Heriot-Watt University

Chemical Engineering

Multiphase Thermodynamics

Laboratory report 2

Name Parvin Salamzada

Group number KM3

Experiment Liquid Phase Chemical Reactor

Date 03.03.2017

Demonstrator Amir Reza Vakhshouri

Contents

Synopsis ........................................................................................................................ 3

Introduction ................................................................................................................... 3

Basic Theory.................................................................................................................. 4

Experimental details ..................................................................................................... 6

Recorded data and Results .......................................................................................... 6

Discussion ..................................................................................................................... 15

Conclusion .................................................................................................................... 16
Synopsis

The chemical reactors are one of main prats of the chemical industries. Thus efficient
designing reactors in order to obtain better yield and higher selectivity are very important.
Homogeneous reaction occurring between ethyl acetate () and sodium hydroxide
() is investigated in this experiment. The reaction occur in batch mode and the
mixture is stirred by help of agitator. Ethyl hydroxide () and sodium acetate ()
are produced from the reaction. The reaction is exothermic and in order to take the
produced heat from the reactor, water is used. In order to determine concentration of
reactants and products as the reaction proceeds, samples are taken from the reactor and
certain amount of solution and indicator is added to the samples. After by using
these obtained results and some equations given in the theory part, the order of reaction
and the rate of reaction at certain times are determined. Activation energy of reaction is
calculated by using Arrhenius equation:

Table 1.
Activation energy Frequency factor
Run
J/mol 1/s
50 rpm 7507.9 0.070360
100 rpm 23275.4 38.989560
150 rpm 21729.1 19.218040

The experiment consist of three part. In each part, the frequency of the stirrer is changes
and its effect on reaction rate is described in the Discussion part. As seen from the table
given above, the activation energy of each run is different. Theoretically, the activation
energy should decrease because as the stirrer speed increase, the kinetic energy of the
molecules increase. The molecules easily break the energy barrier and reacts easily.
When increasing the stirrer speed, the molecules behaves as if the temperature of them
has been increased. Because, in both case the kinetic energy of the molecules increase
and the reaction occurs easily. However, this means there are some deviations with
obtained data. The main reason of these deviations are shown in the Discussion part.

Introduction

Generally, the stirred tank batch reactors commonly used in chemical industry. The
reactants is feed to the reactor and treated altogether for a certain time. They are used
mainly for small scale production of high price products. More uniform residence and ideal
mixing time could be achieved in the batch reactor which means better yields and higher
selectivity in comparison to continuous reactors. However, in most chemical industries,
continues reactors preferred rather than batch. Because for continues reactors, the
capital cost and running costs are less than batch type. Actually, data obtained from lab
experiment could be used to predict behavior of continuous flow reactors. The main
problem related to stirrer tank batch reactor is abrasion of the matrix particles. The reason
behind abrasion the mixer blades, generated shear and air injection.

The main purpose of the experiment is determination of rate and order of reaction
which is to carry out in batch reactor in liquid phase .Moreover, by doing this experiment,
we used to how to run a small lab scale chemical reactor and extract samples from the
reactor mixture. The taken samples are titrated and indicator is added in order to get
proper information about concentration of reactants and reagents .A saponification
reaction occur between Sodium Hydroxide () and Ethyl Acetate () and
Sodium Acetate () and Ethyl hydroxide () are produced:

+ +

Generally investigation of rates of reactions is crucial to predict how much time is

needed to reach equilibrium. In fact, rate of a reactions depends on some factors such
as, the pressure, the temperature, and the presence of a catalyst. So, the reaction could
be optimized by choosing proper conditions.
For e chemical reaction occur between the species, first of all they should come
into contact. Some reactions are lucky enough reacting instantly. However, there are
some reactants that dont have enough energy to react when they comes into contact.
So. These species should collide each other with enough energy in order to break the
bonds and reacting.

Basic Theory

The rate of reaction is determined by the amount of reactants changed into products
in a unit time. As mentioned before, the interaction between the molecules depends on
pressure, temperature, composition as well as stirrer speed Activation energy of
reaction is determined by using Arrhenius given below:

1 = 1

2 = 2

ln( 21)= [11 12]

1 and 2 stands for rate constants for given temperature

stands for activation energy activation energy
stands for universal gas constant
stands for pre-exponential factor

For a constant volume system, reaction rate of component i could be determined by

equation given below:
 1 1
= ()*( ) = ( )*( ) =

Where:
stands for rate of reaction
stands for volume of reaction medium
stands for number of moles
stands for elapsed time
stands for concentration of component

In order to determine the rate of reaction, there are two methods available .They are
integral and differential methods. Integral method is more appropriate for this
experiment and will be used in calculations .Because, as seen from the graphs and
tables given in the Results obtained from the apparatus are so scattered that it is
impossible reliably finding the derivatives needed in the differential method .When
using integral method, the order in the rate equation should be assumed . Then, the
equation is integrated for assumed order . Then, concentration function which is
determined by using guessed value of order versus time graphs is plotted. If any of
these graphs gives straight , then assumed order is the real order of the reaction . [2]

For first order reactions:

= =

0 =k0

0
ln =

For second order reactions:

= = kCi2

0 2 =k0

(0 )
(Ci Ci0) =

Reaction rate
concentration
stands for elapsed time
0 stands for initial concentration
stands for rate constant
 Note: the unit of rate constant is 1/ for 1st order and 3 / for second order. [3]

Apparatus and Experimental details

The unit shown in the picture is used to hold up the lab experiment. The unit contains a
stirred tank which has 2 liter volume. The reactor is supplied with an agitator which
mixes the reactants. An internal heat transfer coil is used in order to keep the reactor at
desired temperature. A thermocouple are used to determine temperature of reaction
medium. Moreover, the reactor is supplied with 4 baffles that help mixing. In order to
make precise calculations it is needed to keep temperature constant.

1.
The reactor is designed in such a way
to make reactions in batch mode. The
reactor can take 200 of material at any
one time and samples of 10ml should be
sufficient for the titration. Before stating the
experiment draw a flow diagram and
determine how the temperature can be
maintained. Some heating/cooling tests
have been done before starting the reaction
First of all, 0.1 reaction solutions are
prepared. Then, 100 of the poured
to the reactor and temperature is settled to
desired value. Then, 100ml of the Ethyl
Acetate is added .Samples are taken instantly from the reactor. A burette and
phenolphthalein indicator is used to determine volume of in sample. The color of
indicator is changed from clear to purple when the solution has an excess of .

Recorded data and Results

Table 1.Given and calculated data for 30 rpm stirring speed and 298 k average temperature

1/
Titrate (0/

Volume )
1/
/(
/ / / 1/
)
0 0 0.05 0 0 0.003188 0.000159
30 6.3 18.7 1.3 0.26 0.037 0.301 7.03 0.003198 0.000118
60 6.8 19 1.8 0.36 0.032 0.446 11.25 0.003215 0.000103
90 7.9 19.5 2.9 0.58 0.021 0.868 27.62 0.003239 0.000068
-
120 11.1 20.2 6.1 1.22 -0.011 #NUM! 0.003314 -3.7E-05
110.91
150 7 22.4 2 0.4 0.03 0.511 13.33 0.003397 0.000102
 -
180 11.2 24.8 6.2 1.24 -0.012 #NUM! 0.003452 -4.1E-05
103.33
240 8.9 26.4 3.9 0.78 0.011 1.514 70.91 0.003497 0.000039
300 8.4 27.7 3.4 0.68 0.016 1.139 42.5 0.003539 0.000057
360 9.4 28.9 4.4 0.88 0.006 2.12 146.67 0.003574 0.000021
420 9.7 29.9 4.7 0.94 0.003 2.813 313.33 0.003543 0.000011
480 10.4 29 5.4 1.08 -0.004 #NUM! -270 0.003511 -1.4E-05
-
540 10.7 28.1 5.7 1.14 -0.007 #NUM! 0.00345 -2.4E-05
162.86
600 10.5 26.2 5.5 1.1 -0.005 #NUM! -220 0.00343 -1.7E-05
660 10.2 25.8 5.2 1.04 -0.002 #NUM! -520 0.00343 -7E-06
720 9.1 25.8 4.1 0.82 0.009 1.715 91.11 0.00344 0.000031
780 9.2 26 4.2 0.84 0.008 1.833 105 0.0145 0.000116

Table 2. Given and calculated data for 30 rpm stirring speed and 315.3 K average temperature
.

Titrate (0/ 1/

Volume ) 1/
/(
/ / / 1/
)
0.000 0.050 0.000 0.000 0.002580 0.000129
30.000 5.400 37.900 0.400 0.080 0.046 0.083 1.739 0.003860 0.000178
60.000 6.400 37.800 1.400 0.280 0.036 0.329 7.778 0.003860 0.000139
90.000 6.900 38.300 1.900 0.380 0.031 0.478 12.258 0.003870 0.000120
120.000 7.200 38.700 2.200 0.440 0.028 0.580 15.714 0.003890 0.000109
150.000 7.600 39.400 2.600 0.520 0.024 0.734 21.667 0.003910 0.000094
180.000 8.500 40.200 3.500 0.700 0.015 1.204 46.667 0.003940 0.000059
240.000 8.100 41.000 3.100 0.620 0.019 0.968 32.632 0.003970 0.000076
300.000 8.600 41.500 3.600 0.720 0.014 1.273 51.429 0.003990 0.000056
360.000 9.900 42.300 4.900 0.980 0.001 3.912 980.000 0.004020 0.000004
420.000 8.700 43.200 3.700 0.740 0.013 1.347 56.923 0.004050 0.000053
480.000 9.400 44.500 4.400 0.880 0.006 2.120 146.667 0.004100 0.000025
540.000 9.500 45.000 4.500 0.900 0.005 2.303 180.000 0.004120 0.000021
600.000 9.500 45.500 4.500 0.900 0.005 2.303 180.000 0.004140 0.000021
660.000 9.900 45.700 4.900 0.980 0.001 3.912 980.000 0.004140 0.000004
720.000 9.700 46.600 4.700 0.940 0.003 2.813 313.333 0.004180 0.000013
780.000 9.500 46.700 4.500 0.900 0.005 2.303 180.000 0.004180 0.000021

Table 3. Given and calculated data for 30 rpm stirring speed and 333.7 Kaverage temperature

Titrate (0/ 1/

Volume ) 1/
/(
/ / / 1/
)
 0.000 0.050 0.000 0.000 0.002580 0.000129
30.000 6.600 42.100 1.600 0.320 0.030 0.390 9.410 0.004010 0.000136
60.000 6.200 46.700 1.200 0.240 0.040 0.270 6.320 0.004180 0.000159
90.000 6.700 52.900 1.700 0.340 0.030 0.420 10.300 0.004410 0.000146
120.000 7.000 55.000 2.000 0.400 0.030 0.510 13.330 0.004490 0.000135
150.000 7.400 59.400 2.400 0.480 0.030 0.650 18.460 0.004660 0.000121
180.000 8.100 62.600 3.100 0.620 0.020 0.970 32.630 0.004780 0.000091
240.000 8.500 65.900 3.500 0.700 0.020 1.200 46.670 0.004900 0.000074
300.000 8.900 67.400 3.900 0.780 0.010 1.510 70.910 0.004960 0.000055
360.000 8.900 68.200 3.900 0.780 0.010 1.510 70.910 0.004990 0.000055
420.000 8.900 68.300 3.900 0.780 0.010 1.510 70.910 0.005000 0.000055
480.000 9.700 67.600 4.700 0.940 0.000 2.810 313.330 0.004970 0.000015
540.000 10.000 67.100 5.000 1.000 0.000 #DIV/0! #DIV/0! 0.004950 0.000000
600.000 9.800 65.400 4.800 0.960 0.000 3.220 480.000 0.004890 0.000010
-
660.000 10.300 62.300 5.300 1.060 0.000 #NUM! -353.330 0.004770
0.000014
-
720.000 10.500 59.900 5.500 1.100 -0.010 #NUM! -220.000 0.004670
0.000023
780.000 9.800 58.200 4.800 0.960 0.000 3.220 480.000 0.004610 0.000009

Table 4. Given and calculated data for 50 rpm stirring speed and 299 K average temperature

Titrate (0/ 1/

Volume ) 1/
/(
/ / / 1/
)
0.000 0.000 0.000 0.050 0.000 0.000 0.002920 0.000146
30.000 6.800 22.600 1.800 0.360 0.032 0.446 11.250 0.002930 0.000094
60.000 6.600 22.700 1.600 0.320 0.034 0.386 9.410 0.002960 0.000101
90.000 7.000 23.000 2.000 0.400 0.030 0.511 13.330 0.003080 0.000092
120.000 8.100 24.200 3.100 0.620 0.019 0.968 32.630 0.003120 0.000059
150.000 7.100 24.600 2.100 0.420 0.029 0.545 14.480 0.003220 0.000093
180.000 7.700 25.600 2.700 0.540 0.023 0.777 23.480 0.003250 0.000075
240.000 7.900 25.900 2.900 0.580 0.021 0.868 27.620 0.003270 0.000069
300.000 9.800 26.100 4.800 0.960 0.002 3.219 480.000 0.003290 0.000007
360.000 9.000 26.300 4.000 0.800 0.010 1.609 80.000 0.003300 0.000033
420.000 8.600 26.400 3.600 0.720 0.014 1.273 51.430 0.003320 0.000046
480.000 8.800 26.500 3.800 0.760 0.012 1.427 63.330 0.003320 0.000040
540.000 9.700 26.500 4.700 0.940 0.003 2.813 313.330 0.003320 0.000010
600.000 9.100 26.500 4.100 0.820 0.009 1.715 91.110 0.003320 0.000030
660.000 9.100 26.500 4.100 0.820 0.009 1.715 91.110 0.003320 0.000030
720.000 9.200 26.500 4.200 0.840 0.008 1.833 105.000 0.003320 0.000027
780.000 9.100 26.500 4.100 0.820 0.009 1.715 91.110 0.325000 0.002920

Table 5. Given and calculated data for 50 rpm stirring speed and 320.1 K average temperature

Titrate 1/
(0/)
Volume converted 1/
NaOH
/(
/ / / 1/
)
0.000 0.000 0.050 0.000 0.000 0.0013 6.5E-05
30.000 6.000 34.100 1.000 0.200 0.040 0.223 5.000 0.00421 0.00017
60.000 6.500 37.400 1.500 0.300 0.035 0.357 8.571 0.00465 0.00016
90.000 7.300 39.800 2.300 0.460 0.027 0.616 17.037 0.00499 0.00014
120.000 7.600 42.000 2.600 0.520 0.024 0.734 21.667 0.00533 0.00013
150.000 8.100 44.300 3.100 0.620 0.019 0.968 32.632 0.00569 0.00011
180.000 8.200 45.500 3.200 0.640 0.018 1.022 35.556 0.00589 0.00011
240.000 8.400 48.000 3.400 0.680 0.016 1.139 42.500 0.00632 0.0001
300.000 8.700 49.800 3.700 0.740 0.013 1.347 56.923 0.00664 8.6E-05
360.000 9.000 50.600 4.000 0.800 0.010 1.609 80.000 0.00679 6.8E-05
420.000 9.200 51.200 4.200 0.840 0.008 1.833 105.000 0.00691 5.5E-05
480.000 9.100 51.600 4.100 0.820 0.009 1.715 91.111 0.00698 6.3E-05
540.000 9.500 51.600 4.500 0.900 0.005 2.303 180.000 0.00698 3.5E-05
600.000 9.300 51.600 4.300 0.860 0.007 1.966 122.857 0.00698 4.9E-05
660.000 8.900 51.500 3.900 0.780 0.011 1.514 70.909 0.00696 7.7E-05
720.000 9.200 51.300 4.200 0.840 0.008 1.833 105.000 0.00692 5.5E-05
780.000 9.200 51.100 4.200 0.840 0.008 1.833 105.000 0.00689 5.5E-05

Table 6. Given and calculated data for 50 rpm stirring speed and 333.9 Kaverage temperature

Titrate (0/ 1/

Volume ) 1/
/(
/ / / 1/
)
0.000 0.000 0.050 0.000 0.000 0.001302 0.000065
30.000 6.900 43.100 1.900 0.380 0.030 0.480 12.260 0.005497 0.000170
60.000 7.500 49.700 2.500 0.500 0.030 0.690 20.000 0.006625 0.000166
90.000 7.600 54.700 2.600 0.520 0.020 0.730 21.670 0.007593 0.000182
120.000 6.900 58.000 1.900 0.380 0.030 0.480 12.260 0.008289 0.000257
150.000 8.600 61.500 3.600 0.720 0.010 1.270 51.430 0.009080 0.000127
180.000 8.700 63.300 3.700 0.740 0.010 1.350 56.920 0.009509 0.000124
240.000 9.600 66.800 4.600 0.920 0.000 2.530 230.000 0.010387 0.000042
- -
300.000 10.100 68.400 5.100 1.020 0.000 #NUM!
1020.000 0.010808 0.000011
360.000 9.900 68.300 4.900 0.980 0.000 3.910 980.000 0.010782 0.000011
420.000 9.800 67.300 4.800 0.960 0.000 3.220 480.000 0.010517 0.000021
-
480.000 10.300 66.800 5.300 1.060 0.000 #NUM! -353.330
0.010387 0.000031
- -
540.000 10.100 66.000 5.100 1.020 0.000 #NUM!
1020.000 0.010181 0.000010
-
600.000 10.500 64.500 5.500 1.100 -0.010 #NUM! -220.000
0.009803 0.000049
-
660.000 10.400 58.300 5.400 1.080 0.000 #NUM! -270.000
0.008355 0.000033
-
720.000 10.600 57.800 5.600 1.120 -0.010 #NUM! -186.670
0.008245 0.000049
-
780.000 11.000 57.100 6.000 1.200 -0.010 #NUM! -120.000
0.008094 0.000081

Table 7. Given and calculated data for 100 rpm stirring speed and 298 K average temperature

Titrate (0/ 1/

Volume ) 1/
/(
/ / / 1/
)
0.000 0.000 0.000 0.050 0.000 0.000 0.002253 0.000113
30.000 6.200 18.300 1.200 0.240 0.038 0.274 6.320 0.002238 0.000085
60.000 5.800 18.100 0.800 0.160 0.042 0.174 3.810 0.002367 0.000099
90.000 6.400 19.800 1.400 0.280 0.036 0.329 7.780 0.002477 0.000089
120.000 6.500 21.200 1.500 0.300 0.035 0.357 8.570 0.002600 0.000091
150.000 7.100 22.700 2.100 0.420 0.029 0.545 14.480 0.002693 0.000078
180.000 7.100 23.800 2.100 0.420 0.029 0.545 14.480 0.002815 0.000082
240.000 7.700 25.200 2.700 0.540 0.023 0.777 23.480 0.002914 0.000067
300.000 8.400 26.300 3.400 0.680 0.016 1.139 42.500 0.002987 0.000048
360.000 8.500 27.100 3.500 0.700 0.015 1.204 46.670 0.003044 0.000046
420.000 8.800 27.700 3.800 0.760 0.012 1.427 63.330 0.003072 0.000037
480.000 8.700 28.000 3.700 0.740 0.013 1.347 56.920 0.003110 0.000040
540.000 9.200 28.400 4.200 0.840 0.008 1.833 105.000 0.003110 0.000025
600.000 9.300 28.400 4.300 0.860 0.007 1.966 122.860 0.003120 0.000022
660.000 9.200 28.500 4.200 0.840 0.008 1.833 105.000 0.003120 0.000025
720.000 9.700 28.500 4.700 0.940 0.003 2.813 313.330 0.003120 0.000009
780.000 9.300 28.500 4.300 0.860 0.007 1.966 122.860 0.251345 0.001759

Table 8. Given and calculated data for 100 rpm stirring speed and 312.8 K average
temperature
Titrate (0/ 1/

Volume ) 1/
/(
/ / / 1/
)
 0.000 0.050 0.000 0.000 0.001182 0.000059
30.000 5.700 30.600 0.700 0.140 0.043 0.151 3.256 0.003327 0.000143
60.000 5.800 33.400 0.800 0.160 0.042 0.174 3.810 0.003620 0.000152
90.000 6.500 34.700 1.500 0.300 0.035 0.357 8.571 0.003762 0.000132
120.000 7.000 36.500 2.000 0.400 0.030 0.511 13.333 0.003967 0.000119
150.000 6.900 37.700 1.900 0.380 0.031 0.478 12.258 0.004108 0.000127
180.000 7.700 39.100 2.700 0.540 0.023 0.777 23.478 0.004278 0.000098
240.000 8.300 40.700 3.300 0.660 0.017 1.079 38.824 0.004478 0.000076
300.000 8.700 41.600 3.700 0.740 0.013 1.347 56.923 0.004594 0.000060
360.000 8.700 42.300 3.700 0.740 0.013 1.347 56.923 0.004686 0.000061
420.000 8.600 42.500 3.600 0.720 0.014 1.273 51.429 0.004712 0.000066
480.000 9.200 42.600 4.200 0.840 0.008 1.833 105.000 0.004726 0.000038
540.000 8.600 42.700 3.600 0.720 0.014 1.273 51.429 0.004739 0.000066
600.000 9.000 42.600 4.000 0.800 0.010 1.609 80.000 0.004726 0.000047
660.000 8.600 42.500 3.600 0.720 0.014 1.273 51.429 0.004712 0.000066
720.000 9.600 42.400 4.600 0.920 0.004 2.526 230.000 0.004699 0.000019
780.000 9.000 42.300 4.000 0.800 0.010 1.609 80.000 0.004686 0.000047

Table 9. Given and calculated data for 100 rpm stirring speed and 334.1 K average
temperature

Titrate (0/ 1/

Volume ) 1/
/(
/ / / 1/
)
0.000 0.050 0.000 0.000 0.001182 0.000059
30.000 6.600 44.200 1.600 0.320 0.030 0.390 9.410 0.004942 0.000168
60.000 7.300 48.100 2.300 0.460 0.030 0.620 17.040 0.005502 0.000149
90.000 7.200 53.000 2.200 0.440 0.030 0.580 15.710 0.006273 0.000176
120.000 6.400 57.100 1.400 0.280 0.040 0.330 7.780 0.006980 0.000251
150.000 8.400 62.400 3.400 0.680 0.020 1.140 42.500 0.007982 0.000128
180.000 7.800 61.200 2.800 0.560 0.020 0.820 25.450 0.007746 0.000170
240.000 9.900 60.800 4.900 0.980 0.000 3.910 980.000 0.007669 0.000008
-
300.000 10.300 60.300 5.300 1.060 0.000 #NUM! -353.330
0.007573 0.000023
360.000 9.900 60.400 4.900 0.980 0.000 3.910 980.000 0.007592 0.000008
420.000 9.900 60.400 4.900 0.980 0.000 3.910 980.000 0.007592 0.000008
480.000 9.800 62.600 4.800 0.960 0.000 3.220 480.000 0.008022 0.000016
-
540.000 10.300 66.300 5.300 1.060 0.000 #NUM! -353.330
0.008787 0.000026
600.000 10.000 67.600 5.000 1.000 0.000 #DIV/0! #DIV/0! 0.008970 0.000000
660.000 9.900 70.100 4.900 0.980 0.000 3.910 980.000 0.009480 0.000009
-
720.000 11.100 72.000 6.100 1.220 -0.010 #NUM! -110.910 0.009890
0.000109
-
780.000 11.000 68.900 6.000 1.200 -0.010 #NUM! -120.000 0.009230
0.000092
Plot 1. Ln (Ci0/Ci) versus time for first order reaction with 30 rpm stirring speed

4.500

4.000 y = 0.0047x
R = 0.9341
3.500
y = 0.0044x
3.000 R = 0.6519
Ln(Ca0/Ca)

2.500 y = 0.0034x
R = 0.3638
2.000
T=315.7 K ave
1.500

1.000 T=333.7 K

0.500
T=298K
0.000
0 200 400 600 800 1000
time (s)

Plot 2. 1/Ca-1/Ca0 versus time for second order reaction with 30 rpm stirring speed

1200.00
y = 0.5261x
R = 0.7485
1000.00
y = 0.5717x
800.00 R = 0.2391
1/Ca-1/Ca0

y = 0.2272x
600.00 R = 0.2479

T=298K
400.00 ave
T=315.3 K
200.00 ave
T=333.7 K
0.00
0 200 400 600 800 1000
time (s)
Plot 3. Ln (Ci0/Ci) versus time for first order reaction with 50 rpm stirring speed

4.500
y = 0.0089x
R = 0.9086
4.000

3.500 y = 0.0032x
R = 0.6117
3.000 y = 0.0033x
R = 0.3167
Ln(Ca0/Ca)

2.500

2.000

T=299
1.500 ave

1.000 T=320.1
K ave
0.500
T=333.9
0.000 K
0 200 400 600 800 1000
time (s)

Plot 4. 1/Ca-1/Ca0 versus time for second order reaction with 50 rpm stirring speed

1200.00

y = 1.4199x
1000.00 R = 0.6095

y = 0.1796x
800.00
R = 0.6896
1/Ca-1/Ca0

600.00 y = 0.23x
R = 0.1363

400.00
T=299K ave

200.00
T=320.1K ave

0.00
0 200 400 600 800 1000 T=333.9 K

time (s)
Plot 5. . Ln (Ci0/Ci) versus time for first order reaction with 100 rpm stirring speed

6.000

y = 0.0077x
5.000
R = 0.7344
y = 0.0028x
4.000 R = 0.7512
Ln(Ca0/Ca)

y = 0.003x
3.000 R = 0.9482

T=298K
2.000 ave

T=312.8K
1.000 ave

334.1
0.000
0 200 400 600 800 1000
time (s)

Plot 6. 1/Ca-1/Ca0 versus time for second order reaction with 50 rpm stirring speed

1200.00 y = 1.7017x
R = 0.6392
1000.00 y = 0.1562x
R = 0.5763
800.00 y = 0.2071x
1/Ca-1/Ca0

R = 0.6395
600.00
T=298K ave
400.00
T=312.8K ave
200.00
T=334.1 K
0.00
0 200 400 600 800 1000
time (s)
Discussion

Key purpose of this lab experiment is investigation of chemical reaction between

and . As they reacts in the batch reactor, sample was taken and certain
amount of solution is added in order to stop conversion of. Then the mixture
is titrated in order to obtain better reaction between these reagents. Phenolphthalein
indicator is used to determine the time when all has been reacted with . The
experiment has been done in three run with different stirrer speed .Moreover, for each
run there are three try with different temperatures and obtained values is shown in the
tables given above. The temperature of the medium should kept constant .However, as
it is shown in the tables, temperature of the medium changes as the reaction proceeds.
The main reason behind that is the reaction is endothermic and some amount of heat is
absorbed by reaction resulting in temperature change .In calculations, average
temperatures were taken in order to make more precise calculations. As seen from the
tables, titrate volume increases as the reaction continues. However, as seen from the
tables for some time increments titrate volume exceeds 10 which is given ion red
colors in the tables. It shows there are some inaccuracies associated with experiments
and these obtained results is excluded while plotting the graph and as seen from the
tables in some cases it gives more conversion more than one which is impossible. The
purpose of the experiment is determination of concentration of for each given
time. The initial concentration and titrate volume are available. As seen from the table
conversion of the reactants approaches to one as the reaction proceeds. Initial
concentration of and its concentration at specified time is used in first order
rate equations and second order rate equation and the obtained value versus time
graphs are constructed in order to determine order of reaction properly. In each graph,
there are three different line and each of these lines is appropriate to different average
temperature but the same stirring speed The order of reaction are determined by help
of R-squared value of the lines . By comparing R-square values of first order plot with
the second order graph, the proper order could be defined. For instance, if R-square
values of first order plot is higher than the second order graph this means the reaction is
first order or vice versa. Actually, comparing R-Square value at one temperature with
other R-square value at the same temperature is enough .However, for the 50
stirrer speed and 320.1 K average temperature when comparing R-square values it
seems the reaction is second order. However, for the same reaction in other two
average temperatures, the reaction is first order, so it is first order reaction. To sum up,
the reaction is first order with respect to .
 In order to determine activation energies of the Figure 2. Molecules distribution
reactions for each of given stirrer speed frequency curve with kinetic energy [6]
factor and the rate constants for at least two
temperature should be available .Actually, it is more
proper to use rate constants at maximum and
minimum temperatures. However, I have use
maximum and minimum rate constants in
calculations .Because, rate constant should get
maximum value at maximum temperature or vice
versa. However, due to experimental inaccuracies,
rate constants doesnt follow this trend. When
comparing the tables of different stirring speed for
the same temperature, it is obvious that as the
stirrer speed increase the conversion of the
components increase and the time to reach a
certain concentration decrease. It is known
theoretically that as stirring speed increase, the activation energy must decrease. The
main reason behind that is as the stirrer speed increase ,the molecules gets more
kinetic energy so, the molecules finds enough energy to break the energy barrier as
shown in the figure 2 [1]. However, as seen from table Table 10 activation energy for
30 stirrer speed is lowest among other. The main reason for this deviation may be
experimental inaccuracies.

Conclusion

Saponification reaction between and is carried out in this experiment by

using a batch reactor which is stirred by help of agitator .The reaction medium is
prepared by following information given in the lab manual . In order to investigate effect
of stirrer speed on rate of reaction the reaction is carried out for 3 different stirrer
speed. Moreover for each stirrer speed the reaction is carried out for three different
temperature. Titration technique is used for determination of concentration of .
Main purpose of this lab experiment was determination of order and rate of reaction
properly. So, in this way, activation energy and frequency factor should be determined
initially. Their values are determined by plotting the graphs given in the Results part. As
discussed in the Discussion part, there are some inaccuracies related to this experiment
which is inevitable in lab experiments and inherent for this type of experiments. The
main reason of inaccuracies was the temperature. It is obvious that the rate of reaction
depends on both temperature and stirrer speed. Stirrer speed is changed in order to see
the relation between the reaction rate and stirrer speed. However, there was
fluctuations in the temperature, so as seen from the results in some cases the reaction
rate for reaction with high stirrer speed is lower than reaction rate for low stirrer speed.
The other reason of inaccuracies is human factor. In this experiment, there was some
parts such as adding solutions to the bruttle has been done by us and there may be
some inaccuracies. To conclude, the experiment was done successfully despite some e
References
1. , . 256
259. . , 2006.
2. . , , 3 . 2005 70 123
3. , , , 3 , 1999
. Page 38 -60.
4. ( )
5. http://khartoumspace.uofk.edu:8080/bitstream/handle/123456789/10162/Saponifi
cation%20A%20Comparative%20Kinetic.pdf?sequence=1&isAllowed=y
6. http://www.dummies.com/education/science/chemistry/what-factors-affect-the-
speed-of-chemical-reactions/
7.