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Ex. No.

1 DETERMINATION OF Na2CO3 AND NaOH IN A MIXTURE BY TITRATION

AIM:
To determine the amount of Na2CO3 and NaOH in a mixture using hydrochloric acid.

Principle:
When a known volume of the mixture of Na2CO3 and NaOH is titrated with HCl using phenolphthalein
indicator, at the end point, all the hydroxide ions (OH-) and only half of the carbonate ions (CO32-) are
reacted with hydrochloric acid.
When the titration is continued with methyl orange indicator, the remaining half of CO32- ions will

be neutralized with HCl at the end point.

A = all hydroxide ions + half of carbonate ions


B = half the carbonate ions after phenolphthalein end point
2B = all carbonate ions
A-B = all hydroxide ions Procedure:
Titration I : Standardization of HCl
Pipette out 20 ml of 0.1 N Na2CO3 solution into a clean conical flask and add 2-3 drops of methyl
orange indicator to the solution. Then titrate the solution against hydrochloric acid taken in the burette.
Record end point (burette reading) when color changes from yellow to orange. Repeat the titration till the
concordant (two consecutive burette readings exactly same) value is obtained.

Titration II: Estimation of Na2CO3 and NaOH in a given mixture


Dilute the given unknown solution to 100 ml in a standard flask using distilled water. Pipette out
20 ml of this made up solution into a clean conical flask. Add 2-3 drops of phenolphthalein indicator to the
solution and titrate against standardized HCl. Record the burette reading as an end point (phenolphthanlien
end point) of the titration when disappearance of pink color is observed. Let’s consider the burette reading
at the end point be ‘A’ ml. To the same solution, add 2-3 drops of methyl orange indicator and continue the
titration till the color changes from yellow to orange and note down the burette reading as methyl orange
end point. Consider it to be ‘B’ ml. Repeat the titration till the concordant (two consecutive burette readings
exactly same) value for A and B is obtained.

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Titration 1 : Standardization of HCl

S.No. Volume of sodium Burette reading Concordant Value Indicator


carbonate solnution Initial Final
(ml)

Methyl orange
(2-3 drops)

CALCULATION: (for Titration 1: Standardization of HCl)


Volume of HCl = V1 ml (end point)
Normality of HCl = ----- ? N1
Volume of Na2CO3 (V2) = 20 ml
Normality of Na2CO3 (N2) = 0.1N
Normality of HCl (N1) = (20 X 0.1) / V1
= _____ N
Titration II: Estimation of Na2CO3 and NaOH in a given mixture.
S.No. Volume of the unknown Burette Reading (ml)
solution (ml)
Initial Volume consumed for Volume consumed for
phenolphthalein end point methyl orange end point
(A) after phenolphthalein end
point (B)

Concordant Value (A) (B)

CALCULATION: (for Titration 2)


I Estimation of the amount of Na2CO3
Volume of HCl V1 = 2B (B is the titre value, after phenolpthalein end point)
Normality of HCl = N1 (from Titration I)

2
Volume of mixture V2 = 20 ml
Normality of Na2CO3 N2 = V1 N1/ V2
= 2B x N1 / 20

Amount of Na2CO3 present in whole of the given solution = N2 x 53 (Eq. wt. of Na2CO3)

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II Estimation of amount of NaOH:
Volume of HCl V1 = (A-B) ml
Normality of HCl (N1) = N1 (from Titration I)
Volume of mixture V2 = 20 ml
Normality of NaOH N2 = V1 x N1/ 20
= (A-B) x N1/ 20

Amount of NaOH present in whole of the given solution = [ N2 x 40 (Eq. wt. of NaOH) ]/10

RESULT:
Amount of Na2CO3 present in the given solution = ----- g
Amount of NaOH present in the given solution = ----- g

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Ex. No. 5 Estimation of amount of chloride in a water sample.
AIM:
To estimate the amount of chloride in a water sample by Mohr’s method.

PRINCIPLE:
It is an example of precipitation reaction. The reaction between chloride and silver nitrate is direct
and simple. It proceeds as follows:
AgNO3 + NaCl → AgCl ↓ + NaNO3
Ag+ + Cl- → AgCl ↓
The completion of the reaction in this case is observed by employing potassium chromate (K2CrO4) solution
as an indicator. At the end point, the yellow color changes into reddish brown due to the reaction
2AgNO3 + K2CrO4 → Ag2CrO4 + 2KNO3
K2CrO4 indicator will not be precipitated as Ag2CrO4 until all the chlorides in the solution have been
precipitated as AgCl.

PROCEDURE:
Titration I - Standardization of silver nitrate solution
10 ml of standard NaCl solution (N/20) is pipetted out into a clean conical flask. 2 drops of 2 %
K2CrO4 indicator is added to it. The solution turns yellow in color. It is titrated against AgNO3 solution
taken in the burette. During each addition of AgNO3, the content in the conical flask is shaken well. At the
end point, yellow color changes into reddish brown (which does not disappear even after shaking).
The titration is repeated till the concordant (two consecutive readings exactly same) value is obtained.

Titration II: Estimation of chloride


The given chloride solution is diluted to 100 ml using distilled water in a standard flask. Exactly 10
ml of this solution is pipetted out into a clean conical flask. To this solution 2 drops of 2 % K2CrO4 indicator
is added. It is titrated against standardized AgNO3 solution from the burette. The addition of AgNO3 solution
is continued until the solution produced a permanent reddish brown color. The titration is repeated till the
concordant value (two consecutive readings exactly same) is obtained. From the volume of AgNO3
consumed, the strength of chloride and hence its amount is calculated.

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Table 1. Standardization of AgNO3.
S.No. Burette Reading (ml) Concordant Indicator
Volume of NaCl solution Initial Final Value (ml)
(ml)

2 % Potassium
chromate
(2 drops)

Table 2. Estimation of Chloride


S.No. Burette Reading (ml) Concordant Indicator
Volume of chloride solution Initial Final Value (ml)
(ml)

2 % Potassium
chromate
(2 drops)

CALCULATION Titration I - Standardization of AgNO3 Solution

Normality of NaCl Solution = N1


Volume of NaCl Solution = 10 ml (V1)
Volume of AgNO3 Solution = V2 (end point)
Normality of AgNO3 Solution = ___ ? N2
N2 = V 1 X N1 / V 2
Titration II - Estimation of Chloride
Volume of chloride solution = 10 m1 (V1)
Normality of chloride solution = ____? N1
Volume of AgNO3 solution = V2 (end point)
Normality of AgNO3 solution = N2 (from tit I)
N1 = V 2 X N2 / V 1
(Amount of chloride present in the = Normality of chloride solution (N1) x 35.46 / 10 whole of
the given solution) = ----- g/ 100 mL

RESULT:
Amount of chloride present in the whole of the given solution is ------- g / 100 mL

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Ex. No. 7 DETERMINATION OF THE STRENGTH OF A MIXTURE OF ACETIC ACID AND
HYDROCHLORIC ACID BY CONDUCTOMETRY

Aim:
To estimate the strength of the mixture of acetic acid and hydrochloric acid present in a
given mixture by conductometry.

Principle:
The conductivity of the solution is related to the mobility of ions which in turn is related
with the size of the ions. When a mixture of acids like a strong acid (hydrochloric acid, HCl) and
a weak acid (acetic acid, CH3COOH) is titrated against a strong base (sodium hydroxide, NaOH),
HCl reacts first followed by CH3COOH. When the titration of strong acid and strong base is carried
out, there is a decrease in conductivity as highly mobile hydrogen ions (H+) are replaced by sodium
ions (Na+).
NaOH + HCl NaCl + H2O
When the whole strong acid is consumed, base reacts with weak acid and conductivity
increases as unionized weak acid becomes the ionized salt.
CH3COOH + Na+ + OH- CH3COO- + H+ + Na+ + OH-
After both the acids are consumed, there is a steep increase in conductivity which gives the
end point and this increase in conductivity is due to the fast moving hydroxide ions from the burette
solution. From this, amount of base consumed for an acid and in turn, the amount of acids present
is calculated.

PROCEDURE:
The given mixture of acids is diluted to 100 ml using distilled water in standard flask. 20
ml of this made up solution is pipetted out into clean beaker and 100 ml of distilled water is added.
The conductivity cell is dipped into the test solution and titrated against NaOH (0.5 ml interval)
with proper stirring. The conductance is measured after each 0.5 ml addition of NaOH. After
complete neutralization, the amount of acid present in the given mixture is determined based on
the volume of NaOH consumed. Volume of base consumed for strong acid and weak acid are

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determined by plotting a graph between conductance and volume of base added, where first end
point corresponds to strong acid and second end point corresponds to weak acid.

TABLE-1: Titration between mixture of acids and NaOH


S.No. Volume of NaOH added (ml) Conductance (ohm-1)

1
2
.
.
.
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CALCULATION
STRENGTH OF HCL
Volume of mixture = 20 ml
Normality of HCl = ---? N1
Volume of NaOH = V1 ml [ Ist end point from graph]
Normality of NaOH = 0.1 N
Strength of HCl = V1 x 0.1
20

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= ------ N.

STRENGTH OF CH3COOH
Volume of mixture = 20 ml
Normality of CH3COOH = --- ? N1
Volume of NaOH = V2 – V1ml [V2 - 2nd end point from
graph]
Normality of NaOH = 0.1 N
Strength of CH3COOH = 0.1 x (V2 – V1)
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= -----------N

RESULT:

1. The strength of HCl present in the whole of the given solution ______________ N.

2. The strength of CH3COOH present in the whole of the given solution _________ N.

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Ex. No. 8 DETERMINATION OF STRENGTH OF AN ACID USING pH METER

Aim
To find out the strength of given hydrochloric acid solution by titrating it against sodium
hydroxide (0.1N) using pH meter.

Principle
When an alkali is added to an acid solution, the pH of the solution increases slowly, but at
vicinity of the end point, the rate of change of pH of the solution is very rapid. From the sharp
break in the curve, we can find out the end point, from which the strength of HCl can be calculated.

Procedure

First standardize the pH meter using different buffers of known pH, then wash the glass
electrode and reference electrode with distilled water and then with the acid solution. The given
acid is diluted to 100 ml using distilled water. 10 ml of this made up solution is pipetted out into a
250 mL clean beaker and 90 ml of distilled water is added to it, so that the glass electrode as well
as the reference electrode are completely dipped. Note the initial pH of the pure acid solution. Fill
the burette with standard NaOH solution and run down into the beaker in small increments (1mL).
Stir the solution well using glass rod. Note down the pH after every successive addition. Continue
the titration till beyond the neutralization point as indicated by an abrupt change in pH. (atleast 30
increments). Plot a pilot graph of volume of NaOH versus pH. The midpoint of the ‘S’ shaped
curve of the graph gives the equivalence point. (Note: near the end point add very small amount of
NaOH, because change in pH will be very much appreciable when the acid is neutralized, further
addition of such a small quantity of 0.01 mL raises the pH about 9 to 10).
In order to get an accurate end point, perform one more similar titration in a small volume
range (1.0 mL on either side of the abrupt change in pH) and measure the pH after addition of
every 0.1 mL of standard NaOH solution. Plot a fair graph of volume of NaOH versus Δ pH / ΔV.
Find out the exact end point from the fair graph. The peak point of the curve from the fair graph
gives the end point.

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Table 1: Pilot titration (HCl Vs NaOH)

S.No Volume of NaOH (V) ml pH

1.
2.

3.

….

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Table 2: Fair titration (HCl Vs NaOH)

S.No. Volume of NaOH (V) ml pH Δ pH ΔV Δ pH / ΔV

1.
2.

3.

….

20.

Pilot Graph Fair Graph

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CALCULATION

Volume of NaOH V1 = ------------- ml [from FAIR graph]

Strength of NaOH N1 = ------------ N

Volume of HCl V2 = 10 ml

Strength of HCl N2 = N

Therefore strength of HCl (N2) = V1 x N1 / V2

= -----------N.
RESULT:

The strength of given hydrochloric acid solution is ------- N.

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