Lab Manual Rxn Eng May-Aug2014

8/12/2019 Lab Manual Rxn Eng May-Aug2014

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CHEMICAL LABORATORY EXPERIMENTS

REACTION ENGINEERING

LABORATORY MANUAL

Lecturer/Instructor:

Name:

Student ID:

Course:

FACULTY OF ENGINEERING, ARCHITECTURE & BUILT

ENVIRONMENT

UCSI UNIVERSITY


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TABLE OF CONTENT

General Instructions

Experiment 1 Batch Saponification Reaction of Et (Ac) and NaOH

Experiment 2 The Effect of Step Change Input

Experiment 3 The Effect of Pulse Input for CSTRs in series

Experiment 4 Pulse Input in a Plug Flow Reactor

APPENDIX

A Batch Reactor

B CSTRs in series

C Tubular Flow Reactor


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(i) Title of the experiment

(ii) Date of the experiment carried out

(iii) Objective of the experiment

(iv) Hypothesis of the experiment

(v) Procedure outline or brief description of the method

(vi) Observation (should be recorded throughout the experiment)

A logbook should be neat. Clarification of procedure and results are

important. Always use a pen to write your logbook. For any mistake or changing

of the data written on the logbook, the usage of liquid paper or eraser is notallowed. Always use a pen to cross out if any errors.

The lab instructor/lecturer will inspect and sign your logbook during the

lab session and possibly grade them at the end of the semester.

(B) Laboratory groupYou will be assigned to a lab group (please refer to the student notice

board or outside the lab after the first session of the laboratory meet up). Studentsare not allowed to change their team member for lab. You are required to work

with you group members as much as possible in terms of understanding the lab

work and sharing information on the different sections that were performed by

different members.


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(C) Laboratory reportsi) Report submission

Report must be submitted one week after the scheduled experiment and

within the 1st 10 minutes of the due lab period. Marks would be deducted

accordingly for late reports or may not be accepted. Students who caught blatantly

copying from other or involved in any plagiarism activities will be required to

resubmit their work, or otherwise zero marks will be given.

i i) Report style/formatLab report must be in hand written or typed. Each of the group members

must contribute in the report. Report should contain the following:

Front page (refer the at Appendices A)

Table of content

Objective

Introduction/background of the experiment

Material and Methodology

Results and discussion

Conclusion

Limitation of the Experiment

Reference

Appendix (if any)

Lab reports are to be assembled in a logical and orderly way. Tedious

calculations must be placed in sequential order in the report. The report shall be:


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(i) Written in passive tense.Example: Five milligram of solid was weighted.

(ii) Graph must be with title, axis labels with units and legend whennecessary. The scale of the graph should be adjusted to fit the

graph data.

(iii) Plagiarism will not be allowed and tolerated.(iv) Use suitable analysis method during explanations for the graph

such as R-value, slope of the line, line equations, etc in explaining

the experiment.

(v)

Only chemical compound structures can be drawn usinghandwriting.

Report outlines and marks distributions:

Introduction/

Background

3% Contain a concise summary of the experiment that is carried

out. Includes the statement of purpose, an introduction into

technique used and a brief overview of the instrumentation.

Material&

Methodology

3% Contains all relevant experimental procedures, materials and

instrument parameters used in the analysis or during the

experiment.

Results&

Discussion

5% -Show all the results from the experiment by using graph,

diagram, table, etc. All the data must be at appropriate

units. The calculation should shows in systematic basis.

Show only one example calculation for repeat data trials.

Include statistical analysis if any. All results must be

expressed to correct significant figures and in correct units.

-Explanation of the figures or graph or data should followed

by supporting reference or relevant/logical analysis.

Conclusion 2% Conclusion should reflect an understanding of the chemical


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theory involved and achievement of the experiment

objective.

Limitation of

the

experiment

2% It may include the limitation of the technique or

methodology of the experiment based on literature study.

Includes also any error that encounter during the experiment

is carried out. Suggest for improvement to avoid error.

Reference 3% A minimum of 3 references should be cited in the

experiment report.

Format 2% Front page, table of content, reference writing style, graph,

figure, table, etc.

(D) Laboratory RulesAll the laboratory rules already learned will be applicable all the time and

the students are required to comply with all the rules when there are in the

lab.

1. Wear closed shoes, lab coat and eye protection (goggles) at all the time whilein the laboratory.

2. DO NOT wear bulky clothes or loose sleeves and long pants. Wear suitableattire for lab work. Those with long hair do tie it before entering the lab.

(lecturer/instructor preserve the right to not allow student who not follow this

rule from enter the lab)3. Switch off your hand phones.4. Always be punctual. Students who come later than 15 minutes will not

allowed to perform the experiment.


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5. Eating and drinking in the lab are strictly prohibited in the lab.6. Students must have a towel (for cleaning purposes), a logbook and their lab

manual during the lab session.

7. Clean your bench and return all the apparatus to their respective places beforeyou leave the lab.

8. Read the lab manual and understand the lab before you going to the lab.9. Use only the amount of the reagents required. Avoid wastage.10.Dispose of excess reagents as instructed, never return excess reagents into the

bottle.

11.Make sure you know where the following safety devices are: eyewash station,emergency shower, fire extinguisher, fire alarm station.

12.Clean up the broken glass and report to the lab instructor or lecturerimmediately.

13.Always follow the instruction of the lab instructor or lecturer before start thelab.

14.Do not casually dispose chemicals into the sink. Some chemicals may washeddown the sink, while others may require a different method of disposal. If a

chemical can go in the sink, be sure to wash it away rather than risk an

unexpected reaction between chemical 'leftovers' later.


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EXPERIMENT 1: Batch Saponification of Et(Ac) and NaOH

OBJECTIVES

- To carry out a saponification reaction between NaOH and Et(Ac) in abatch reactor .

- To determine the reaction rate constant.

PROCEDURES

1. Perform the general start-up procedures as in Appendix A.2. To begin a batch reaction experiment, close valve V3 and V7, switch on

pump P2 and open valve V8 to obtain highest possible flow rate into the

reactor .Fill reactor R1 with 0.1 M Et(Ac) to 1-L volume .Stop pump P2 .

3. Switch on pump P1 and open V4 to obtain highest possible flow rate intothe reactor .Fill reactor R1 with the 0.1 M NaOH until solution reaches a

total of 2-L volume .Stop pump P1.

4. Switch on stirrer M1 and start the timer immediately.5. Record the conductivity values at 1 minute interval.6. Stop the experiment when the conductivity values remain constant (i.e.

steady state condition).

7. Open valve V10 and drain all the solution from the reactor into waste tankB4.


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ANALYSIS AND DISCUSSION

Solution mixture volume = ____________

Initial concentration of NaOH in the reactor vessel = ____________

Initial concentration of Et(Ac) in the reactor vessel = ____________

Time, t

(min)

Conductivity

QI01 (mS/cm)

Concentration

NaOH, CA(M)

Conversion, X

(%)

ln CA dCA/dt ln dCA/dt

1

2

3

4

5

6

7

8

9

10

11

12

13

14

15

16

17

18

19

20


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1. Use the sample table for data collection.2. Plot a graph of conversion vs. time.3. For an equimolar reaction with the same initial reactants concentration

( 0= 0) , the rate law is shown to be :

-= -

=

ln (-

) = ln k + a ln

is the concentration of NaOH in the reactor at time t.

4. Plot a graph of ln (

) vs. ln and evaluate the slope and y-axis

intercept.

5. Determine the order of the reaction, and the rate constant, k from the slopeand the intercept values.


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EXPERIMENT 2: The Effect of Step Change Input

OBJECTIVES

- In this experiment a step-change input would be introduced and theprogression of the tracer will be monitored via the conductivity

measurements in all the three reactors.

PROCEDURES

1. Perform the general start-up procedures as in Appendix B.2. Fill up the feed tank B1 with deionised water .Open V1 and V2.3. Prepare about 30L of 0.025 M sodium chloride solution in feed tank B2.4. Set the 3way valve V5 position towards pump P1.Close valve V7.5. Open valves V6 and V13 .Switch on Pump P1 to initially fill up all three

reactors with deionised water .Record each reactor volume.

6. Regulate the pump speed to obtain a flow rate of approximately 150ml/min on flow meter FI01.Make sure that no air bubbles are trapped in

the piping and conductivity probe, hence will affect the reading.

NOTE: It is important to maintain the liquid level in each reactor .Adjust

the flow rate is necessary.

7. Switch on stirrers 1, 2 and 3 and set the speed 200 rpm.8. Continue pumping the de-ionized water until all conductivity readings

(QI01,QI02 AND QI 03) are stable at low values. Make sure that the

overflow piping is free from the air bubble.

NOTE: Regulate the drain valve to make sure the solution flowing inside

the overflow tube.

9. Record these conductivity values at time, 0.


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10.Switch off pump P1 .Quickly set the 3way valve V5 position towardspump P2 .Switch on pump P2 and start the timer simultaneously.

11.Regulates the pump speed, to maintain the flow rate at 150 ml/min on flowmeter FI01.

12.Record all conductivity values (QI01,QI02 AND QI03) at a suitableinterval (e.g. 1 minute ) in an appropriate table.

13.Continue recording the conductivity values until all readings are almostconstant.

14.Switch off pump P2.Close valves V5.15.

Drain all liquids in each reactor by opening valves V10 to V14.


Flowrate of Deionized water from tank = _________

Flowrate of NaCl from tank = _________

Speed of stirrer M1, M2 and M3 = _________

C0 = _________

Record the conductivity readings for the three CSTRs in series (QI01 ,QI02 AND

QI03 )

Time (min) Q1 (mS/cm) Q2 (mS/cm) Q3 (mS/cm)

0

2

4

6

8

10

12


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14

16

18

20

22

24

26

28

30

32

34

36

On the same graph, plot all 3 conductivity readings against time, together with the

step change input. Observe the transient behavior in the three CSTRs in series and

discuss.


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EXPERIMENT 3: The Effect of Pulse Input for CSTRs in series

OBJECTIVES

- In this experiment a pulse input would be introduced and the progressionof the tracer will be monitored via the conductivity measurements in all

the three reactors

PROCEDURES

1. Fill up the feed tank B1 with deionised water. Open V1 and V2.2. Prepare about 30L of 0.025M Sodium Chloride solution in feed tank B2.3. Set the 3-way valve V5 position towards pump P1. Close valve V7.4. Open valve V6 and V13. Switch on pump P1 to initially fill up all three

reactors with deoinised water. Record each reactor volume.

5. Regulate the pump speed, P1 to obtain a flow rate of approximately 150ml/min on flow meter FI01. Make sure that no air bubbles are trapped in

the piping, overflow tube and conductivity probe, hence will affect the

reading.

NOTE: It is important to maintain the liquid level in each reactor. adjust

the flow rate is necessary. If air trap inside the overflow tube, adjust drain

valve.

6. Switch on stirrers 1, 2 and 3 and set the speed to 200 rpm.7. Continue pumping the de-ionized water until all the conductivity readings (QI01,

QI02 and QI03) are stable at low values.

8. Record these conductivity values at time, to9. Switch off pump P1. Quickly set the 3-way valve V5 position towards pump P2.

Switch on pump P2 and start the timer simultaneously.

10.Regulates the pump speed, to maintain the flow rate at 150 ml/min on flow meterFI01.


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11.Let pump P2 run for 5 minutes and then switch off pump P2. Set the 3-way valveV5 towards P1. Switch on pump P1 back and let it run till the end of experiment.\

12.Record all conductivity values (QI01, QI02 and QI03) at suitable interval (e.g 1minute) in an appropriate table.

13.Continue recording the conductivity values until all readings are almostconstant.

14.Switch off pump P2. Close valves V5. 15.Drain all liquids in each reactor by opening valves V10 to V14.


Flowrate of distilled water from tank = ________

Flowrate of NaCl from tank = ________

Speed of stirrer M1, M2 and M3

CO

Record the conductivity readings for the three CSTRs in series (QI01,

QI02 and QI03)

Time (min) Q1 (mS/cm) Q2 (mS/cm) Q3 (mS/cm)

0

2

4

6

8

10

12

14

16

18


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20

22

24

26

28

30

32

34

36

On the same graph, plot all 3 conductivity readings against time, together with the

pulse change input. Observe the transient behavior in the three CSTRs in series

and discuss. Thus, compare this experiment with previous experiment 2. What can

you discuss about both effect?


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11.Continue recording the conductivity values until all readings are almostconstant and approach the stable low level values.


Flowrate =

Input type =

Time Conductivity (mS/cm) Time Conductivity (mS/cm)

(min) Inlet Outlet (min) Inlet Outlet

0.0

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

4.5

5.0


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APPENDIX A : BATCH REACTOR

General Start-up Procedures

1. Prepare the following solutions:a) 15 liter of sodium hydroxide, NaOH (0.1 M) in tank B1.b) 15 liter of ethyl acetate, Et (Ac) (0.1 M) in tank B2.

2. Ensure that all valves are initially closed except by-pass valves V3, V7and V14.

3. Fill water bath tank B3 with water. Close the water bath tank.4. Turn on the power for the control panel.5. Switch on the stirrer M1 and adjust the knob to obtain a speed of 200 rpm.

Switch off the stirrer M1.

6. Open valves V2, V6 and V13.7. The unit is now ready for experiment.

General Shut-down Procedures

1. Keep the cooling water to continue flowing.2. Switch off pumps P1, P2 and P3. Switch off stirrer M1.3. Switch off both heaters W1 and W2. Let the liquid in the reaction vessel

R1 to cool down to room temperature.

4. Turn off the power for the control panel.5. Keep the solutions for subsequent experiment. Otherwise, open valves V1

to V8 to drain all solutions from feed tanks B1 and B2.

6. Open valves V10 to drain any liquid from reactor R1 into waste tank B4.


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APPENDIX B : CSTR IN SERIES


1. Ensure all the valves are closed initially.2. Prepare a 30-L of salt solution (e.g. sodium chloride, NaCl; 0.025 M).3. Fill the feed tank B2 with the NaCl solution.4. Turn on the power for the control panel.5. Connect the water de-ionizer to the laboratory water supply. Open valve

V16 and fill up feed tank B1 with de-ionizer water. Close valve V16.

6. Open valve V3 and V6. Switch three way valve V5 to the left side towardspump P2. Switch on pump P2. Regulate speed of pump to obtain a flow

rate of approximately 150 ml/min at flow meter FI-01. Switch off pump

P2. Drain all liquid from the three reactors.

7. Open valve V1. Switch three way valve V5 to the right side towards pumpP1. Switch on pump P1. Regulate speed of pump to obtain a flow rate of

approximately 150 ml/min at flow meter FI-01. Allow the de-ionized

water to overflow from reactor R3 until the conductivity value stabilizes atlow value. Switch off pump P1.

Note:Make sure there is no bubble trap inside the overflow reactor, if air

bubble blocks the flow, regulate the drain valve.

8. The unit now is ready for experiments.


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1. Switch off both pumps P1, P2. Close valves V1 and V3.2. Open valves V10 to V14 to drain all liquid into waste tank.3. If the equipment is not going to be used for long period of time, drain all

liquid for both feed tanks by opening valves V1 to V5. Rinse the feed

tanks with clean water.

4. Turn off the power for the control panel.


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APPENDIX C : TUBULAR FLOW REACTOR


1. Ensure that all valves are initially closed except valve V7.2. Prepare a 20 liter of salt solution (e.g. sodium chloride, NaCl; 0.05 M).3. Fill the tank B2 with the NaCl solution.4. Connect the water de-ionizer to the laboratory water supply. Open valve

V19 and fill up feed tank B1 with the de-ionized water. Close valve V19.

5. Turn on the power for the control panel.6. Open valves V2 and V10. Switch on pump P1. Adjust P1 to obtain a flow

rate of approximately 150 ml/min at flow meter FI-01. Close valves V10

and switch off pump P1.

7. Open valves V6 and V12. Switch on pump P2. Adjust P2 to obtain a flowrate of approximately 150 ml/min at flow meter FI-02. Close valves V12

and switch off pump P2.

8. The unit is now ready for experiment.


1. Switch off both pumps P1, P2 and P3. Close valves V2 and V6.2. Switch off the heaters.3. Keep the cooling water circulating through the reactor while the stirrer

motor is running to allow the water jacket to cool down to room

temperature.

4.If the equipment is not going to be used for long period of time, drain allliquid from the unit by opening valves V1 to V16. Rinse the feed tanks

with clean water.

5. Turn off the power for the control panel

Documents

Lab Manual Rxn Eng May-Aug2014