OBJECTIVE:

Determination of rate constant for saponification of ethyl acetate with NaOH via conductometry
in CSTR under pseudo steady state conditions.

ABSTRACT:
This experiment was performed to study the saponification reaction of sodium hydroxide and
ethyl acetate in continuous stirred tank reactor (CSTR). It was also done to observe the effect of
concentration on the electrical conductivity with respect to time. The results were recorded in the
form of table and graph was plotted to calculate the rate of constant. The values were compared
with the theoretical to determine the trend of the slope of the graph.

APPARATUS:
Glass wares (beakers), continuous stirred tank reactor (CEM-MKII) mounted on chemical
reactor service unit (CEX-MKII), conductivity meter.

REAGENTS:
Distilled water, 5 liters standard NaOH solution (0.06 M), 5 liters standard ethyl acetate (0.06M),
calibration solutions of conductivity meter.

INTRODUCTION:
CSTR (continuous stirred tank reactor) runs at steady sate with continuous flow of reactants and
products; the feed assumes a uniform composition throughout the reactor, exit stream has the
same composition as in the tank. This type of reactor is suitable for liquid phase, gas-liquid
reactions and solid-liquid reactions. It provides good temperature control, continuous operation,
simplicity of construction and low operating (labor) cost. It easily adapts to two phase runs and
easy to clean. CSTR is used when agitation is required. The reactor gives lowest conversion per
unit volume as well as by-passing and channeling is possible with poor agitation. Conductivity is
the measure of the amount of electrical current a material can carry or ability to carry current.
Electrical conductivity is also known as specific conductance. Conductivity is an intrinsic
property of a material. Conductivity is denoted by σ and has SI units of Siemens per meter (S/m).
It is reciprocal of the electrical resistivity. Conductivity gradually increases in a metallic
conductor as the temperature is lowered. In electrolytes, entire ions move, carrying their net
electrical charge. In electrolytic solutions, the concentration of the ionic species is an important
factor in the conductivity of the material. The higher the concentration of ions in solution, the
higher its conductivity will be. Temperature also affects the conductivity of an electrolytic
solution. A conductivity meter measures the amount of electrical current or conductance in a
solution. Conductivity meters are used in any water treatment or monitoring situation as well as
in environmental laboratories. The meter is equipped with a probe. The probe is handheld and
after it is placed in the liquid to be measured, the meter applies voltage between two electrodes
inside the probe. Electrical resistance from the solution causes a drop in voltage, which is read by
the meter. The meter converts this reading to milli or micro Siemens per centimeter [1].
 APPLICATIONS:

 CSTRs are most commonly used in industrial processing, particularly in homogeneous

liquid phase flow reactions, where constant agitation is required.
 Fermenters are CSTRs used in biological processes in many industries such as brewing,
antibiotics and waste treatment. CSTRs are also used in the pharmaceutical industry as a
loop reactor [2].

 Hot water
Feed Tanks circulator

CSTR 

(mounted)
Conductivity
display &
selector switch

Peristaltic
pump

Figure 1: Labelled diagram of continuous stirred tank reactor

PROCEDURE:
 5 liter (0.06 M) standard solutions of NaOH and ethyl acetate were being prepared.
 Feed vessels were rinsed with distilled water.
 NaOH and ethyl acetate solutions were being poured in feed vessels.
 Agitator motor control was adjusted at 1 and 4.
 Peristaltic pumps were being adjusted to deliver 65 mL/min flowrate for each reagent.
 The conductivity of the NaOH in feed vessel was noted down.
 The conductivity and temperature of the reaction mixture was being monitored after
every 3 minutes.
 Readings were taken till (pseudo) steady state was achieved i.e. nearly 45 minutes.
 Conductivity meter probe was rinsed.
 CSTR into a measuring flask was drained and the volume of reaction mixture in CSTR
was noted down.
 Chemical Reactor service unit and reactor were being washed with distilled water and
any residual water was being drained.
  Electrical connections were being turned off.

OBSERVATIONS & CALCULATIONS:

TABLE # 1: VALUES OF CONDUCTIVITY WITH RESPECT TO TIME:
Time (min) Instantaneous conductivity 𝜆 (𝑆)
(mS)
0 5.1 0.0051
3 5.4 0.0054
6 5.1 0.0051
9 4.06 0.00406
12 3.66 0.00366
15 3.2 0.0032
18 2.8 0.0028
21 1.87 0.00187
24 2.10 0.00210
27 2.83 0.00283
30 3.40 0.00340
33 3.87 0.00387
36 4.13 0.00413
39 4.37 0.00437
42 4.51 0.00451
45 4.52 0.00452

Initial concentration of NaOH in feed vessel 𝐶𝐴𝜇 = 0.06 𝑀

Initial concentration of NaOH in mixed feed (CAo) = 𝑣𝐴𝑣𝐴+𝑣𝐵 𝐶𝐴𝜇 = (65/65+65) X 𝐶𝐴𝜇 = 0.03 M
Concentration of NaOH in reactor after infinite time = 𝐶𝐴∞ = 𝐶𝐴𝑂 − 𝐶𝐵𝑂 = 0
Initial concentration of Na-acetate in mixed feed (CCo) = 0
Concentration of Na-acetate in reactor after infinite time = 𝐶𝐶∞ = 𝐶𝐴𝑂 = 0.03 M
Initial conductivity of solution in reactor at zero time = 𝜆𝑂 = 𝜆𝐴𝑂 + 𝜆𝐶𝑂 = 𝜆𝐴𝑂 (𝜆𝐶𝑂=0)
𝜆𝐴𝑂 = 0.195[1+0.0184(𝑇−294)] 𝐶𝐴𝑂
𝜆𝑂 = 𝜆𝐴𝑂 = 0.00628 Siemens
𝜆∞ = 𝜆𝐴∞ + 𝜆𝐶∞ = 𝜆𝐶 ∞ (𝜆𝐴∞ = 0)
𝜆𝐶∞ = 0.070[1+0.0284(𝑇−294)] 𝐶𝐶∞
𝜆∞ = 𝜆𝐶∞ = 0.00233 Siemens
(Pseudo) steady state conductivity of solution in reactor = 𝜆 = 0.00451 Siemens
Volume of reaction mixture = V = 1.7 L
Change in concentration of NaOH is proportional to change in conductivity of solution hence,

𝐶𝐴 = 0.0165 M
Component material balance (NaOH) around reactor:
Input- output + generation – consumption = Accumulation
CSTR is a steady state reactor. Hence, accumulation term will be zero. Also NaOH is consumed
in reactor.
𝑣𝐶𝐴𝑜−𝑣𝐶𝐴−(−𝑟𝐴) 𝑉= 0
𝑣𝐶𝐴𝑜−𝑣𝐶𝐴−(𝑘𝐶𝐴2) 𝑉=0

(k) = 3.79 L/mol.min

DISCUSSION & CONCLUSION:

From literature, the value of conductivity increases with the increase in concentration with
respect to time. But the table shown above indicates an abnormal trend. There could be some
reasons such as faulty apparatus, incompetency of the observer, improper handling of the molar
solutions, side reactions or inconsistency of flowrates etc. The rate constant at pseudo-state
comes out to be 3.79 L/mol.min. Comparing this positive value with the theoretical one, it is
being confirmed that the saponification reaction between NaOH and ethyl acetate is second order
elementary reaction.

REFERENCES:
1. Hoffman, R.J., Differential conductivity meter for fluids and products containing such
meters. 1992, Google Patents.
2. Uppal, A., W. Ray, and A. Poore, The classification of the dynamic behavior of
continuous stirred tank reactors—influence of reactor residence time. Chemical
Engineering Science, 1976. 31(3): p. 205-214.