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CHEMICAL REACTION ENGINEERING

LAB MANUAL

FOR
Under Graduates in Chemical Engineering

Wah Engineering College

Faculty Members
Lab Incharge: Dr. K. S. Baig
Lecturer Fazeel Ahmad
Lab Engineer Waqas khan
Lab Assistant: Ehteshamss Sabir

DEPARTMENT OF CHEMICAL ENGINEERING


WAH ENGINEERING COLLEGE,
UNIVERSITY OF WAH, WAH CANTT
Table of contents
Introduction
List of equipment
List of experiments
General safety guideline
Potential hazard
List of chemicals
CLO, PLO contents
Experimental detail
MSDS

i
List of Equipments
1. Batch Reactor
2. Continuous Stirred Tank Reactor
3. Continuous Stirred Tank Reactor in Series
4. Tubular Reactor

List of Experiments
Experiment 01: To find the reaction rate constant in a stirred batch reactor and study the
temperature effect on the rate of reaction.

Experiment 02: To find the reaction rate constant in a stirred batch reactor and study the
concentration effect on the rate of reaction.

Experiment 03: To find the reaction rate constant in a stirred batch reactor and study the stirrer
effect on the rate of reaction.

Experiment 04: To find the reaction rate constant in a continuous stirred tank reactor and study
the temperature effect on the rate of reaction.

Experiment 05: To find the reaction rate constant in a continuous stirred tank reactor and study
the concentration effect on the rate of reaction.

Experiment 06: To find the reaction rate constant in a continuous stirred tank reactor and study
the stirrer effect on the rate of reaction.

Experiment 07: To find the reaction rate constant in a continuous stirred tank reactor and study
the effect of flowrate on the rate of reaction.

Experiment 08: To find the reaction rate constant in a tubular reactor and study the temperature
effect on the rateof reaction.

Experiment 09: To find the reaction rate constant in a tubular reactor and study the concentration
effect on the rate of reaction.

Experiment 10: To find the reaction rate constant in a tubular reactor and study the effect of
flowrate on the rate of reaction
CLEANLINESS AND SAFETY GUIDELINES

Cleanliness
The Chemical Reaction Engineering Laboratory contains equipment that uses water
or chemicals as the fluid. There are “housekeeping” rules that students are required to clean up
theirarea at the conclusion of the performance of an experiment. Cleanup will include
 Removal of spilled water (or any liquid) or chemicals
 Wiping the table top on which the equipment is mounted

The lab should always be as clean as or cleaner than it was when you entered.
Cleaning the lab is your responsibility as a user of the equipment.

Safety
This is to serve as a guide and not as a comprehensive manual on safety. Every
staff/student has, at all time, a duty to care for Health and Safety of himself/herself and
of all people who may be affected by his/her action.
 Lab coat or Jackets MUST is worn all times.
 Rubber gloves should be worn when handling corrosive materials,
 Heat proof gauntlets when discharging any equipment involving heat.
 Wear fully covered shoes with strong grip.
 Goggles must be used whenever necessary especially when dealing with high
pressure equipment and chemicals
 Sometimes the floor may be wet. Therefore, care is essential.
 Always switch off power before removing plugs from sockets.
 Cables mustbe suspended and not lying on the floor.
 All cables and hoses should be routed to avoid walkways.
 This should be disposed of in the glass bin, not in the usual waste bin.
 Breakage should also be reported to the Instructor in charge.

Any appropriate instruction sheets should be studied before starting the experiment.
Particular attention should be given to the recommended precautions, startup procedure
and sequence of operation.
There should be NO Eating, No Smoking is strictly prohibited in all laboratories

In case of emergency, report to the Instructor, in charge or doctor/ambulance/fire fighter


Potentential Hazards
List of chemicals
1. Sodium hydroxide

2. Ethyle acetate

3. Distilled water

Lab Assessment Rubrics


(Chemical reaction engineering)

Points
2 1 0 Score
Criteria Excellent Satisfactory Unsatisfactory
Lab Report (Notebook) (10)
Introduction & Introduction provides all necessary Introduction is nearly complete, Some introductory data, but still
Experimental background principles for the missing some minor points & missing some major points &
procedure experiment & Experimental Experimental procedure is written in Experimental procedure is written in
procedure is well-written in bullets bullets format, important experimental bullets format, still missing some
important experimental details.
format step by step, all experimental details are covered, some minor details
details are covered. missing.

Data One component of data is Two components of data is Data is brief and missing significant
incomplete: incomplete: pieces of information.
1. Tables 1. Tables
2. Graphs 2. Graphs
3. Results 3. Results
Error Analysis Experimental errors, their possible Experimental errors and their possible Experimental errors are mentioned.
effects, and ways to reduce errors are effects are discussed.
discussed.
Calculations All calculations are shown, and the Some calculations are shown, and the Some calculations are shown, and the
results are correct and labeled results are correct and labeled results labeled appropriately.
appropriately. appropriately.
Conclusion Conclusions includes findings, Conclusions includes what was No conclusions were included in
possible source of error, and what learned from experiment. report or shows little effort.
was learned from experiment.
Lab Work (10)
Attendance 95 % 80 % 75 %

Pre-experiment 1. Standardization of equipment. Only proper Cleaning and washing of Some cleaning and washing of
Activities 2. Cleaning and washing of apparatus. apparatus.
apparatus.
3. Clear practical understanding.

Participation & Used time well in lab and focused Did the lab but did not appear very Participation was minimal, OR
Recording attention on the experiment & Makes interested. Focus was lost on several student was hostile about participating
rich observations and Records occasions & Makes many & Makes few observations and
relevant data in an organized and observations, but they may be Records little data
skillful way insufficient to generate data and
Records data, but organization is
lacking.
Post Experiment 1. Appropriate cleaning/ washing Appropriate cleaning/ washing of Some Appropriate cleaning / washing
Activities of items. items. of items.
2. Protection of items and
accessories.
3. Proper shutdown.
Safety Lab is carried out with full attention Lab is carried out with some attention Safety procedure were ignored, and/or
to relevant safety procedures. The to relevant safety procedures. The set- some aspect of the experiment posed a
set-up, experiment, and tear-down up, experiment, and tear-down posed threat to the safety of the student or
posed no safety threat to any no safety threat to any individual, but others
individual. several safety procedures need to be
reviewed.

Lab Engineer: ----------------------------- Lab Incharge: -------------------------------

Nomenclature

aµ sodium hydroxide conc. in feed vessel (mol/ dm3)


ao sodium hydroxide conc. in mixed feeds (mol/ dm3)
al sodium hydroxide conc. in reactor at time t (mol/ dm3)
a∝ sodium hydroxide conc. In reactor after infinite time (mol/dm3)
b ethyl acetate conc. (mol/ dm3) (same subscripts as above for a)
c sodium acetate conc. (mol/ dm3) (same subscripts as above for a)
F total volume feed rate (dm3/s)
Fa volume feed rate of sodium hydroxide. (dm3/s)
Fb volume feed rate of ethyl acetate. (dm3/s)
k specific rate constant
r reaction rate
T reactor temperature (K)
V volume of reactor (dm3)
Xa conversion of sodium hydroxide = ao – a1/ ao
Xc conversion of sodium acetate = Co – Co/ C∝
EXPERIMENT 1
To find the reaction rate constant in a batch reactor at room temperature.

THEORY

Batch Reactors

Batch reactors are used for most of the reactions carried out in a laboratory as well as in the
industries. The reactants are placed in a test-tube, flask or beaker. They are mixed together, often
heated for the reaction to take place and are then cooled. The products are taken out and, if
necessary, purified carefully.

Figure 1 Batch Reactor

Problems of Batch reactor


During loading and after unloading some concentration of the reactants as well as product may
remain in the reactor which may cause following problem.
1. It may reduce next product batch purity.
2. It may cause the wastage of chemicals to clean the previous batch.
3. It may cause the fouling on the internal part of the reactor.
REACTIONS

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

Assuming that the initial concentrations are equal and that the converted concentration is X then
the final concentrations are

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

a-X a-X X X

13
Order of reaction

The powers to which the concentrations are raised is called the order of the reaction. The order
refers to the empirically found rate expression, it can have a fractional value and need not be an
integer.
Second-order reaction
The simplest kind of second-order reaction is one whose rate is proportional to the square of the
concentration of one reactant. These generally have the form 2A → products. A second kind of
second-order reaction has a reaction rate that is proportional to the product of the concentrations
of two reactants. Such reactions generally have the form A + B → products.
From the kinetic analysis of a general second order reaction it can be shown that

𝑿
𝒌. 𝒕 = −
𝒂(𝒂 − 𝑿)

Where k is the reaction rate constant, t is the time of reaction,a is the initial concentration of
sodium hydroxide and X is the conversion.

EXPERIMENTAL SETUP

APPARATUS:

Figure 2 Batch Reactor

14
APPARATUS

 Batch Reactor
 Stop Watch
 Beaker
 Volumetric Cylinder

CHEMICALS:

 Sodium Hydoxide
 Ethyl Acetate
 Water

PROCEDURE:

 Make 1 liter batches of 0.05 M of sodium hydroxide in the beaker and 0.05 M ethyl acetate
in the beaker to 20°C.
 Adjust the set point of the temperature controller to 25°C.
 Charge the batch reactor with 0.5 liter of of sodium hyroxide solution and ethyl acetate
solution through beaker.
 The experiment involves the storage and collection of conductivity data, as the time pass
conductivity will decrease and note readings with the help of conductivity cell. The data
output port must be connected to data logger interface. This will enable data logging of the
conductivity at selected time intervals over a selected period. If computer is not available,
conductivity can be recorded manually at different time intervals by reading the value
directly from the conductivity meter in the console.
 Collection of data will be until a steady state condition is reached in the Batch reactor and
this takes approximately 30 minutes by using stopwatch.
 Switch on the chilled water circulator.

It has been determined that the degree of conversion of reagents affects the conductivity of the
reactor contents so that the readings of conductivity can be used to calculate the amount of
conversion.

15
PRECAUTIONS

1. Do not adjust the rpm of peristaltic pump during running position of the pump.
2. Do not stop the stirrer during the running of batch reactor during the process.
3. Do not change the volume in the beaker during experiment.
4. Put all the batch of your reactants in the reactor at once and take product from the reactor at
once.

ERRORS

1. There may be errors for not taking sample weight in correct amount.
2. There may be error in calibrating the peristaltic pump.
3. There may be error for feeding the batch within given time.

INTERPRETATION OF RESULTS:

Observations & Calculations.

Table no. 1

Observation Time(mint) RPM Flow rate(ml/min)


1
2
3
4
5

 Note down the observations, organize the data and tabularize the data.
 To calulate the specific rate constant k, plot a graph of Xa and time. The slope of the graph
will be rate constant.
 Also analyze the data. The conductivity measurements must now be translated into degree of
conversion of the constituents.
16
 Both sodium hydroxide and sodium acetate contribute conductance to the reaction solution
while ethyl acetate and ethyl alcohol do not. The conductivity of a sodium hydroxide solution
at a given concentration and temperature is not same as that of a sodium acetate solution at the
same molarity and temperature and a relationship has been established allowing conversion to
be inferred from conductivity.

IDEAR RESULT PLOT

35
Flow rate vs RPM
Product flow rate/(ml/mint)

30

25

20

15

10

0
1 2 3 4 5 6 7 8 9
RPM

Figure no.3 product flow rate vs Pump rpm

POSSIBLE QUESTIONS

1. Can we use other fluids for cooling the reactor mixture after completion of exothermic
reaction.?
2. Can we use other type of pump than peristatic one?.
3. What is difference between molar and molal solution ?.
4. If you increase the temperature of heater then what will be the effect on conductivity?.
Conclusion

With the increase of pump flow rate , product flow rate goes on increasing because pump

speed causes more product out from the reactor. ……………………………………………

17
EXPERIMENT 2

To find the reaction rate constant in a stirred batch reactor at the room temperature.

THEORY

Batch Reactor

Batch Reactors are defined as reactors in which no flow of mass across the reactor boundaries,
once the reactants have been charged.

Characteristics of Batch Reactors

1. Each batch is a closed system.

2. The total mass of each batch is fixed.

3. The volume or density of each batch may vary as reaction proceeds.

4. The energy of each batch may vary as reaction proceeds; heat exchanger may be provided
to control temperature.

5. The reaction (residence) time for elements of the reacting fluid is the same.

6. The operation of the reactor is inherently unsteady-state; batch composition changes with
respect to time.

7. At any time, the batch is uniform in composition, temperature because of the efficient and
vigorous stirring

REACTION:

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

Assuming that the initial concentrations are equal and that the converted concentration is X then
the final concentrations are

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

18
a-X a-X X X

Order of reaction

The powers to which the concentrations are raised is called the order of the reaction. The order
refers to the empirically found rate expression; it can have a fractional value and need not be an
integer.
Second order reaction
The simplest kind of second-order reaction is one whose rate is proportional to the square of the
concentration of one reactant. These generally have the form 2A → products. A second kind of
second-order reaction has a reaction rate that is proportional to the product of the concentrations
of two reactants. Such reactions generally have the form A + B → products

From the kinetic analysis of a general second order reaction it can be shown that

𝑿
𝒌. 𝒕 = −
𝒂(𝒂 − 𝑿)

Where k is the reaction rate constant ,t is the time of reaction a is the initial concentration of
sodium hydroxide and X is the conversion.

EXPERIMENTAL SETUP
19
APPARATUS:

Figure 4 Stirrer Batch reactor

 Batch reactor
 Stop Watch
 Beaker
 Volumetric Cylinder

CHEMICALS:

 Sodium Hydoxide
 Ethyl Acetate
 Water

PROCEDURE:

 Make 1 liter batches of 0.05 M of sodium hydroxide and 0.05 M ethyl acetate to 30°C in
the beaker.
 Adjust the set point of the temperature controller to 30°C at the panel.
 Charge the batch reactor with 0.5 liter of of sodium hyroxide solution and ethyl acetate
solution through beaker.

20
 The experiment involves the storage and collection of conductivity data, as the time pass
conductivity of the cell decreases and the data output port must be connected to data logger
interface. This will enable data logging of the conductivity at selected time intervals over
a selected period. If computer is not available, conductivity can be recorded manually at
different time intervals by reading the value directly from the conductivity meter in the
console.
 Collection of data will be until a steady state condition is reached in the reactor and this
takes approximately 30 minutes by using stopwatch.
 Switch on the chilled water circulator.
 Repeat all steps for concentrations 1.0 M, 1.5 M,2.0 and 2.5 M.

It has been determined that the degree of conversion of reagents affects the conductivity of the
reactor contents so that the readings of conductivity can be used to calculate the amount of
conversion.

PRECAUTIONS

1) Do not switch of the stirrer during the reaction.


2) Do not shake the reactants solution when the reactants batch is prepared.
3) Do not switch on or off temperature controller without permission of your laboratory
supervisor.

ERRORS

1. There may be error for not operating stirrer properly during the reaction.
2. There may be error for not taking correct amount of reactants.

INTERPRETATION OF RESULTS:

Observations & Calculations.

Table no. 2

Observation time(min) Conversion(X)


1

21
2
3

 Note down the observations, organize the data and tabularize the data.
 To calulate the specific rate constant k, plot a graph of Xa and time. The slope of the graph
will be rate constant.
 Also analyze the data. The conductivity measurements must now be translated into degree of
conversion of the constituents.

Both sodium hydroxide and sodium acetate contribute conductance to the reaction solution while
ethyl acetate and ethyl alcohol do not. The conductivity of a sodium hydroxide solution at a given
concentration and temperature is not same as that of a sodium acetate solution at the same molarity
and temperature and a relationship has been established allowing conversion to be inferred from
conductivity

IDEAL RESULTS PLOT

350
conversion vs
300 time
250
conversion

200
150
100
50
0
0 50 100150200250300
time (sec)

Figure 5 conversion vs time

22
3.5

3
conductivity/(ms/cm)

2.5

1.5

0.5

0
1 2 3 4 5 6 7 8
time (mint)

Figure 6 conductivity vs time

Figure 7 concentration vs time

POSSIBLE QUESTIONS

1. Can we use condutivity meter as the reaction proceed?.


2. Is the conversion in all the reactors is same.?if varies then how much it varies?.
3. What is 1 molar solution?.
4. What is difference between molar and molal solution?.

23
5. What is the behavior of conductivity with the increase in the temperature and pressure in
case of solid and liquids and gases?.

Conclusion

………………………………………………………………………………………………
………………………………………………………………………………………………
………………………………………………………………………………………………
………………………

24
EXPERIMENT 3
To find the reaction rate constant in a plug flow reactor at the room temperature.

THEORY

Role of mixing in chemical reactions


Chemical reactions are often accompanied by mixing and without mixing. Whether they are

combined in a small flask that is swirled by hand or in a hundred-gallon mechanically-stirred

vessel, reactants generally undergo reaction faster and or more completely when mixed properly.

Mixing can influence not just reaction rate but also product distribution if more than one product

is possible.

At the laboratory scale, the competition between reaction and mixing are not always readily seen
but it can be seen in the industrial scale. Mixing effects become more critical in industrial reactions
where the rates of reaction, mixing and heat transfer approach one another.

REACTION:

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

Assuming that the initial concentrations are equal and that the converted concentration is X then
the final concentrations are

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

a-X a-X X X

From the kinetic analysis of a general second order reaction it can be shown that

𝑿
𝒌. 𝒕 = −
𝒂(𝒂 − 𝑿)

Where k is the reaction rate constant and t is the time of reaction.

25
EXPERIMENTAL SETUP

APPARATUS:

Figure 7 Plug Flow Reactor

 Batch Reactor
 Stop Watch
 Beaker
 Volumetric Cylinder

CHEMICALS:

 Sodium Hydoxide
 Ethyl Acetate
 Water

26
PROCEDURE:

 Make up 1 liter batches of 0.05 M of sodium hydroxide and 0.05 M ethyl acetate to 10°C.
 Adjust the set point of the temperature controller to 30°C.
 Charge the batch reactor with 0.5 liter of of sodium hyroxide solution and ethyl acetate
solution.
 The experiment involves the storage and collection of conductivity data, the data output
port must be connected to data logger interface. This will enable data logging of the
conductivity at selected time intervals over a selected period. If computer is not available,
conductivity can be recorded manually at different time intervals by reading the value
directly from the conductivity meter in the console.
 Collection of data will be until a steady state condition is reached in the reactor and this
takes approximately 30 minutes.
 Switch on the chilled water circulator.
 It has been determined that the degree of conversion of reagents affects the conductivity of
the reactor contents so that the readings of conductivity can be used to calculate the amount
of conversion.

PRECAUTIONS

1. Before the startup of reaction always check product lines valve position.
2. Do not touch the chemicals with hands during the experimentations.
3. Always use coolent outside the tubes to avoid damage of tubes.

INTERPRETATION OF RESULTS:

Observations & Calculations.

Table no. 3

Observation time(min) Conversion(X)


1
2
3

27
 Note down the observations, organize the data and tabularize the data.
 To calulate the specific rate constant k, plot a graph of Xa and time. The slope of the graph
will be rate constant.
 Also analyze the data. The conductivity measurements must now be translated into degree of
conversion of the constituents.
 Both sodium hydroxide and sodium acetate contribute conductance to the reaction solution
while ethyl acetate and ethyl alcohol do not. The conductivity of a sodium hydroxide solution
at a given concentration and temperature is not same as that of a sodium acetate solution at the
same molarity and temperature and a relationship has been established allowing conversion to
be inferred from conductivity.

𝛬𝑜 − 𝛬1
𝑎1 = (𝑎∞ − 𝑎𝑜) [ ] + 𝑎𝑜
𝛬𝑜 − 𝛬∞
𝑎𝑜 − 𝑎1
𝑋𝑎 =
𝑎𝑜

ERRORS

1. There may be error for not operating stirrer properly during the reaction.
2. There may be error for not taking correct amount of reactants.
3. There may be error during calibration of peristatic pump.

IDEAL RESULTS PLOTS

4
conductivity(ms/cm)

3
2
1
0
1 2 3 4 5 6 7 8
time (minutes)

Figure 8 conductivity vs time


28
350
conversion(mole/dm3) conversion vs
300 time
250
200
150
100
50
0
0 50 100150200250300
time (sec)

Figure 9 conversion vs time

Possible Questions

What will be effect of concentration on the rate of reaction if we increase the speed of Agetator?.

If we do not use Agetator then what will be change in conversion of all these reactors?.

Conclusion…………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
……

29
EXPERIMENT 4
To find the reaction rate constant in a continuous stirred tank reactor at the room
temperature.

Theory

Continuous Stirred Tank Reactor


Is a well-mixed vessel that operates at steady-state (Qin=Qout=Q). The main assumption in this
case is that the concentration of the incoming fluid will become instantaneously equal to the
outgoing upon entering the vessel.
Characteristics of Continuous Stirred Tank Reactor (CSTR):
1. The flow through the vessel both input and out streams, is continuous but not necessary at
a constant rate.
2. The system mass inside each vessel is not necessary fixed.
3. The volume or density of each batch may vary as reaction proceeds.
4. The energy of each batch may vary as reaction proceeds; heat exchanger may be provided
to control temperature.
5. The reaction (residence) time for elements of the reacting fluid is the same.
6. The operation of the reactor may be steady state or unsteady-state.
7. The fluid properties are uniform in composition, temperature anywhere in the vessel
because of the efficient and vigorous stirring

REACTION:

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

Assuming that the initial concentrations are equal and that the converted concentration is X then
the final concentrations are

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

a-X a-X X X

From the kinetic analysis of a general second order reaction it can be shown that

30
𝑿
𝒌. 𝒕 = −
𝒂(𝒂 − 𝑿)

Where k is the reaction rate constant and t is the time of reaction.

EXPERIMENTAL SETUP

APPARATUS:

 Continuous Stirred Tank Reactor


 Stop Watch
 Beaker
 Volumetric Cylinder

CHEMICALS:

 Sodium Hydoxide
 Ethyl Acetate
 Water

PROCEDURE:

 Make up 1 liter batches of 0.05 M of sodium hydroxide and 0.05 M ethyl acetate to 20°C.
 Adjust the set point of the temperature controller to 30°C.
 Run the peristaltic pump in order to flow the sodium hyroxide solution and ethyl acetate
solution into the reactor.
 The experiment involves the storage and collection of conductivity data, the data output
port must be connected to data logger interface. This will enable data logging of the
conductivity at selected time intervals over a selected period. If computer is not available,
conductivity can be recorded manually at different time intervals by reading the value
directly from the conductivity meter in the console.
 Collection of data will be until a steady state condition is reached in the reactor and this
takes approximately 30 minutes.
 Repeat all steps for temperatures 30°C, 35°C, 40°C and 45°C.

31
It has been determined that the degree of conversion of reagents affects the conductivity of the
reactor contents so that the readings of conductivity can be used to calculate the amount of
conversion.

PRECAUTIONS

1. Do not change the rpm of pump before achieving the steady state condition.
2. Do not change the concentration of the reactants in the vessel before achiveing steady state
3. Do not touch the chemicals while making solutions

ERRORS

1. There may be error during calibration of the pump.


2. There may be some un reacted reactants which will effect on the conductivity of our
product.

INTERPRETATION OF RESULTS:

Record the conductivity of the contents of the reactor over the period of the reaction, the
conductivity measurements must now be translated into degree of conversion of the constituents.

Enter the following known constants

Fa=

Fb=

aμ=

bμ=

cμ=

T=

V=

Calculate the following values.

32
𝐹𝑎
𝑎𝑜 = .a
𝐹𝑎 + 𝐹𝑏 μ

𝐹𝑎
𝑏𝑜 = .b
𝐹𝑎 + 𝐹𝑏 μ

Covert the readings of conductivity into concentrations

𝛬𝑜 − 𝛬1
𝑎1 = (𝑎∞ − 𝑎𝑜) [ ] + 𝑎𝑜
𝛬𝑜 − 𝛬∞

𝛬𝑜 − 𝛬1
𝑐1 = 𝑐∞ [ ]
𝛬𝑜 − 𝛬∞
a1 is value of sodium hydroxide concentration and c1 is sodium acetate concentrtaion and
degree of conversion are Xa and Xc.

𝑎𝑜 − 𝑎1
𝑋𝑎 =
𝑎𝑜
𝑐1
𝑋𝑐 =
𝑐∞

(𝐹𝑎+𝐹𝑏) 𝑎𝑜−𝑎1
To calulate specific rate constant k: 𝑘=( ).( )
𝑉 𝑎12

IDEAL RESULT PLOTS

4.5
4
conductivity(ms/cm)

3.5
3
2.5
2
1.5
1
0.5
0
1 2 3 4 5 6 7 8
time (minutes)

Figure 10 conductivity vs time


33
POSSIBLE QUESTIONS

1. Is the conversion will be same in all these reactors with and without stirring effec at
constant temperature ?.
2. It is possible to use one Plug flow reactor in place of three CSTR to achieve same
conversion at variation in the temperature ?.
3. What is the order of conductivity in case of gases,liquids and sloids.

Conclusion

………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………

34
EXPERIMENT 5
To find the reaction rate constant in a continuous stirred tank reactor and study the
concentration effect on rate of reaction.

THEORY

Continuous Stirred Tank Reactor


Is a well-mixed vessel that operates at steady-state (Qin=Qout=Q). The main assumption in this
case is that the concentration of the incoming fluid will become instantaneously equal to the
outgoing upon entering the vessel.
Characteristics of Continuous Stirred Tank Reactor (CSTR):
1. The flow through the vessel(s), both input and out streams, is continuous but not
necessary at a constant rate.
2. The system mass inside each vessel is not necessary fixed.
3. The volume or density of each batch may vary as reaction proceeds.
4. The energy of each batch may vary as reaction proceeds; heat exchanger may be provided
to control temperature.
5. The reaction (residence) time for elements of the reacting fluid is the same.
6. The operation of the reactor may be steady state or unsteady-state.
7. The fluid properties are uniform in composition, temperature anywhere in the vessel
because of the efficient and vigorous stirring
35
REACTION:

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

Assuming that the initial concentrations are equal and that the converted concentration is X then
the final concentrations are

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

a-X a-X X X

From the kinetic analysis of a general second order reaction it can be shown that

𝑿
𝒌. 𝒕 = −
𝒂(𝒂 − 𝑿)

Where k is the reaction rate constant and t is the time of reaction.

EXPERIMENTAL SETUP

APPARATUS:

 Continuous Stirred Tank Reactor


 Stop Watch
 Beaker
 Volumetric Cylinder

CHEMICALS:

 Sodium Hydoxide
 Ethyl Acetate
 Water

PROCEDURE: Concentration Effect

 Make up 1 liter batches of 0.05 M of sodium hydroxide and 0.05 M ethyl acetate to 20°C.

36
 Adjust the set point of the temperature controller to 20°C.
 Run the perstaltic pump in order to flow the sodium hyroxide solution and ethyl acetate
solution into the reactor.
 The experiment involves the storage and collection of conductivity data, the data output
port must be connected to data logger interface. This will enable data logging of the
conductivity at selected time intervals over a selected period. If computer is not available,
conductivity can be recorded manually at different time intervals by reading the value
directly from the conductivity meter in the console.
 Collection of data will be until a steady state condition is reached in the reactor and this
takes approximately 30 minutes.
 Switch on the chilled water circulator.
 Repeat all steps for concentrations 1.0 M, 0.02 M, 2.0 M and 1.5 M.

It has been determined that the degree of conversion of reagents affects the conductivity of the
reactor contents so that the readings of conductivity can be used to calculate the amount of
conversion.

PRECAUTIONS

1. Do not touch the chemicals while pouring them into the beakers
2. Do not not adjust the rpm of the pump before steady state has been achieved.
3. Do not start and then stop stirrer during the reaction completion.

ERRORS

1. There may be error for solution concentration it may be different concentration than
required.
2. There may be error of calibrating of pump.
3. There may be error in conductivity cell readings.

INTERPRETATION OF RESULTS:

Record the conductivity of the contents of the reactor over the period of the reaction, the
conductivity measurements must now be translated into degree of conversion of the constituents.

37
Enter the following known constants

Fa=

Fb=

aμ=

bμ=

cμ=

T=

V=

Calculate the following values.

𝐹𝑎
𝑎𝑜 = .a
𝐹𝑎 + 𝐹𝑏 μ

𝐹𝑎
𝑏𝑜 = .b
𝐹𝑎 + 𝐹𝑏 μ

Covert the readings of conductivity into concentrations

𝛬𝑜 − 𝛬1
𝑎1 = (𝑎∞ − 𝑎𝑜) [ ] + 𝑎𝑜
𝛬𝑜 − 𝛬∞

𝛬𝑜 − 𝛬1
𝑐1 = 𝑐∞ [ ]
𝛬𝑜 − 𝛬∞
a1 is value of sodium hydroxide concentration and c1 is sodium acetate concentrtaion and
degree of conversion are Xa and Xc.

𝑎𝑜 − 𝑎1
𝑋𝑎 =
𝑎𝑜
𝑐1
𝑋𝑐 =
𝑐∞

(𝐹𝑎+𝐹𝑏) 𝑎𝑜−𝑎1
To calulate specific rate constant k: 𝑘=( ).( )
𝑉 𝑎12

38
IDEAL RESULT PLOTS

45
40
time vs 1/ca
35
1/CA(mole /dm3)

30
25
20
15
10
5
0
0 5 10 15 20 25 30 35 35
time/mint

Figure 11 concentration vs time

POSSIBLE QUESTIONS

1. What will be effect of concentration on the rate of reaction if we increase the speed of
Agitator?.
2. If we do not use Agitator then what will be change in conversion of all these reactor?.

Conclusion……………………………………………………………………………………
…………………………………………………………………………………………………
…………………………………………………………………………………………………
……………………………

39
EXPERIMENT 6
To find the reaction rate constant in a continuous stirred tank reactor and study the stirrer
effect on rate of reaction.

THEORY

Role of mixing in chemical reactions :


Chemical reactions are often accompanied by mixing. Whether they are combined in a small
flask that is swirled by hand or in a hundred-gallon mechanically-stirred vessel, reactants
generally undergo reaction faster or more completely when mixed properly. Mixing can
influence not just reaction rate but also product distribution if more than one product is possible.

At the laboratory scale, the competition between reaction and mixing are not always readily seen.
Mixing effects become more critical in industrial reactions where the rates of reaction, mixing and
heat transfer approach one another

REACTION:

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

Assuming that the initial concentrations are equal and that the converted concentration is X then
the final concentrations are

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

a-X a-X X X

From the kinetic analysis of a general second order reaction it can be shown that

𝑿
𝒌. 𝒕 = −
𝒂(𝒂 − 𝑿)

Where k is the reaction rate constant and t is the time of reaction.

40
EXPERIMENTAL SETUP

APPARATUS:

 Continuous Stirred Tank Reactor


 Stop Watch
 Beaker
 Volumetric Cylinder

CHEMICALS:

 Sodium Hydoxide
 Ethyl Acetate
 Water

PROCEDURE: Stirrer Effect

 Make 1 liter batches of 0.05 M of sodium hydroxide and 0.05 M ethyl acetate.
 Adjust the set point of the temperature controller to 20°C.
 Set the agitator speed controller to 7.0 rpm.
 Switch on both feed pumps and the agitator motor, and begin taking readings.
 Run the perstaltic pump in order to flow the sodium hyroxide solution and ethyl acetate
solution into the reactor.
 The experiment involves the storage and collection of conductivity data, the data output
port must be connected to data logger interface. This will enable data logging of the
conductivity at selected time intervals over a selected period. If computer is not available,
conductivity can be recorded manually at different time intervals by reading the value
directly from the conductivity meter in the console.
 Collection of data will be until a steady state condition is reached in the reactor and this
takes approximately 30 minutes.
 Switch on the chilled water circulator.
 Repeat all steps for agitator speed controller to 14 rpm, 21 rpm, 28 rpm and 34 rpm.

41
It has been determined that the degree of conversion of reagents affects the conductivity of the
reactor contents so that the readings of conductivity can be used to calculate the amount of
conversion.

PRECAUTIONS

1. Do not vary rpm of the agitator in a single time.


2. Do not on off agitator before completion of the reaction.
3. Do not start agitator before the reactants have been reached in the reactor.
4. Take care of yourself while washing the reactor after the completion of reaction.

ERROR

1. There may be error for taking redaings during the runing position of the agitator.
2. There may be problem in the conductivity after consective readings have been taken.

INTERPRETATION OF RESULTS:

Record the conductivity of the contents of the reactor over the period of the reaction, the
conductivity measurements must now be translated into degree of conversion of the constituents.

Enter the following known constants

Fa=

Fb=

aμ=

bμ=

cμ=

T=

V=

Calculate the following values.

𝐹𝑎
𝑎𝑜 = .a
𝐹𝑎 + 𝐹𝑏 μ
42
𝐹𝑎
𝑏𝑜 = .b
𝐹𝑎 + 𝐹𝑏 μ

Covert the readings of conductivity into concentrations

𝛬𝑜 − 𝛬1
𝑎1 = (𝑎∞ − 𝑎𝑜) [ ] + 𝑎𝑜
𝛬𝑜 − 𝛬∞

𝛬𝑜 − 𝛬1
𝑐1 = 𝑐∞ [ ]
𝛬𝑜 − 𝛬∞
a1 is value of sodium hydroxide concentration and c1 is sodium acetate concentrtaion and
degree of conversion are Xa and Xc.

𝑎𝑜 − 𝑎1
𝑋𝑎 =
𝑎𝑜
𝑐1
𝑋𝑐 =
𝑐∞

(𝐹𝑎+𝐹𝑏) 𝑎𝑜−𝑎1
To calulate specific rate constant k: 𝑘=( ).( )
𝑉 𝑎12

IDEAL RESULTS PLOTS

45
40
time vs 1/ca
35
1/CA (mole/dm3)

30
25
20
15
10
5
0
0 5 10 15 20 25 30 35 35
time/mint

Figure 12 concentration vs time

43
POSSIBLE QUESTIONS:

1. How the conductivity varies with the speed of agitator?.


2. Is the conversin achieved is same in series of three reactor?.
3. What is molar solution ?.

Conclusion……………………………………………………………………………………
…………………………………………………………………………………………………
…………………………………………………………………………………………………
……………………………

44
45
EXPERIMENT 7
To find the reaction rate constant in a continuous stirred tank reactor and study the effect
of flowrate on rate of reaction.

THEORY

Continuous Stirred Tank Reactor


Is a well-mixed vessel that operates at steady-state (Qin=Qout=Q). The main assumption in this
case is that the concentration of the incoming fluid will become instantaneously equal to the
outgoing upon entering the vessel.
Characteristics of Continuous Stirred Tank Reactor (CSTR):
1. The flow through the vessel both input and out streams, is continuous but not necessary at
a constant rate.
2. The system mass inside each vessel is not necessary fixed.
3. The volume or density of each batch may vary as reaction proceeds.
4. The energy of each batch may vary as reaction proceeds; heat exchanger may be provided
to control temperature.
5. The reaction (residence) time for elements of the reacting fluid is the same.
6. The operation of the reactor may be steady state or unsteady-state.
7. The fluid properties are uniform in composition, temperature anywhere in the vessel
because of the efficient and vigorous stirring

REACTION:

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

Assuming that the initial concentrations are equal and that the converted concentration is X then
the final concentrations are

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

a-X a-X X X

From the kinetic analysis of a general second order reaction it can be shown that

46
𝑿
𝒌. 𝒕 = −
𝒂(𝒂 − 𝑿)

Where k is the reaction rate constant and t is the time of reaction.

APPARATUS:

 Continuous Stirred Tank Reactor


 Stop Watch
 Beaker
 Volumetric Cylinder

CHEMICALS:

 Sodium Hydoxide
 Ethyl Acetate
 Water

PROCEDURE:Effect of Flowrate

 Make 1 liter batches of 0.05 M of sodium hydroxide and 0.05 M ethyl acetate in the beaker.
 Adjust the set point of the temperature controller to 20°C.
 Run the perstaltic pump in order to flow the sodium hyroxide solution and ethyl acetate
solution into the reactor.
 The experiment involves the storage and collection of conductivity data, the data output
port must be connected to data logger interface. This will enable data logging of the
conductivity at selected time intervals over a selected period. If computer is not available,
conductivity can be recorded manually at different time intervals by reading the value
directly from the conductivity meter in the console.
 Collection of data will be until a steady state condition is reached in the reactor and this
takes approximately 30 minutes.
 Switch on the chilled water circulator.
 The experimental procedure is same with the exception that flow rates can be varied to
change the residence time of the reactants.

47
 Calulate the degree of conversion of the reactants at steady state using the conductivity
readings for different values of Fa and Fb.

It has been determined that the degree of conversion of reagents affects the conductivity of the
reactor contents so that the readings of conductivity can be used to calculate the amount of
conversion.

PRECAUTIONS

4. Do not touch the chemicals while pouring them into the beakers
5. Do not not adjust the rpm of the pump before steady state has been achieved.
6. Do not start and then stop stirrer during the reaction completion.

ERRORS

4. There may be error for solution concentration it may be different concentration than
required.
5. There may be error of calibrating of pump.
6. There may be error in conductivity cell readings.

INTERPRETATION OF RESULTS:

Record the conductivity of the contents of the reactor over the period of the reaction, the
conductivity measurements must now be translated into degree of conversion of the constituents.

Enter the following known constants

Fa=

Fb=

aμ=

bμ=
48
cμ=

T=

V=

Calculate the following values.

𝐹𝑎
𝑎𝑜 = .a
𝐹𝑎 + 𝐹𝑏 μ

𝐹𝑎
𝑏𝑜 = .b
𝐹𝑎 + 𝐹𝑏 μ

Covert the readings of conductivity into concentrations

𝛬𝑜 − 𝛬1
𝑎1 = (𝑎∞ − 𝑎𝑜) [ ] + 𝑎𝑜
𝛬𝑜 − 𝛬∞
𝛬𝑜 − 𝛬1
𝑐1 = 𝑐∞ [ ]
𝛬𝑜 − 𝛬∞
a1 is value of sodium hydroxide concentration and c1 is sodium acetate concentrtaion and
degree of conversion are Xa and Xc.

𝑎𝑜 − 𝑎1
𝑋𝑎 =
𝑎𝑜
𝑐1
𝑋𝑐 =
𝑐∞

(𝐹𝑎+𝐹𝑏) 𝑎𝑜−𝑎1
To calulate specific rate constant k: 𝑘=( ).( )
𝑉 𝑎12

IDEAL RESULTS PLOT

49
conversion vs time
1
0.8
conversion

0.6
0.4
0.2
0
1 2 3 4 5 6 7 8 9 10 11 12
time /mint

Figure 13 conversion vs time

POSSIBLE QUESTIONS

1. What will be the effect of agitator speed on the conversion of reaction ?.


2. What is effect of pump rpm on the conductivity values?.
3. What is effect of stirring on the rate of reaction?.

Conclusion

………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………

50
EXPERIMENT 8
To find the reaction rate constant in a tubular reactor and study the temperature effect on
rate of reaction.

THOERY

Batch Reactors

Batch reactors are used for most of the reactions carried out in a laboratory as well as in the
industry. The reactants are placed in a test-tube, flask or beaker. They are mixed together, often
heated for the reaction to take place and are then cooled. The products are taken out and, if
necessary, purified carefully. This procedure is also carried out in industry, the key difference
being one of size of reactor and the quantities of reactants.
Problems of batch reactor
During loading and after unloading some concentration of the reactants as well as product may
remain in the reactor which may cause following problem.
1. It may reduce next product batch purity.
2. It may cause the wastage of chemicals to clean the previous batch.
3. It may cause the fouling on the internal part of the reactor.
REACTION:

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

Assuming that the initial concentrations are equal and that the converted concentration is X then
the final concentrations are

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

a-X a-X X X

From the kinetic analysis of a general second order reaction it can be shown that

𝑿
𝒌. 𝒕 = −
𝒂(𝒂 − 𝑿)

Where k is the reaction rate constant and t is the time of reaction.

APPARATUS:
51
Figure 14 Plug flow reactor

 Tubular Reactor
 Stop Watch
 Beaker
 Volumetric Cylinder

CHEMICALS:

 Sodium Hydoxide
 Ethyl Acetate
 Water

PROCEDURE: Temperature Effect

 Make 1 liter batches of 0.05 M of sodium hydroxide and 0.05 M ethyl acetate in the beaker.
 Adjust the set point of the temperature controller to 10°C.
 Run the perstaltic pump in order to flow the sodium hyroxide solution and ethyl acetate
solution into the reactor.
 The experiment involves the storage and collection of conductivity data, the data output
port must be connected to data logger interface. This will enable data logging of the
conductivity at selected time intervals over a selected period. If computer is not available,
conductivity can be recorded manually at different time intervals by reading the value
directly from the conductivity meter in the console.

52
 Collection of data will be until a steady state condition is reached in the reactor and this
takes approximately 30 minutes.
 Switch on the chilled water circulator.
 Repeat all steps for temperatures 20°C, 30°C, 40°C and 50°C.

It has been determined that the degree of conversion of reagents affects the conductivity of the
reactor contents so that the readings of conductivity can be used to calculate the amount of
conversion.

PRECAUTIONS

1. Do not vary rpm of the agitator in a single time.


2. Do not on off agitator before completion of the reaction.
3. Do not start agitator before the reactants have been reached in the reactor.
4. Take care of yourself while washing the reactor after the completion of reaction.

ERROR

There may be error for taking redaings during the runing position of the agitator.

There may be problem in the conductivity after consective readings have been taken.

INTERPRETATION OF RESULTS:

Enter the following known constants from the experiment:

Fa=

Fb=

aμ=

bμ=

cμ=

53
T=

V=

Calculate the following values

𝐹𝑎
𝑎𝑜 = .a
𝐹𝑎 + 𝐹𝑏 μ

𝐹𝑎
𝑏𝑜 = .b
𝐹𝑎 + 𝐹𝑏 μ

Covert the readings of conductivity into concentrations

𝛬𝑜 − 𝛬1
𝑎1 = (𝑎∞ − 𝑎𝑜) [ ] + 𝑎𝑜
𝛬𝑜 − 𝛬∞

𝛬𝑜 − 𝛬1
𝑐1 = 𝑐∞ [ ]
𝛬𝑜 − 𝛬∞
a1 is value of sodium hydroxide concentration and c1 is sodium acetate concentrtaion and
degree of conversion are Xa and Xc.

𝑎𝑜 − 𝑎1
𝑋𝑎 =
𝑎𝑜
𝑐1
𝑋𝑐 =
𝑐∞

(𝐹𝑎+𝐹𝑏) 𝑎𝑜−𝑎1 1
To calulate specific rate constant k: 𝑘=( ).( ) . 1000∗60
𝑉 𝑎12

54
IDEAL RESULTS PLOTS

10
conversion vs time
8
Xa/1-Xa

6
4
2
0
1 2 3 4 5 6 7 8 9 10 11
time(mint)

Figure 14 conversion vs time

Conclusion

………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
.

55
EXPERIMENT 10
To find the reaction rate constant in a tubular reactor and study the effect of flowrate on
rate of reaction.

THEORY

PLUG FLOW REACTOR

Plug Flow Reactors (PFR) are defined to be flow reactors characterized by the absence of mixing
in the direction of flow and absence of variation normal to the direction of flow.

Characteristics of Plug Flow Reactors(PFR)

1. The flow through the vessel(s), both input and out streams, is continuous but not necessary
at a constant rate.

2. The system mass inside each vessel is not necessary fixed.

3. The density of the flowing system may vary in the direction of flow.

4. There is no axial mixing of fluid inside the reactor, composition changes along the flow
direction.

5. There is complete radial mixing of fluid inside the reactor; uniform fluid properties along
the direction normal to flow direction.

6. The energy may vary as reaction proceeds; heat exchanger may be provided to control
temperature.

7. The reaction (residence) time for elements of the reacting fluid is the same.

8. The operation of the reactor may be steady state or unsteady-state.

REACTION:

NaOH+CH3COOC2H5 CH3COONa+C2H5OH

Assuming that the initial concentrations are equal and that the converted concentration is X then
the final concentrations are

NaOH+CH3COOC2H5 CH3COONa+C2H5OH
56
a-X a-X X X

From the kinetic analysis of a general second order reaction it can be shown that

𝑿
𝒌. 𝒕 = −
𝒂(𝒂 − 𝑿)

Where k is the reaction rate constant and t is the time of reaction.

EXPERIMENTAL SETUP

APPARATUS:

 Tubular Reactor
 Stop Watch
 Beaker
 Volumetric Cylinder

CHEMICALS:

 Sodium Hydoxide
 Ethyl Acetate
 Water

PROCEDURE:Effect of Flowrate

 Make up 1 litre batches of 0.05 M of sodium hydroxide and 0.05 M ethyl acetate to 10°C.
 Adjust the set point of the temperature controller to 10°C.
 Run the perstaltic pump in order to flow the sodium hyroxide solution and ethyl acetate
solution into the reactor.
 The experiment involves the storage and collection of conductivity data, the data output
port must be connected to data logger interface. This will enable data logging of the
conductivity at selected time intervals over a selected period. If computer is not available,
conductivity can be recorded manually at different time intervals by reading the value
directly from the conductivity meter in the console.
57
 Collection of data will be until a steady state condition is reached in the reactor and this
takes approximately 30 minutes.
 Switch on the chilled water circulator.
 The experimental procedure is same with the exception that flow rates can be varied to
change the residence time of the reactants.
 Calulate the degree of conversion of the reactants at steady state using the conductivity
readings for different values of Fa and Fb.

It has been determined that the degree of conversion of reagents affects the conductivity of the
reactor contents so that the readings of conductivity can be used to calculate the amount of
conversion.

PRECAUTIONS

1. Do not change the rpm of pump before achieving the steady state condition.
2. Do not change the concentration of the reactants in the vessel before achiveing steady state
3. Do not touch the chemicals while making solutions

ERRORS

1. There may be error during calibration of the pump.


2. There may be some un reacted reactants which will effect on the conductivity of our
product.

INTERPRETATION OF RESULTS:

Enter the following known constants from the experiment:

Fa=

Fb=

58
aμ=

bμ=

cμ=

T=

V=

Calculate the following values

𝐹𝑎
𝑎𝑜 = .a
𝐹𝑎 + 𝐹𝑏 μ

𝐹𝑎
𝑏𝑜 = .b
𝐹𝑎 + 𝐹𝑏 μ

Covert the readings of conductivity into concentrations

𝛬𝑜 − 𝛬1
𝑎1 = (𝑎∞ − 𝑎𝑜) [ ] + 𝑎𝑜
𝛬𝑜 − 𝛬∞

𝛬𝑜 − 𝛬1
𝑐1 = 𝑐∞ [ ]
𝛬𝑜 − 𝛬∞
a1 is value of sodium hydroxide concentration and c1 is sodium acetate concentrtaion and
degree of conversion are Xa and Xc.

𝑎𝑜 − 𝑎1
𝑋𝑎 =
𝑎𝑜
𝑐1
𝑋𝑐 =
𝑐∞

(𝐹𝑎+𝐹𝑏) 𝑎𝑜−𝑎1 1
To calulate specific rate constant k: 𝑘=( ).( ) . 1000∗60
𝑉 𝑎12

59
IDEAL RESULTS PLOTS

Figure 15 concentration vs time

POSSIBLE QUESTIONS
1 If the reaction is endothermic then what will be the effect of by increasing flow rate on rate
constant?.
2 If the reaction is higher order then what will effect by increasing flow rate on the rate
constant?.
Conclusion

………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………

60
MATERIAL SAFETY DATA SHEET

PRODUCT: CAUSTIC SODA PEARL Date of Issue: Dec 2015

1. IDENTIFICATION OF CHEMICAL PRODUCT AND SUPPLIER

PRODUCT IDENTIFICATION:

Product Names: Supplier’s Product Code:

CAUSTIC SODA PEARL 2512

Other Names: Sodium hydroxide, Sodium hydrate, Lye

Recommended Use: General chemical

Formula:

Molecular formula H-Na-O

Structural formula NaOH

Chemical family Alkali hydroxide

Supplier: Formula Chemicals (N.S.W.) Pty Ltd

61
Address: 86 Hermitage Rd West Ryde NSW 2114

Telephone Number: (02) 9807 4266

Emergency Telephone: (02) 9807 4266 or Poisons Information Centre 131126

ACN: 001 129 406

2. HAZARDS IDENTIFICATION

HAZARDOUS SUBSTANCE. DANGEROUS GOODS

Classified as hazardous according to the criteria of NOHSC.

Hazard Category: C Corrosive,

Risk phrases: R35 Causes severe burns, R41 Risk of serious damage to eyes

Safety phrases: S2 Keep out of reach of children. S26 In case of contact with eyes,

rinse immediately with plenty of water and contact a doctor or Poisons

Information Centre. S37/39 Wear suitable gloves and eye/face

protection.

SUSDP Classification: Schedule 6

ADG Classification: Class 8 Corrosive

3. COMPOSITION/INFORMATION ON INGREDIENTS

Synonyms: Caustic soda, Sodium hydrate, Lye

62
Appearance: White deliquescent solid in small bead form, absorbs water on exposure

to air.

Ingredients:

Chemical Name, CAS No Proportion Risk Phrases

Sodium hydroxide 1310- 95 - 100 % R35, R41

73-2

All the constituents of this material are listed on the Australian Inventory of Chemical Substances (AICS)

63
4. FIRST AID MEASURES

Poison Information Centres in each state can provide additional assistance for scheduled poisons. Phone

131126 from anywhere in Australia.

Ingestion:

Never give anything by mouth if victim is rapidly losing consciousness, or is unconscious or convulsing.

Rinse mouth thoroughly with water. Do NOT induce vomiting. If victim can swallow, have him/her

drink 250 to 300 mL of water to dilute material in stomach. If vomiting occurs naturally, have victim

lean forward to reduce risk of aspiration. Repeat administration of water. Obtain medical attention

immediately.

Eye Contact:

Immediately flush the contaminated eye(s) with lukewarm, gently flowing water for 30 minutes, by the

clock, holding the eyelid(s) open. Take care not to rinse contaminated water into the non-affected eye.

If irritation persists, repeat flushing. If available, a neutral saline solution may be used to flush the

contaminated eye(s) an additional 30 minutes. Obtain medical attention immediately.

Skin Contact:

First aiders avoid direct contact with this chemical. As quickly as possible, flush contaminated area

with lukewarm, gently running water for at least 30 minutes, by the clock. Under running water, remove

contaminated clothing, shoes, and leather goods (e.g. watchbands, belts). If irritation persists, repeat

flushing. Obtain medical attention immediately. Completely decontaminate clothing, shoes and leather

goods before re-use or discard.

Inhalation:

Remove source of contamination or move victim to fresh air. Obtain medical advice immediately.

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Other First Aid:

Provide general supportive measures (comfort, warmth, rest). Consult a physician and/or the nearest

Poison Information Centre for all exposures except minor instances of inhalation contact.

Notes to physician:

Treat symptomatically as for strong alkalis.

5. FIRE FIGHTING MEASURES

Specific hazards:

Non-combustible material.

Fire fighting further advice:

Not combustible. Can react with some metals generating flammable hydrogen gas. Contact with some

organic chemicals can produce violent or explosive conditions. Reaction with water may generate

enough heat to ignite combustible material.

Suitable Extinguishing media:

Water fog (or if unavailable fine water mist or spray), foam, dry agent (carbon dioxide, dry chemical

powder).

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6. ACCIDENTAL RELEASE MEASURES

Small Spills: Wear personal protective equipment. Sweep up but avoid generating dust. Contain

solutions using sand or diatomaceous earth. Collect and seal in properly labeled drums. Wash remaining

area with large volumes of water.

Large Spills:

PRECAUTIONS Restrict access to area. Clear area of unprotected personnel. Provide adequate

protective equipment and ventilation. Remove chemicals which can react with the spilled material. Spills

of solutions containing material are slippery.

CLEANUP Contain spill or leak. Do not allow entry into sewers or waterways.

Neutralise the final traces and flush area with water. Spilled solutions should be contained by dyking

with inert material, such as sand or earth. Solutions can be recovered or carefully diluted with water

and cautiously neutralised with acids such as acetic acid or hydrochloric acid.

DISPOSAL Federal, state and local regulations should be reviewed prior to disposal. May be possible

to neutralise, dilute and flush the material into a sewer. May be possible to atomise dilute solutions in

an approved combustion chamber. Harmful to aquatic life in high concentrations.

7. HANDLING AND STORAGE

HANDLING Avoid generating mist or spray. When diluting solution, add sodium hydroxide to water

in small amounts. Heat evolved when dissolving may cause boiling and spattering. Add to large

volumes of cold water only. Label containers. Keep containers closed when not in use. Empty containers

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may contain residues which are hazardous. Use smallest possible amounts in designated areas with

adequate ventilation. Have emergency equipment (for fires, spills, leaks, etc.) readily available.

STORAGE CONDITIONS Materials that react violently with sodium hydroxide should not be stored

in the same area. Use corrosion-resistant structural materials and lighting and ventilation systems in the

storage area. Store in suitable labelled containers. Keep containers tightly closed when not in use and

when empty. Protect from damage. Containers made of nickel alloys are preferred. Steel containers are

acceptable if temperatures are not elevated. Storage tanks should be above ground and surrounded with

dykes capable of holding entire contents. Limit quantity of material in storage. Restrict access to storage

area. Post warning signs when appropriate. Keep storage area separate from populated work areas.

Inspect periodically for deficiencies such as damage or leaks.

Class 8 goods are not to be loaded with Classes 1, 4.3, 5.1, 5.2, 6*, 7, or foodstuffs or foodstuff empties.

* when Class 6 is a cyanide and Class 8 is an acid. Do not store or transport with strong acids.

8. EXPOSURE CONTROLS/PERSONAL PROTECTION

Exposure Standards: TLV/TWA: 2 mg/m3, peak, NOHSC Australia.

Engineering Controls: Maintain concentration below recommended exposure limit.

Engineering control methods to reduce hazardous exposures are preferred. General methods include

mechanical ventilation, (dilution and general exhaust), process or personnel enclosure, control of

process conditions and process modification (e.g. substitution of a less hazardous material).

Administrative controls and personal protective equipment may be also required. Use a corrosion-

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resistant ventilation system separate from other exhaust ventilation systems. Exhaust directly to the

outside. Use local exhaust ventilation, and process enclosure if necessary, to control airborne spray /

mists. Supply sufficient air to make up for air removed by exhaust systems.

Personal Protection:

RESPIRATORY PROTECTION : If engineering controls and work practices are not effective in

controlling exposure to this material, then wear suitable personal protective equipment including

approved respiratory protection.

Have appropriate equipment available for use in emergencies such as spills or fire. If respiratory

protection is required, institute a complete respiratory protection program including selection, fit testing,

training, maintenance and inspection.

CONCENTRATIONS IN AIR: UP TO 50 mg/m3: Powered air-purifying respirator with dust and mist

filter(s); or SAR operated in a continuous flow mode. UP TO 100 mg/m3: Full-face piece SCBA; or

full-face piece SAR; or full-face piece respirator with high-efficiency particulate filter(s). UP TO 250

mg/m3 Positive pressure, full-face piece SAR. EMERGENCY OR PLANNED ENTRY IN

UNKNOWN CONCENTRATION OR IDLH CONDITIONS: Positive pressure, full-face piece SCBA;

or positive pressure, full-face piece SAR with an auxiliary positive pressure SCBA. ESCAPE: Full-face

piece respirator with high-efficiency particulate filter(s); or escape-type SCBA. NOTE: The IDLH

concentration for sodium hydroxide is 250 mg/m3. NOTE: Substance causes eye irritation or damage;

eye protection needed.

ABBREVIATIONS: SAR = supplied-air respirator; SCBA = self-contained breathing apparatus. IDLH

= Immediately Dangerous to Life or Health.

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NOTE: In these recommendations the IDLH concentration is defined as the maximum concentration

which would not cause any escape impairing symptoms or irreversible health effects to a person exposed

for 30 minutes if the respirator failed.

EYE/FACE PROTECTION Splash proof chemical safety goggles. A face shield may also be

necessary.

SKIN PROTECTION Impervious gloves, coveralls, boots and/or other resistant protective clothing.

Have a safety shower/eye-wash fountain readily available in the immediate work area.

RESISTANCE OF PROTECTIVE CLOTHING: SODIUM HYDROXIDE: GOOD: Chlorinated

polyethylene (CPE), natural rubber, neoprene, nitrile/polyvinyl chloride (PVC), nitrile, polyethylene

(PE), PVC, polyurethane, styrene-butadiene rubber (SBR), Viton/chlorobutyl rubber, Silvershield,

SBR/neoprene FAIR/POOR: Butyl rubber

SODIUM HYDROXIDE SOLUTIONS, LESS THAN 30%: GOOD: PE, neoprene/natural rubber

SODIUM HYDROXIDE SOLUTIONS, 30-70%: VERY GOOD: Natural rubber, neoprene,

nitrile/PVC, nitrile, PE, PVC, Viton, Saranex GOOD: Butyl rubber, CPE, Viton/neoprene, butyl

rubber/neoprene, Teflon, natural rubber/neoprene/nitrile-butadiene rubber, SBR, neoprene/natural

rubber, neoprene/PVC FAIR/POOR: Polyvinyl alcohol, nonwoven PE

NOTE: Resistance of specific materials can vary from product to product. Evaluate resistance under

conditions of use and maintain clothing carefully.

PERSONAL PROTECTION COMMENTS Remove contaminated clothing promptly. Keep

contaminated clothing in closed containers. Discard or launder before rewearing. Inform laundry

personnel of contaminant's hazards. Do not eat, drink or smoke in work areas. Wash hands thoroughly

after handling this material. Maintain good housekeeping.

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9. PHYSICAL & CHEMICAL PROPERTIES

Appearance:

White deliquescent solid in small bead form

Odour threshold: Odourless

Specific Gravity: approx 1.1 - 1.5

Flash Point: Non-combustible (does not burn)

Flammability limits Non-flammable

pH: 12 (0.05% soln); 13 (1% soln); 14 (5% soln)

Solubility in water: Completely soluble

10. STABILITY AND REACTIVITY

INCOMPATIBILITY -MATERIALS TO AVOID:

STRONG ACIDS - may react violently.

METALS - reaction may produce flammable and explosive hydrogen gas.

ORGANOHALOGEN COMPOUNDS - may react to form spontaneously combustible compounds.

NITRO AND CHLORO ORGANIC COMPOUNDS - may react explosively.

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HAZARDOUS DECOMPOSITION PRODUCTS None

HAZARDOUS POLYMERIZATION Does not occur

CORROSIVITY TO METALS Corrosive to aluminium, tin, zinc. Corrosive to steel at elevated

temperatures.

Fire/Explosion Hazard:

EXPLOSION DATA - SENSITIVITY TO MECHANICAL IMPACT Not applicable

EXPLOSION DATA - SENSITIVITY TO STATIC CHARGE Not applicable

FIRE HAZARD COMMENTS Sodium hydroxide and its solutions will not burn or support

combustion. However, reaction of sodium hydroxide with a number of commonly encountered materials

(see Chemical Reactivity) can generate sufficient heat to ignite nearby combustible materials.

FIRE EXTINGUISHING AGENTS Use an extinguisher appropriate to the material which is burning

FIRE FIGHTING PROCEDURES Water can be used to extinguish a fire in an area where sodium

hydroxide is stored.

COMBUSTION PRODUCTS None

Fire fighters to wear full body protective clothing with breathing apparatus

11. TOXICOLOGICAL INFORMATION

Acute Effects:

Ingestion:

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There are no reported cases of industrial workers ingesting sodium hydroxide or its solutions. Should

ingestion occur, severe pain; burning of the mouth, throat and oesophagus; vomiting; diarrhoea; collapse

and possible

death may result.

Eye contact:

Extremely corrosive. Can penetrate deeply causing irritation or severe burns depending on the

concentration and duration of exposure. In severe cases, ulceration and permanent blindness may occur.

Skin contact:

Extremely corrosive. Capable of causing severe burns with deep ulceration. Can penetrate to deeper

layers of skin. Corrosion will continue until removed. Severity depends on concentration and duration

of exposure. Burns are not immediately painful; onset of pain may be minutes to hours.

Inhalation:

Effects of inhaling sodium hydroxide mists have not been clearly established. Most references indicate

that irritation of the nose, throat and lungs would occur due to the corrosive nature of sodium hydroxide.

However, there are no actual reports of industrial workers exposed to sodium hydroxide experiencing

these symptoms.

Long term Effects:

HEALTH EFFECTS There have been no documented effects due to long-term exposure to

sodium hydroxide.

CARCINOGENICITY Sodium hydroxide has been implicated as a cause of cancer of the oesophagus

in individuals who have ingested it. The cancer may develop 12 to 42 years after the ingestion incident.
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Similar cancers have been observed at the sites of severe thermal burns. These cancers may be due to

tissue destruction and scar formation rather than the sodium hydroxide itself. Not classed as a

carcinogen by Worksafe Australia.

TERATOGENICITY AND EMBRYOTOXICITY Insufficient information

TOXICOLOGICAL SYNERGISTIC MATERIALS Insufficient information

MUTAGENICITY Insufficient information

POTENTIAL FOR ACCUMULATION None

Toxicity Data:

ANIMAL TOXICITY DATA Lethal dose (rabbits, oral): 500 mg/kg. Irritant dose (rabbits, dermal):

500 mg/24 hours - severe skin irritant. Irritant dose (rabbits, ocular): 50 ug/24 hour - severe eye irritant.

More detailed information about the effects of chemicals on health can be obtained from NOHSC

Australia.

12. ECOLOGICAL INFORMATION

Avoid contaminating waterways.

13. DISPOSAL CONSIDERATIONS

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Refer to State Land Waste Management Authority. Decontaminate empty containers before disposal, by

triple rinsing with water, using rinse water in further processing or neutralize rinse water.

14. TRANSPORT INFORMATION

UN No: 1823

Proper Shipping Name: SODIUM HYDROXIDE SOLID

Class: 8

Packing Group: 2

Hazchem Code: 2X

EPG 8A1

Segregation not to be loaded with Classes 1, 4.3, 5.1, 5.2, 6, 7, Class 8 strong acids or

Dangerous Goods foodstuffs or foodstuff empties.

15. REGULATORY INFORMATION

Classified as hazardous according to the criteria of NOHSC, Schedule 6 poison according to SUSDP, Class

8 according to ADG

R-phrases: R35, causes severe burns and R41, risk of serious damage to eyes.

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S-phrases: S2, keep out of reach of children, S26, in case of contact with eyes, rinse immediately with

plenty of water and seek medical advice, S37/39, wear suitable gloves and eye/face protection.

16. OTHER INFORMATION

References:

(1) National Code of Practice for the preparation of MSDS [NOHSC:2011(1999), (2) List of Designated

Hazardous Substances [NOHSC:10005:1999] (3) ADG Code 6th Edition (4) Orica Chemicals Sodium

Hydroxide MSDS issued Feb 2000

Contact Point: Quality Assurance Manager Tel (02) 9807 4266

DISCLAIMER: All information given in this data sheet and by the company's technical staff is compiled from the best information currently available to the company.

The company accepts no responsibility whatsoever for its accuracy or for any results which may be obtained by customers. Any customer who relies upon any advice

or information given in this data sheet by the company or by its technical staff does so entirely at its own risk, and the company will not be liable for any loss or damage

thereby suffered notwithstanding any want of care on the part of the company or its staff in compiling or giving the advice or information.

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