECTOR DISPLAY
INSTRUMENTATION
PROCEDURE
RESULT
The strength of iron present in the given solution = ----N
The amount of iron present in the given solution = ----------- ppm
CHEMISTRY PRACTICALS -- VIVA-VOCE – QUESTION BANK
1.ESTIMATION OF HARDNESS
1. What is Hardness?
2. What are the two types of hardness.
3. Write the structure of EDTA.
4. Give the reaction between EBT and metal ions.
5. What is the pH range for a complex stability.
6. What is the buffer used here?
7. Give the reason for formation of red and blue colour .
8. What are the ill effects of hardness.
9. What may be the range of hardness in a portable water sample.
10. What is the need of filtration during the experiment?
11. What are the units by which hardness is expressed?
12. What is the other name for Eriochrome black T?
2.ESTIMATION OF ALKALINITY
1. What is alkalinity?
2. What are the ions responsible for alkalinity?
3. What are the five possible alkalinities?
4. What are the indicators used ?
5. What is equivalent. weight of CaCO3.
6. Why we are taking CaCO3 equivalence as reference?
7. What is the reaction of Phenolphthalein end point?
8. What is PPM?
9. Explain Lewis concept.
10. Expalin Bronsted – Lowry concept .
11. What is the colour of phenolphthalein in acidic and basic mediums?
12. What is the colour of methyl orange in acidic and basic mediums?
4.ESTIMATION OF CHLORIDE:
1. Explain the principle behind the argentometry?
2. What do you mean by back titration?
3. Why are we taking excess (40ml) of Silver nitrate?
4. Why are we getting a blurred solution during the titration?
5. What is the reaction between alum and burette solution ( thio cyanate)?
6. What type of medium do you prefer for chloride estimation?
7. What is the colour change that infers you regarding the end point?
8. What is break point chlorination?
9. What is the relationship between ppm and gm/ml?
10. What are the different sources of chlorine in water?
9. pH METRY
1. Define pH
2. Give the principle of pH metry
3. Name the electrodes used in the determination of pH of a solution.
4. Which electrode acts as anode and which acts as cathode?
5. What is the effect of temperature on pH
6. What is the effect of dilution on pH of an acidic solution?
7. What is the pOH of pure water at 25°C
8. What is a combined electrode?
9. What is the significance of pH titration?
10. Brief the function of calomel electrode.
11. What is the pH of lime juice, blood and de-ionised water?
12.WATER OF CRYSTALLISATION
1. What is the molecular formula for hydrated copper sulphate?
2. Give the reaction for the dehydration of copper sulphate?
3. What is the colour change for dehydration of copper sulphate?
4. What is the molecular weight of hydrated copper sulphate?
5. What is gravimetry?
6. What are the precautions to be taken during gravimetric analysis?