Title: Lab Exp.

Report 2 CSTR
By: Abdelmoniem Attia
ID: 141514
Submitted to TA: Rana Adel & Wafaa Hosny

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Abstract
In this work, Saponification reaction of ethyl acetate by sodium hydroxide is studied
experimentally in a continuous stirred tank reactor. The aim of this experiment is to determine
the order of reaction and the reaction rate constant. Once the CSTR reaches steady-state
operation, at specific time intervals withdraw 30 ml sample at the outlet stream and add 45 ml of
0.1 M HCl to it. Load the mixture into 3 separate conical flasks and perform back titration using
phenolphthalein indicator. The rate constant after evaluation from the graphs is approximately
0.0004 mol dm-3 s-1 and saponification of ethyl acetate is a zero-order reaction.

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Contents
Abstract.......................................................................................................................................................3

Introduction.................................................................................................................................................5

Integrated rate laws to find the order of reaction mathematically............................................................6

Method for following the progress of a reaction to find the order of reaction experimentally.................7

Continuous Stirred Tank Reactor.............................................................................................................7

Experimental procedure...............................................................................................................................8

Calculations.................................................................................................................................................8

Conclusion.................................................................................................................................................13

Bibliography..............................................................................................................................................14

List of Tabl
Table 1 NaOH titration volume as a function of time..................................................................................9
Table 2 Concentration, Natural logarithm of the concentration and the inverse of the concentration as a
function of time.........................................................................................................................................11

List of FiguresY
Figure 1 Schematic of a continuous stirred tank reactor (CSTR).................................................................8
Figure 2 shows the concentration of NaOH versus time............................................................................12
Figure 3 shows the natural logarithm of [NaOH]t=ti / [NaOH]t=t0 versus time............................................13
Figure 4 shows 1/[NaOH] versus time.......................................................................................................13

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Introduction
A chemical reaction takes place when one or more chemical species lose their chemical identity.
The identity of a chemical species is determined by the kind or number of atoms in the
compound and the configuration or structure of those species atoms [CITATION Pro1 \l 1033 ].

Reaction kinetic is the study of the rates of chemical reactions. The reaction rate for a particular
reactant or product can be expressed as the rate of disappearance/formation per unit volume. The
rate of a reaction is also defined to be proportional to the concentration of reacting species raised
to a certain power called the order of reaction. The order of reaction shows how the
concentration of a reagent affects the rate of a reaction. The proportionality constant k is called
the rate constant. Orders are determined experimentally and cannot be deduced from the
stoichiometry of a reaction [CITATION Pro1 \l 1033 ].

Rate = k [A]m[B]n

m and n are order of reaction in A and B, respectively.

k is the rate constant

One possibility: The rate of reaction is proportional to the concentration of reactant A

Rate=k[A]

Another possibility: The rate of reaction is proportional to the square of the concentration of
reactant A

Rate=k[A]2

It is also possible that [A] does not affect the rate of reaction and thus the reaction is zero order
with respect to A. [ CITATION Jim13 \l 1033 ]

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Integrated rate laws to find the order of reaction mathematically
Using calculus, the differential rate law for a chemical reaction can be integrated with respect to
time to give an equation that relates the amount of reactant or product present in a reaction
mixture to the elapsed time of the reaction.

The integrated rate law for a first-order reaction has the form of the equation

For these second-order reactions, the integrated rate law is:

The integrated rate law for a zero-order reaction also has the form of the equation of a straight
line:

[ CITATION Wil12 \l 1033 ]

Method for following the progress of a reaction to find the order of reaction
experimentally
 Sampling

This method involves taking samples from the reaction mixture at various times and
then carrying out chemical analysis on each sample.

 Continuous

In this method a physical property is monitored over a period of time.

[CITATION ElH11 \l 1033 ]

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Continuous Stirred Tank Reactor
There are several types of reactors used in chemical or biochemical industries. A continuous
stirred tank reactor is like a batch reactor in that it consists of a tank and a stirrer, however with
the addition of an inlet and an outlet that allow for a constant flow into and out of the reactor.
Once the reactor is started up and reaches steady-state, it is usually assumed to have a constant
volume as well as constant and homogeneous temperature, pressure, and composition
[ CITATION Maz15 \l 1033 ].

Figure 1 Schematic of a continuous stirred tank reactor (CSTR)

Kinds of Phases Usage Advantages Disadvantages

Present
Liquid Phase When Agitation is Continuous operation Lowest conversion
required per unit volume
Good temperature
Gas-liquid rxns Series configurations control By passing and
for different channelling possible
concentration streams Easily adapts to two with poor agitation.
Solid-liquid rxns phase runs

Low operating cost

Easy to clean

Simplicity of
construction

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[ CITATION Uni00 \l 1033 ]

Experimental procedure

 Pumps P1 and P2 are switched on. The feed flow rates F1 and F2are adjusted to be at 300
cm3/min and 100 cm3/min corresponding to NaOH and ethyl acetate using valves V1 and
V2.
 Start the stopwatch as soon as possible.
 After specific time intervals, withdraw 30 cm3 of the product sample at the reactor outlet.
 Quench this sample with 45 cm3 of HCl.
 Partition the 75 cm3 solution into 3 separate flasks or beakers.
 Rinse the burette then fill it with NaOH.
 Add about 3 drops of phenolphthalein indicator to detect the endpoint
 Perform 3 back titrations using each of the flasks with 0.1 M NaOH until the endpoint is
reached
 Record in a table the volume of NaOH added in each accurate titration.
 Do titration calculations to determine the hydroxide ion concentration in the sample.

Calculations

Sample # Time (min) Sample Vol. (ml) Volume of HCl Volume of NaOH
used in used in titration
quenching (ml) (ml)
1 0 30 45 16.5
2 2 30 45 16
3 5 30 45 18.1
4 9 30 45 16.2
5 14 30 45 16.7
6 20 30 45 17.4
Table 1 NaOH titration volume as a function of time

Initial amount, in moles of HCl added =45*10-3*0.1=4.5*10-3

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Amount in moles of HCl equivalent to neutralize=0.1*16.5*10-3=1.65*10-3

Amount in moles of HCl left over from the reaction with NaOH in the sample=2.85*10-3

Concentration of NaOH at time (t=0 minutes) =Amount in moles of NaOH (1:1 ratio)/30*10-
3
=0.095 mol dm-3

Initial amount, in moles of HCl added =45*10-3*0.1=4.5*10-3

Amount in moles of HCl equivalent to neutralize=0.1*16*10-3=1.6*10-3

Amount in moles of HCl left over from the reaction with NaOH in the sample=2.9*10-3

Concentration of NaOH at time (t=2 minutes) =Amount in moles of NaOH (1:1 ratio)/30*10-
3
=0.0966 mol dm-3

Initial amount, in moles of HCl added =45*10-3*0.1=4.5*10-3

Amount in moles of HCl equivalent to neutralize=0.1*18.1*10-3=1.81*10-3

Amount in moles of HCl left over from the reaction with NaOH in the sample=2.69*10-3

Concentration of NaOH at time (t= 5 minutes) =Amount in moles of NaOH (1:1 ratio)/30*10-
3
=0.0896 mol dm-3

Initial amount, in moles of HCl added =45*10-3*0.1=4.5*10-3

Amount in moles of HCl equivalent to neutralize=0.1*16.3*10-3=1.62*10-3

Amount in moles of HCl left over from the reaction with NaOH in the sample=2.88*10-3

Concentration of NaOH at time (t= 9 minutes) =Amount in moles of NaOH (1:1 ratio)/30*10-
3
=0.096 mol dm-3

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Initial amount, in moles of HCl added =45*10-3*0.1=4.5*10-3

Amount in moles of HCl equivalent to neutralize=0.1*16.7*10-3=1.67*10-3

Amount in moles of HCl left over from the reaction with NaOH in the sample=2.83*10-3

Concentration of NaOH at time (t=14 minutes) =Amount in moles of NaOH (1:1 ratio)/30*10-
3
=0.09433 mol dm-3

Initial amount, in moles of HCl added =45*10-3*0.1=4.5*10-3

Amount in moles of HCl equivalent to neutralize=0.1*17.4*10-3=1.74*10-3

Amount in moles of HCl left over from the reaction with NaOH in the sample=2.76*10-3

Concentration of NaOH at time (t= 20 minutes) =Amount in moles of NaOH (1:1 ratio)/30*10-
3
=0.092 mol dm-3

Table 2 Concentration, Natural logarithm of the concentration and the inverse of the
concentration as a function of time

Trial Time (min) [NaOH] (M) ln( [NaOH] t0/ 1/[NaOH] (M-1)

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 [NaOH]ti )

1 0 0.095 0 10.52
2 2 0.0966 0.0167 10.35
3 5 0.0896 0.0585 11.16
4 9 0.096 0.0104 10.42
5 14 0.09433 0.00707 10.60
6 20 0.092 0.032 10.86

0.1

0.1

f(x) = - 0x + 0.09
[NaOH] (mol/dm3)

0.09
R² = 0.09

0.09

0.09

0.09

0.09
0 5 10 15 20 25
Time (min)

Figure 2 shows the concentration of NaOH versus time

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 0.07

0.06
Ln([NaOH]t=t0/[NaOH]t=t)

0.05

0.04

0.03

f(x) = 0x + 0.02
0.02 R² = 0.02

0.01

0
0 5 10 15 20 25
Time (min)

Figure 3 shows the natural logarithm of [NaOH]t=ti / [NaOH]t=t0 versus time

11.4

11.2

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1/[NaOH] (dm3/mol)

10.8
f(x) = 0.01x + 10.56
R² = 0.08
10.6

10.4

10.2

10

9.8
0 5 10 15 20 25
Time (min)

Figure 4 shows 1/[NaOH] versus time

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Conclusion
In this investigation, hydrolysis of ethyl acetate with sodium hydroxide has been studied.
Progress of the saponification reaction was monitored by sampling (back titration). The
experimental data is juxtaposed with the integrated rate laws to check which graph did the set of
data points fit the most. From the experimental findings the reaction is zero order and the
reaction rate constant is 0.0004 mol dm-3 s-1. However, this does not agree with previous
experimental findings where the saponification reaction was experimentally determined as
second order with respect to the reactants. The disagreement in results could arise from the
wrong timing of taking the samples, namely the timing of the process should have started before
the steady state is reached. Taking the sample beyond the time the steady-state has been reached
would result in the exit conditions=reactor conditions. This explains why the concentration is
approximately constant as time transpires.

Bibliography
Clark, J. (2013). ORDERS OF REACTION AND RATE EQUATIONS. Retrieved from
Chemguide: https://www.chemguide.co.uk/physical/basicrates/orders.html#top

El Hamouz, A., & Fuqha, M. (2011). HOMOGENEOUS BATCH REACTOR. Nablus: An-Najah
National University Department of Chemical Engineering.

Fogler, P. (n.d.). Chapter 1 (Mole balances). Retrieved from Chemical Reaction Engineering:
http://umich.edu/~elements/5e/lectures/umich.html

Mazzotti, P. D. (2015). Separation Processes Laboratory (SPL). ETH Swiss Federal Institute of
Technology Zurich.

Michigan, U. o. (2000, May 16). Continuous Stirred Tank Reactors (CSTRs). Retrieved from
Bits and Pieces- Chemical Reaction Engineering:
http://umich.edu/~elements/asyLearn/bits/cstr/index.htm

Robinson, W. R. (2012). Integrated Rate laws. In Chemistry. Open Stax.

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