Safonification Conductometrically SS-13062021 Upload

SS/Chem/BHU
Determine the rate constant of the saponification of Ethylacetate

by NaOH conductometrically.
A) Requirements:
Ethylacetate solution (N/25), NaOH (N/25), Acetic acid (N/10), Oxalic acid,
Conductometer and Conductivity cell, Burette, Pipette, Conical flask, beakers.
B) Theory:
In the presence of base, NaOH, the hydrolysis of CH3COOEt ester takes place to
produce H3CCOO-Na+ and EtOH as follows:
H3CCOOEt + NaOH → H3CCOO-Na+ + EtOH
The reaction follows the 2nd order kinetics. The rate of the reaction can given by:
𝑑
Rate = − 𝑑𝑡 [𝐸𝑠𝑡𝑒𝑟] = 𝑘 [𝑒𝑠𝑡𝑒𝑟][𝑂𝐻−]
where k = Second order rate constant in unit of mol-1LS-1.
The integrated expression of 2nd order rate equation can be given as

1 𝑥
𝑘= … . . (1)
𝑡 𝑎 (𝑎 − 𝑥)
where, a = initial concentration of reactant, x= concentration of product at
time, t. (a-x) = concentration of the remaining reactant at time t.
In the above reaction hydroxide ion progressively consumed by acetate ion. Since
the ionic mobility of OH- ( 0 = 198.5 Ohm-1cm2mol-1) is much higher than CH3COO-
ion ( 0 = 40.9 Ohm-1cm2mol-1); the conductance of the reaction mixture
progressively decreased with the time t. The conductance measurement of the
reaction mixture thus provides a means of estimation of the amounts of these ions
present and hence allow us to monitor the progress of reaction with time.
If the conductance of the reaction mixture are Co, Ct & C∞ at the beginning (t = 0),
any intermediate time (t = t) and at completion of reaction (t = ∞) respectively (where,
Co > Ct > C∞), then,
a  (C0-C∞),
x  (C0-Ct)
hence, (a-x)  (Ct-C∞).
Thus, the equation (1) can be rewritten as:
(𝒄𝟎 − 𝒄𝒕 )
=𝒌𝒂𝒕
(𝒄𝒕 − 𝒄∞ )
Plot of (Co - Ct)/ (Ct - C∞) vs. t (time) gives a straight line passing through origin with
positive slope of ‘k x a’. Since, the initial concentration of the ester is known, k can
be obtained from the slope. While, Ct is determined from the measurements of
conductance at different time interval, C∞ can be determined indirectly by measuring
the conductance of a mixture of solution having same concentration of NaOH and
SS/Chem/BHU
acetic acid. For, determination of C0 only NaOH solution of same concentration need
to be measured.
C) Procedure:
1. Preparation of exact N/10 Oxalic acid standard solution.
2. Standardization of ~N/10 NaOH (given) with prepared oxalic acid solution.
3. Preparation of 100 mL N/25 NaOH (exact).
4. 50 ml (N/25) exact ethyl acetate was prepared.
5. Measure the conductance of 50 mL N/25 NaOH which is considered as C0.
6. Prepare the reaction mixture by adding 50mL of N/25 NaOH in 50 mL of N/25
ethyl acetate.
7. Start taking conductance reading using conductivity cell connected to
conductivity meter. The conductivity meter should be calibrated before start
of the experiment.
8. The conductance reading of the reaction mixture in different time should be
noted in Table 2. This reading is denoted as Ct value.
9. After about one hour (when the variation of conductance will be very small),
reaction mixture is heated (~80 C for ~30 mints), then cooled and
conductance reading is taken in a same way. This reading is marked as C.
[Note: Alternatively, the conductance of solution containing 50 ml N/25 NaOH
and 50 ml N/25 AcOH can be treated as C∞].
D) Observation and Calculation:

Laboratory temperature: 30.5 C
Weight of Oxalic acid taken = 0.635 g
Strength of the prepared 100 mL oxalic acid solution=
(0.635/63.5)x (1000/100)= 0.1N
1. Table 1: Standardization of NaOH solution by titrating against standard oxalic

acid solution.
S.No. Volume of Volume of Concordant

oxalic acid NaOH required value/ ml
taken / ml / ml
1. 10
2.
3.
Calculation
V1N1 = V2N2 ; N2 = say, 0.101N
2. Preparation of exact 100 ml (N/25) NaOH solution: Add 60 mL of distilled water

in 40mL of 0.101 N NaOH.
3. Preparation of exact (N/25) ethyl acetate (50 ml) solution.
4. Table 2: Observation table for conductance measurement:

C0= 6.03 mS
C = 3.76 ms
SS/Chem/BHU
a= C0 - C = 2.27 mS
S.No. Time Conductance (Co-Ct) / (Ct-C∞) / (Co-Ct) C𝑜 – C𝑡

𝑘=
/min / mS, (Ct) mS mS /(Ct-C∞) 𝑎𝑡(C𝑡 – C∞ )
1. 2 5.61 0.42 1.85 0.227 0.050
2. 4 5.06 0.97 1.30 0.746 0.0821
3. 6 4.79 1.24 1.03 1.203 0.0883
4. 8 4.59 1.44 0.83 1.734 0.0954
5. 10 4.45 1.58 0.69 2.289 0.1008
6. 12 4.35 1.68 0.59 2.847 0.1045
7. 14 4.27 1.76 0.51 3.450 0.1085
8. 16 4.22 1,81 0.46 3.934 0.1083
9. 18 4.17 1.86 0.41 4.536 0.1110
10. 20 4.13 1.90 0.37 5.135 0.1131
11. 22 4.10 1.93 0.34 5.676 0.1136
12. 24 4.07 1.96 0.31 6.322 0.1160
[No need of reporting kavg from Table 4]
Determine the slope of the straight line in Graph 1:

Slope = 0.375= k a
k = slope/a= 1.65 x 10-1 mol-1Lmin-1.
E) Result: The rate constant (k) for base (NaOH) catalysed hydrolysis of ethyl
acetate at laboratory temperature (30.5 C) was found to be 1.65 x 10-1 mol-
1Lmin-1.
Graph 1: The variation of conductance with time during the progress of reaction of
ethylacetate hydrolysis in base medium:
For Example, a plot (Origin programme is used to plot).
= (= )
= .

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SS/Chem/BHU

Determine the rate constant of the saponification of Ethylacetate

H3CCOOEt + NaOH → H3CCOO-Na+ + EtOH

The integrated expression of 2nd order rate equation can be given as

Thus, the equation (1) can be rewritten as:

D) Observation and Calculation:

1. Table 1: Standardization of NaOH solution by titrating against standard oxalic

S.No. Volume of Volume of Concordant

2. Preparation of exact 100 ml (N/25) NaOH solution: Add 60 mL of distilled water

3. Preparation of exact (N/25) ethyl acetate (50 ml) solution.

4. Table 2: Observation table for conductance measurement:

S.No. Time Conductance (Co-Ct) / (Ct-C∞) / (Co-Ct) C𝑜 – C𝑡

[No need of reporting kavg from Table 4]

Determine the slope of the straight line in Graph 1:

For Example, a plot (Origin programme is used to plot).

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