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Contents

ABSTRACT ................................................................................................................................................. 2
NOMENCLATURE ..................................................................................................................................... 3
1.0 INTRODUCTION ................................................................................................................................. 4
2.0 THEORY ............................................................................................................................................... 6
3.0 MATERIALS AND METHODS........................................................................................................... 8
3.1 EXPERIMENTAL PROCEDURE .................................................................................................. 8
3.2 APPARATUS.................................................................................................................................... 9
3.2 MODEL DEVELOPMENT ............................................................................................................ 13
3.3 MATERIAL BALANCE .................................................................................................................. 13
3.4 ENERGY BALANCE ..................................................................................................................... 14
4.0 RESULTS ........................................................................................................................................... 16
4.1 EXPERIMENTAL RESULTS........................................................................................................ 16
5.0 DISCUSSION ..................................................................................................................................... 17
6.0 CONCLUSION ................................................................................................................................... 18
7.0 REFERENCES................................................................................................................................... 19
8.0 APPENDICES .................................................................................................................................... 22
8.1 SAMPLE OF CALCULATIONS ................................................................................................... 22
8.2 GRAPHS ......................................................................................................................................... 27
8.3 RAW DATA ..................................................................................................................................... 30

ABSTRACT
The kinetics of the reactions of acetic anhydride-excess water has been studied at
temperatures above 30 degrees of the reactants to avoid a longer duration of the experiment. The
experiment was carried under adiabatic conditions in a thermos-flask fitted with a negative
coefficient thermistor and kinetic data reported in this work. Also data logging was chosen at 15
seconds as the interval between samples and 1500 seconds as the total running time of the
experiment. The key ultimatum was to observe the trend of the temperature immediately after
adding 25 ml of 0.5 M sulphuric acid as a catalyst. The same techniques were applied for the
kinetic studies of excess acetic anhydride-water reactions at temperatures of up to 55 degrees.
The reaction kinetics of excess acetic anhydride-water reactions which has not been determined
previously was modeled using the same adiabatic analysis and the average activation energy,
heat of reaction, pre-exponential factor and the order of reaction with respect to water has been
determined. The studies have shown that the two processes appear to be completely different
and might proceed through different reaction mechanisms pathways for the production of acetic
acid.

The kinetics of the reactions acetic anhydride-excess water, excess acetic anhydridewater has been modeled as a function of temperature in an adiabatic batch reactor (thermosflask) using a negative coefficient thermistor as a measuring device. The results has shown that
the acetic anhydride-excess water process at 1: 10 mole ratio the process remains first order at
moderate temperatures of up to 55 degrees with the activation energy similar to that reported at
25 degrees.
Excess acetic anhydride-water reactions which have no literature information on its
kinetics were shown to follow a first order kinetics with respect to the water. The activation energy
for all experimental analysis were determined to be approximately 47112.67 J/mol, 50623.9 J/mol
and 52037.33 J/mol. The heat of reaction which was assumed to be independent of temperature
for the excess acetic anhydride/water is approximately. The heat of mixing was assumed
negligible and was not considered in the heat of reaction calculations.

NOMENCLATURE
Symbol

Definition

Concentration of ions in solution (mol/dm3)

Concentration of acetic anhydride (mol/dm3)

Concentration of acetic anhydride (mol/dm3)

, ,

Specific heat capacities of acetic anhydride, acetic acid


and water respectively (kJ/kg)
Mass of acetic anhydride, acetic acid and water
respectively (kg)
Acid dissociation constant

Reaction rate constant (min-1)

, ,

Conversion of acetic anhydride to acetic acid

Rate of reaction (mol/ dm3.min)

Reaction temperature (oC)

Heat of reaction (J/mol)

Molar conductivity (Sm2 mol-1)

Molar conductivity at infinite dilution (Sm2 mol-1)

Fraction of ions present in solution

1.0 INTRODUCTION
Recent studies integrated in laboratory prove that in trying to understand the
dynamic behavior of chemical processes involving reactions, it is important to have
complete information on the kinetics of the process. Understanding the kinetics of a
reaction involves having a model of the reaction and the corresponding reaction
parameters. This is important because if the kinetics of a reaction is not fully understood,
several problems may arise, such as ineffective reaction control, unsafe conditions and
runaway reactions which can lead to equipment damage, explosion and the release of
toxic substances into the environment. For a majority of reactions, there is hardly any
information regarding the kinetics, thermodynamics, and physical parameters that
characterize such reactions which is rather inauspicious.
The hydrolysis of acetic anhydride to produce acetic acid is a fast exothermic
reaction. This is an important reaction needed for the synthesis of an equally important
chemical (acetic acid) hence the need for information about the progress of the reaction
such as kinetic and thermodynamic parameters. The kinetics of acetic anhydride
hydrolysis to acetic acid has been studied with a number of techniques for measuring
reaction rate reported in literature. (Ampelli et al, 2003) integrated an ultraviolet-visible
(UV-Vis) spectrometer with an isoperibolic reaction calorimeter to study the kinetics of
hydrolysis of acetic anhydride. An acidbase indicator was added to the reaction mixture
and the change of its color as the reaction progressed was followed by the UVVis
spectrometer. (Haji & Erkey), developed a reaction set up that employed in-situ Fourier.
Transform Infrared Spectroscopy (FTIR) to monitor the kinetics of acetic anhydride
hydrolysis to acetic acid. (Kralj et al., 1992) investigated the kinetics of acetic acid
production from the hydrolysis of acetic anhydride. She estimated kinetic parameters
such as reaction rate constant activation energy, and order of reaction by measuring the
conductivity of a weak electrolyte (acetic acid). (Hirota et al, 1996) used calorimetric
techniques to study the hydrolysis of acetic anhydride in an adiabatic reaction vessel by
estimating kinetic and thermodynamic parameters such as reaction rate constant
activation energy, and heat transfer coefficient. In view of the foregoing, it can be seen
that most of the techniques used for studying the kinetics of acetic anhydride hydrolysis

reported in the literature involve the collection of experimental data from colorimetric,
calorimetric, titration, conductivity and spectroscopy experiments and the data is
subsequently subjected to differential or integral method of analysis to determine the
kinetic parameters. In spite of these experimental efforts aimed at determining the kinetics
of the hydrolysis process, very little work has been done in modelling the process.
Mathematical modelling of the hydrolysis process enables its representation in a
mathematical sense. Dynamic simulation of the formulated model can be utilized in
analyzing the behavior of the process, provision of insights into the mechanisms that drive
the process, understanding the response of the process to changes in operating
conditions, design of controllers and design of entirely new processes thereby leading to
vast improvements in process economics, design, operation and control.
Model predictions make it possible to identify optimal design and operational
parameters and this consequently leads to the maximization of the systems performance.
The aim of this work is to estimate the kinetic parameters for the hydrolysis of acetic
anhydride to acetic acid in an adiabatic batch reactor. A dynamic model of the process
was developed and the kinetic parameters were estimated in the process of validating the
model.

2.0 THEORY

The hydrolysis of acetic anhydride in water, in the presence of a catalyst (Sulphuric


acid) is described by:
(3 )2 + 2 23

This reaction can be assumed to have simple power law kinetics of the form

The concentration of the protonic acid remains constant for the duration of the run
and thus K is a catalytic rate constant that includes this concentration, also in power law
form. For any system of this particular type, the instantaneous value of the acetic
anhydride concentration cab be eliminated between the material and thermal balance
equations to give a linear equation. Use of this equation requires that values of the
gradient of temperature with respect to time be found.
If the concentration of acetic anhydride at any time t is C, then the rate of the reaction is
given by:
=

= 0 At = 0
The heat generation rate is:

(). =

= 0 At = 0
Substituting into the first equation into the above equation, and integrating with respect to time
and using the boundary conditions we obtain:

( 0 )
(0 ) () =
For the n-th order case, the rate may be expressed in Arrhenius form:

= = .

Using =

and rearranging, the equation results in;

= 0 ( 0 )
Using = when the reaction is complete gives:
(0 0) = ( 0 ) And thus =

Substitution for in equation (5) and rearranging, we have:

0
[0 ( 0 )]
0

= .

Taking logarithms of both sides of this equation gives:

ln|| = ln|| -
And so plot of ln (LHS) versus 1/T should be linear with an intercept of ln (A) and gradient of
E/R.

3.0 MATERIALS AND METHODS


The equipment used for the experiments was a batch reactor integrated with a
conductivity meter graduated in milli Siemens. 500 cm3 of distilled water was measured
and poured into the reactor.
Forty (40) cm3 of acetic anhydride was then dispensed into the reactor using a
syringe. The mains of the reactor were then connected and initial temperature and
conductivity measurements were recorded. Sixteen (16) conductivity measurements
were recorded at different times for 16 steps in the experiment.

3.1 EXPERIMENTAL PROCEDURE

Ensure that the reactor has been set up with the special temperature sensor and
computer interface for the adiabatic reaction as described in the installation
section.

If possible the reactants should be at approximately 30 degrees before mixing. If


they are cooler than this, the reaction will take much longer time to complete.

Charge the reactor with 100 mL of acetic anhydride and 250 mL of demineralized
water.

Start the reactor agitator and adjust the variable speed drive to position 5.0

Add 150 mL of glacial acetic acid (since the water and acetic anhydride are
mutually insoluble, but are both soluble in acetic acid, this ensures that the
reaction mixture is homogeneous-the acetic acid does not form part of the
reaction).

Start the data logging program choosing 15 seconds as the interval between
samples and 1500 seconds as the total running time of the experiment (a longer
duration will be required if the temperature of the reactants is less than 30
degrees). It is essential to log data until the temperature in the reactor begins to
fall again.

Immediately add 25ml of 0.5M sulphuric acid as a catalyst. The reaction will
commence.

Switch off the agitator.

When the reaction has completed, the temperature data can be viewed within
software, either in tabular or graphical format.

The data should be saved as an excel file .It is then possible to carry out the
second part of analysis described above by calculating the terms of equation (6),
and plotting the graph.

In order to find dT/dt, it will be necessary to extract the linear region of data from
a graph of temperature versus time for the experiment. This will entail discarding
the first few points and also any points after the temperature reaches the peak
value.

Repeat the experiment (described above) using different quantities of sulphuric


acid catalyst (e.g. 15ml to 40ml in 5ml increments).

3.2 APPARATUS

Figure 1: Batch Reactor (Thermo-flask)

Figure 2: Schematic System design

Figure 3: Reactor connection

Figure 4: Schematic Drawing of Batch Reactor

Figure 5: Cooling water supply connection

The conductivity measurements recorded were converted to concentration values


by relating it to the conductivity of the solution as shown in Equation (1) (see Table 1).
The conductivity measurements recorded were converted to concentration values by
relating it to the conductivity of the solution as shown in
Equation (1) (see Table 1).
=

Where:
is the molar conductivity of the solution. The molar concentration of the electrolyte c
is expressed in terms of the acid dissociation constant as follows:

(1)
2

The fraction of ion present in the solution is given as:


=

(+
)

Where:
is the molar conductivity at infinite dilution. The values and are reasonably
constant at the initial temperature of the reaction. They are respectively 39.1 Sm2 mol-1
and 1.810-5

3.2 MODEL DEVELOPMENT


The liquid phase hydrolysis reaction of acetic anhydride to produce acetic acid was
carried out in a constant volume adiabatic batch reactor whose schematic is shown in
Figure 1. The reaction is exothermic and proceeds according to the following
stoichiometry:
(3 )2 + 2 23 +

In formulating the model, the following assumptions were made:

The volume of the reactor is fixed

No nuclear reaction occurs; hence rate of material generation is zero.

The content of the reactor is perfectly mixed (lumped system).

The implication of the last assumption is that all intensive properties of the stream leaving
the reactor system are identical to those inside the system.
The reactor model was obtained from material and energy conservation laws applied to
the reactor.

3.3 MATERIAL BALANCE

The equations describing the material balance of acetic anhydride and acetic acid in the
reactor are given as:

= 2

Fractional conversion of acetic anhydride to acetic acid is given as:

The rate of the hydrolysis reaction is described by the following equation:


=

3.4 ENERGY BALANCE


The equation describing the energy balance of the reactor obtained from applying the law
of conservation of energy to the reactor is given as:

[ ]

= ( )

The Equation can be expanded to obtain:


[ + + ]

= ( )

And are the moles and molar specific heat capacities of the chemical species in
the reactor. (J/mol) is the heat of reaction. The reactor model is described by the
system of equations which is a set of non-linear differential and algebraic equations
(DAEs) and describes the dynamic behavior of the concentration of all chemical species
present in the batch reactor and the temperature profile of the reactor content.

Figure 6: Reactor Model

Figure 1: Schematic of adiabatic batch reactor with variables

4.0 RESULTS
4.1 EXPERIMENTAL RESULTS

30 ml

ln = ln
(mol/s)
14.61

A (Pre-exponential
factor)
2.21 106

E (ACTIVATION
ENERGY) (J/mole)
47112.67

35 ml

16.24

1.13 107

50623.9

45 ml

15.78

7.13 106

52037.326

VOLUME

5666.67
1 () = 2.21 106 (
)

2 () = 1.13 107 (

6089
)

3 () = 7.13 106 (

6259
)

The reaction order was determined to be first order for all experimental analysis, 30, 35 and 45
ml.

=
The rate information obtained from the concentration-time plot enabled one to calculated specific
rate constant k (T) of the processes at any time (t) and temperature (T). Arrhenius plots was thus
generated from which kinetic parameters of runs were extracted. The values obtained for the
specific rate constants as a function of temperature

5.0 DISCUSSION
With the objective set forth, the experimental results in the hydrolysis of acetic anhydride
to acetic acid in an adiabatic batch reactor studied showed that there is a strong relationship that
exists between reaction rates and changes in temperature for exothermic reactions as stated in
the literature. The reactions between excess water and acetic anhydride thus hydrolysis reactions
was carried out at 40 to 55 degrees Celsius. The extent of the reactions was followed by
monitoring the changes in temperature in the reaction vessel (thermos-flask). The experimental
and the adiabatic curves are shown in Figures. The profiles of experimental and adiabatic curves
are shown in Figures respectively. The experimental reaction profiles (Hydrolysis of acetic
anhydride to acetic acid in an adiabatic batch reactor, shows that hydrolysis Acetic Anhydride to
acetic acid is a success. This can be observed from the set graphs plotted and the reaction rate
calculated and also the rate constant. On the other hand, another interesting finding was the
cooling parts of the process. Hydrolysis-Acetic Anhydride, showed very gradual cooling, this
however showed that after a certain period of time the reaction reached equilibrium and became
constant producing a straight horizontal slope in the graph of temperature versus time.
There may be several possible explanations to these observations. A possible explanation for this
might be that the rate of heat loss during the cooling processes is higher for hydrolysis-Acetic
Anhydride to Acetic Acid. The observed differences discussed is however very significant. The
reaction order for all the hydrolysis - experiments were first order with respect to the acetic
anhydride. This is shown in the rate-concentration plots in the Figures 6-8. This result is consistent
with other researchers Kralj and Haji et al.
The rate law temperature dependence were satisfactorily correlated by means of the
Arrhenius function for the hydrolysis- Anhydride to Acetic Acid. Graphs shows the Arrhenius plots
of the hydrolysis- Anhydride to Acetic Acid. From the plots the values of the activation energies
and pre-exponential factors were determined as shown in the equations mentioned under theory.
Similarities of the activation energies (47112.67 J/mol, 50623.9 J/mol and 52037.33 J/mol) which
agrees very well with what is reported by Haji and Kralj. The average activation energy reported
in the literature is 50623.9 J/mol, Haji which differs by + 0.65% from the average value reported
in this work.

6.0 CONCLUSION
The use batch reactor for the following the hydrolysis pf acetic anhydride reaction has
been demonstrated. The analysis of the batch reactor data showed that the hydrolysis of acetic
anhydride is a pseudo-first-order reaction. The rate constants were calculated from the batch data
using both integral and differential methods of analysis and were used to predict the performance
of a semi batch reactor. Predicted acetic anhydride n acetic acid concentrations. We as the
students found this laboratory experience good opportunity to implement many of the concepts
we have learned from the experiment.
The fastest reaction occurs when adiabatic batch rector was launched at 30oC. This is
expected because the higher temperature allows for the rate of reaction to increase faster. The
lower temperature is expected to provide the slowest reaction. Regardless of the temperature
started at reaction will release enough heat to increase the temperature. This shows that the rate
of the reaction is irrelevant regarding the total release of heat, and the total heat released will be
equal regardless of the temperature the reaction is started in.
Recommendations for the future projects would be to resolve the hydrolysis of acetic
anhydrate using Heuns method, instead of Eulers. This will provide more accurate results
compared to that of Eulers method Eulers. This will provide more accurate results compared to
that Eulers method. Additionally, one could possibly increase the initial concentration of acetic
anhydride in the reactor to see if the reaction constant will plateau after a certain amount of time.

7.0 REFERENCES
1. Fogler, H.S. Elements of Chemical Reaction Engineering 4th ed., Prentice Hall,
Upper Saddle River, New Jersey, 2006.
2. Levenspiel, O.Chemical Reaction Engineering 3rd ed., John Wiley & Sons, Inc.,
New York, 1999.
3. Froment, G.F., Bischoff, K.B. and De Wilde, J. Chemical reactor analysis and
design 3rd ed.,John Wiley & Sons, Inc., New York, 2011
4. Smith, J.M.Chemical Engineering Kinetics 3rd ed., McGraw-Hill Inc., New York,
1981.
5. Hirota, W.H., Rodrigues, R B., Sayer, C. and Guidi, R. "Hydrolysis of acetic
anhydride: Non-adiabatic calorimetric determination of kinetics and heat
exchange". Chemical Engineering Science, Vol. 65, 2010, pp.38493858.
6. Asprey, S.P., Wojciechowski, B.W., Rice, N.M. and Dorcas, A. "Applications of
temperature scanning in kinetic investigations: the hydrolysis of acetic anhydride".
Chemical Engineering Science, Vol. 51, Number 20, 1996, pp.46814692.
7. Ampelli, C., Di Bella, D., Lister, D.G., Maschio, G. and Parisi, J. "The Integration
of an Ultraviolet-Visible Spectrometer and a Reaction Calorimeter". Journal of
Thermal Analysis and Calorimetry, Vol. 72, 2003, pp.875883.
8. Haji, S. and Erkey, C. "Kinetics of hydrolysis of acetic anhydride by in-situ FTIR
spectroscopy. An experiment for the undergraduate laboratory". Chemical
Engineering Education, Vol. 39, Number 1, 2005, pp.5661.
9. Kralj, A.K. "Checking the kinetics of acetic acid production by measuring the
conductivity". Journal of Industrial and Engineering Chemistry, Vol. 13, Number 4,
2007, pp.631636.
10. Ampelli, C., Di Bella, D., Lister, D.G., and Maschio "Fitting isoperibolic calorimeter
data for reactions with pseudo-first order chemical kinetics". Journal of Thermal
Analysis and Calorimetry, Vol. 79, 2005, pp.8994.
11. Susanne, F., Smith, D. S., and Codina, A. "Kinetic Understanding Using NMR
Reaction Profiling". Organic Process Research & Development, Vol. 16, Number
1, 2011, pp. 61-64.

12. Wiseman, F.L. "New insight on an old reaction the aqueous hydrolysis of acetic
anhydride". Journal of Physical Organic Chemistry, Vol. 25, Number 12, 2012, p.
1105.
13. Assirelli, M., Xu, W., and Chew, W. "Reactor kinetics studies via process Raman
spectroscopy, multivariate chemo metrics, and kinetics modeling". Organic
Process Research & Development, Vol. 15, Number 3, 2011, pp. 610-621.
14. Zogg, A., Fischer, U. & Hungerbuhler, K. "A new approach for a combined
evaluation of calorimetric and online infrared data to identify kinetic and
thermodynamic parameters of a chemical reaction". Chemometrics and Intelligent
Laboratory Systems, Vol. 71, Number 2, 2004, pp.165176.
15. Suja M.R. and Thyagarajan, T. "Modelling of continuous stirred tank reactor using
artificial intelligence techniques". International journal of simulation modelling, Vol.
8, Number 3, 2009, pp. 145155.
16. Amenaghawon, N.A. and Obahiagbon, K.O. "Computer Simulation of Complex
Reactions in a Non-Isothermal Continuous Stirred Tank Reactor". Advances in
Agriculture, Sciences and Engineering Research, Vol. 2, Number 8, 2012, pp. 318327 Andres, H., Hu, Z., Snowling, S., and Schraa, O. "Model-Based Optimum
Design of Sequencing Batch Reactors for COD and Nitrogen Removal from a
Slaughterhouse Wastewater". Proceedings of the Water Environment Federation,
Vol. 20, Number 7, 2006, pp. 5100-5107
17. Brown, L. and Holme, T. Chemistry for Engineering Students, 2nd ed., Brooks
Cole, 2010.
18. Luyben, W.L. Process Modelling, Simulation and Control for Chemical Engineers.
2nd ed., McGraw- Hill Inc., New York, 1996.
19. Pantelides, C.C. The mathematical modelling of the dynamic behavior of process
systems, Centre for Process Systems Engineering, Imperial College London,
2003.
20. Van Ness, H.C., Smith, J.M. & Abbot, M.M. Introduction to Chemical Engineering
Thermodynamics 6th ed., McGraw-Hill Inc., New York, 2001.

21. Shatynski, J.J. and Hanesian, D. "Adiabatic kinetic studies of the cytidine/acetic
anhydride reaction by utilizing temperature versus time data". Industrial &
engineering chemistry research, Vol. 32, Number 4, 1993, pp.594599.

8.0 APPENDICES
8.1 SAMPLE OF CALCULATIONS
Table: Densities at room at temperature
Species
Acetic Anhydride
Water
Acetic acid

Molecular weight (Kg/kmol)


102.09
18
60.05

Volumes in m3
0.00025
0.00010
0

Density (Kg/m3)
1087
998.3
1049

30 ml
Temperature vs time was plotted for the raw data collected as seen in figure 222. The gradient
from the linear part of the graph will give the value of temperature change with time.

From the graph, the two points were collected:


2 1
=
2 1
2 1
47 43.9
=
=
= 0.034 /
2 1 420 330

The reaction order was found to be first order and there for n = 1 (graph 2222)

Finding gradient

The equation below was plotted on a graph assuming n = 1.

= .

0
[0 ( 0 )]
0

( 0 )
0
0 [0 0 ]

= .

Logarithms of both sides of this equation were taken and plotted:

ln|| = ln|| -

A plot of ln (LHS) versus 1/T was done with y-intercept being = ln A and a gradient of -

ln|| = ln|| -
2 1
=

2 1
=

2 1
=

2 1

3.2 + 1.5
=

0.0032 0.0029

= 5666.67

= () = 8.314 (5666.67)
= 47112.67
ln|| = ln|| -

5666.67

To get A, pre-exponential factor. Let T = 0


There the equation is reduced to ln|| = ln||
When T= 0
= = 14.61
= 14.61 = 2.21 106
The equation for the graph then becomes:
5666.67
1 () = 2.21 106 (
)

For 35 ml
2 1
=
= 0.034 /
2 1
2 1
=
=

2 1
= () = 8.314 (6089) = 50623.9
ln|| = ln|| -

6089

ln = ln = 16.24
When T= 0

6089

ln|| = 16.24 -

= 16.24 = 1.13 107


2 () = 1.13 107 (

6089
)

For 45 ml
Equation was found to be
= () = 8.314 (6259)
= 52037.326

ln|| = 15.78 -

6259

= 15.78 = 7.13 106


3 () = 7.13 106 (

6259
)

Rates of reactions

=
= 8.525 106 /3

T = 325.95 K at equilibrium temperature.

= 2.21 106

47112.67
)
8.314325.95

8.525 106

= 5.307 107 /3
Determining the reaction order involved iteration of nth power. First assumption was made to be
zero order. This assumption was used in the derived equations for respective assumptions e.g.

1st order, zero order and 2nd order reactions. These plots were used to determine the values of k
for runs at various temperatures and used to determine the activation energy.
Zero Order
N=0

= =

At t = 0,

=
1st order
N=1

= =

At t = 0

ln (
) =

2nd order

= = 2

At t = 0,

=
1
1

All the above correlations when applied to plot a graph results in a linear graph.
Then if the data collected do not fall on a straight line for n = 0, 1, 2, then we should stop guessing
reaction orders and proceed to either the differential method of analysis or to regression.
Differential Method
Taking the natural log

= =

ln (

) = ln + ln

The reaction order can be found from a ln-ln plot of:


(

In order to determine the value of K in the equation

determined using the coordinates of the ln (

= = , the gradient was first

vs time graph. The slope of this graph was linear,

by using a line of best fit the closest points or coordinates were chosen to calculate the gradient.
1 =
1 =

2 1
2 1

0.1657 0.0441
285 60

1 = 4.52 104
Therefore the value of 1 is found to be 4.52 104

2 =
2 =

2 1
2 1

0.064 0.0164
195 45

2 = 3.34 104

3 =
3 =

2 1
2 1

0.0324 0.0311
105 95

3 = 1.5 104

15
60
105
150
195
240
285
330
375
420
465
510
555
600
645
690
735
780
825
870
915
960
1005
1050

Conductivity (mS)

15
45
75
105
135
165
195
225
255
285
315
345
375
405
435
465
495
525
555
585
615
645
675
705
735
765
795
825
855
885
915
945
975
1005
1035
1065

Temperature (oC)

8.2 GRAPHS

30 ml H2SO4
Ln (LHS) vs 1/T

Temperature vs Time

60.00

50.00

40.00

30.00

20.00

10.00

0.00

Time (s)

Conductivity Variation

1.5

1.4

1.3

1.2

1.1

Time (s)

15
60
105
150
195
240
285
330
375
420
465
510
555
600
645
690
735
780
825
870
915
960
1005
1050

Conductivity (mS)

15
45
75
105
135
165
195
225
255
285
315
345
375
405
435
465
495
525
555
585
615
645
675
705
735
765
795
825
855
885
915
945
975
1005
1035
1065

Temperature (oC)

35 ml H2SO4

Ln (LHS) vs 1/T

Temperature vs Time

60

50

40

30

20

10

Time (s)

Conductivity vs Time

1.50

1.40

1.30

1.20

1.10

1.00

Time (s)

45 ml H2SO4
Ln (LHS) vs 1/T

Temperature vs time
50
40
30
20
10
0

15
45
75
105
135
165
195
225
255
285
315
345
375
405
435
465
495
525
555
585
615
645
675
705
735
765
795
825
855
885
915
945
975
1005
1035
1065

Temperature (oC)

60

Time (s)

conductivity vs time
1.6

1.4
1.2
1
0.8
0.6
0.4
0.2
0
0

200

400

600

800

1000

8.3 RAW DATA


Stirrer Speed:

Rpm

Reagent Mixture:

38

Acetic Anhydride

100

mL

Glacial Acetic Acid

150

mL

H2O

250

mL

H2SO4 (27.18) solution

30

mL

30 ml Sulphuric Acid (catalyst)


Time (s)

T (KELVINS)

15
30
45
60
75
90
105
120
135
150
165
180
195
210
225
240
255
270
285
300
315
330
345
360

31.2
32.6
33.3
34
34.7
35.2
35.8
36.2
36.7
37.2
37.7
38.2
38.8
39.3
39.9
40.4
40.9
41.6
42.2
42.7
43.3
43.9
44.4
44.9

Temperature
(oC)
304.35
305.75
306.45
307.15
307.85
308.35
308.95
309.35
309.85
310.35
310.85
311.35
311.95
312.45
313.05
313.55
314.05
314.75
315.35
315.85
316.45
317.05
317.55
318.05

Conductivity
(mS)
1.21
1.22
1.23
1.23
1.24
1.24
1.25
1.26
1.28
1.29
1.24
1.25
1.26
1.28
1.29
1.30
1.31
1.32
1.33
1.34
1.34
1.35
1.36
1.35

375
390
405
420
435
450
465
480
495
510
525
540
555
570
585
600
615
630
645
660
675
690
705
720
735
750
765
780
795
810
825
840
855
870
885
900
915
930
945
960
975

45.5
46.0
46.5
47.0
47.6
48.0
31.2
32.6
33.3
34.0
34.7
35.2
35.8
36.2
36.7
37.2
37.7
38.2
38.8
39.3
39.9
40.4
40.9
50.7
52.7
52.7
52.8
52.8
52.8
52.8
52.8
52.8
52.8
52.8
52.7
52.7
52.7
52.7
52.6
52.6
52.6

318.65
319.15
319.65
320.15
320.75
321.15
304.35
305.75
306.45
307.15
307.85
308.35
308.95
309.35
309.85
310.35
310.85
311.35
311.95
312.45
313.05
313.55
314.05
323.85
325.85
325.85
325.95
325.95
325.95
325.95
325.95
325.95
325.95
325.95
325.85
325.85
325.85
325.85
325.75
325.75
325.75

1.36
1.35
1.36
1.36
1.37
1.37
1.37
1.38
1.38
1.39
1.39
1.39
1.39
1.39
1.39
1.40
1.40
1.40
1.40
1.40
1.40
1.40
1.40
1.40
1.40
1.40
1.40
1.40
1.40
1.40
1.41
1.40
1.40
1.40
1.40
1.40
1.39
1.39
1.39
1.38
1.38

990
1005
1020
1035
1050
1065

52.6
52.5
52.5
52.4
52.4
52.4

325.75
325.65
325.65
325.55
325.55
325.55

1.37
1.37
1.37
1.37
1.36
1.36

35 ml Sulphuric Acid (catalyst)


Stirrer Speed:

Reagent Mixture:

38

Acetic Anhydride

10

mL

Glacial Acetic Acid

250

mL

H2O

150

mL

H2SO4 (27.18) solution

35

mL

Time
(s)
15
30
45
60
75
90
105
120
135
150
165
180
195
210
225
240
255

rpm
C

T (oC)

Temperature (K)

Conductivity (mS)

34.10
35.00
36.70
36.20
36.70
37.10
37.60
38.00
38.50
38.90
39.40
39.90
40.30
40.80
41.30
41.70
42.20

307.25
308.15
309.85
309.35
309.85
310.25
310.75
311.15
311.65
312.05
312.55
313.05
313.45
313.95
314.45
314.85
315.35

1.13
1.14
1.16
1.17
1.18
1.19
1.19
1.20
1.21
1.21
1.22
1.23
1.23
1.24
1.24
1.25
1.25

270
285
300
315
330
345
360
375
390
405
420
435
450
465
480
495
510
525
540
555
570
585
600
615
630
645
660
675
690
705
720
735
750
765
780
795
810
825
840
855
870

42.70
43.10
43.60
44.10
44.70
45.00
45.50
46.00
46.40
46.80
47.20
47.60
48.10
48.50
48.80
49.00
49.50
49.70
50.00
50.20
50.50
50.70
50.90
51.10
51.30
51.60
51.70
51.90
52.00
52.10
52.20
52.20
52.30
52.30
52.30
52.30
52.30
52.30
52.00
51.30
52.8

315.85
316.25
316.75
317.25
317.85
318.15
318.65
319.15
319.55
319.95
320.35
320.75
321.25
321.65
321.95
322.15
322.65
322.85
323.15
323.35
323.65
323.85
324.05
324.25
324.45
324.75
324.85
325.05
325.15
325.25
325.35
325.35
325.45
325.45
325.45
325.45
325.45
325.45
325.15
324.45
325.95

1.26
1.26
1.27
1.27
1.29
1.30
1.30
1.31
1.31
1.32
1.32
1.33
1.33
1.34
1.34
1.34
1.35
1.35
1.36
1.36
1.36
1.36
1.40
1.40
1.40
1.41
1.41
1.41
1.41
1.41
1.44
1.44
1.44
1.44
1.44
1.44
1.44
1.44
1.43
1.42
1.40

885
900
915
930
945
960
975
990
1005
1020
1035
1050
1065

52.7
52.7
52.7
52.7
52.6
52.6
52.6
52.6
52.5
52.5
52.4
52.4
52.4

325.85
325.85
325.85
325.85
325.75
325.75
325.75
325.75
325.65
325.65
325.55
325.55
325.55

1.40
1.40
1.39
1.39
1.39
1.38
1.38
1.37
1.37
1.37
1.37
1.36
1.36

45 ml Sulphuric Acid (catalyst)

Stirrer Speed

Reagent Mixture

38

Acetic Anhydride

10

mL

Glacial Acetic Acid

250

mL

H2O

150

mL

H2SO4 (27.18) solution

45

mL

Time
15
30
45
60
75
90
105
120
135
150

Temp oC
32.7
33.3
33.7
34.1
34.6
34.9
35.4
35.8
36.2
36.7

Temp K
305.7
306.3
306.7
307.1
307.6
307.9
308.4
308.8
309.2
309.7

Rpm
C

Cond
1.07
1.12
1.14
1.16
1.16
1.19
1.20
1.21
1.22
1.23

165
180
195
210
225
240
255
270
285
300
315
330
345
360
375
390
405
420
435
450
465
480
495
510
525
540
555
570
585
600
615
630
645
660
675
690
705
720
735
750
765

37.2
37.6
38.1
38.6
39.1
39.6
40.1
40.6
41.1
41.6
42.1
42.6
43.1
43.8
44.2
44.6
45.1
45.6
46.1
46.5
47.0
47.4
47.9
48.3
48.6
48.9
49.2
49.6
49.9
50.2
50.4
50.6
50.9
51.1
51.3
51.4
51.5
51.7
51.8
51.9
52.0

310.2
310.6
311.1
311.6
312.1
312.6
313.1
313.6
314.1
314.6
315.1
315.6
316.1
316.8
317.2
317.6
318.1
318.6
319.1
319.5
320.0
320.4
320.9
321.3
321.6
321.9
322.2
322.6
322.9
323.2
323.4
323.6
323.9
324.1
324.3
324.4
324.5
324.7
324.8
324.9
325.0

1.25
1.25
1.26
1.27
1.26
1.29
1.30
1.31
1.31
1.33
1.34
1.35
1.35
1.36
1.37
1.37
1.36
1.37
1.39
1.40
1.40
1.41
1.41
1.42
1.42
1.42
1.43
1.44
1.45
1.45
1.46
1.46
1.46
1.46
1.46
1.48
1.49
1.49
1.49
1.50
1.50

780
795
810
825
840
855
870
885
900
915
930
945
960
975
990
1005
1020
1035
1050
1065
1080
1095
1110
1125
1140

52.0
52.1
52.2
52.2
52.2
52.3
52.3
52.3
52.3
52.3
52.2
52.2
52.2
52.2
52.2
52.2
52.1
52.1
52.1
52.0
52.0
52.0
51.9
51.9
51.8

325.0
325.1
325.2
325.2
325.2
325.3
325.3
325.3
325.3
325.3
325.2
325.2
325.2
325.2
325.2
325.2
325.1
325.1
325.1
325.0
325.0
325.0
324.9
324.9
324.8

1.50
1.50
1.50
1.50
1.50
1.50
1.50
1.50
1.50
1.50
1.49
1.49
1.49
1.49
1.46
1.48
1.46
1.47
1.48
1.48
1.47
1.48
1.48
1.48
1.48