Nazarbayev University
Chemical Reaction Engineering
Laboratory manual
Fall 2017
SAFETY 1
EXPERIMENTAL PROTOCOL ERROR! BOOKMARK NOT DEFINED.
REPORT STRUCTURE 4
FORMS 5
STATEMENT OF DUE DILIGENCE 8
RISK ASSESSMENT FORM 9
Safety
Before starting the experiment read carefully the present manual and the instrument manual. If
you have any questions, ask the Supervisor or the Teaching Assistant.
Wear safety coat, gloves and googles, and apply any other required measures according to the
instructors request. Keep the lab tidy and clean up everything with deionized water after the
experiment.
Before starting the experiment sign the Statement of Due Diligence.
Experiment 1: Determination of the reaction kinetic rate by using a batch reactor
Objective
The objective of this lab exercise is the determination of the reaction constant k and the overall
reaction order, which are necessary for the relevant calculations and the elaboration of the
experimental data in the next lab exercises.
Materials and Equipment
400 ml of a solution of ethyl acetate (concentration is given during the lab)
400 ml of a solution of sodium hydroxide (concentration is given during the lab)
batch reactor (maximum volume 0.95 lt)
Experimental Procedure
The procedure to carry out this practice is:
1. Prepare glass beakers with 400 ml of solutions of sodium hydroxide and ethyl acetate.
2. Switch the batch reactor system on.
3. Measure the conductivity with a sensor of the sodium hydroxide solution from the beaker.
4. First introduce inside the batch reactor the solution of sodium hydroxide with the help of the
funnel through the hole.
5. Record the conductivity and the temperature every 30 seconds for 15 minutes.
6. Take note of the results on the table.
7. At the end of the experiment, empty the reactor and clean it with water several times.
8. Rinse measuring sensor with water.
9. Switch the system off.
Results and Tables
1. With the data obtained, complete the following table using the formula bellow to calculate the
percentage conversion of the reactants:
= (1 ) 100%
Time (min) Conductivity ( ) Reaction Temperature (oC) % Conversion
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
6.5
7.0
7.5
8.0
8.5
9.0
9.5
10.0
10.5
11.0
11.5
12.0
12.5
13.0
13.5
14.0
14.5
15.0
2. With Plot the graph of the % conversion versus time.
3. Find the reaction constant k and the overall reaction order.
Report structure
Prepare a report containing the following parts at least:
Title
Objective
Materials and Equipment
Experimental Procedure (containing all your actual measurements)
Process Flowsheet
Results and Tables (completed)
Questions (with answers)
Conclusion
References
Before delivery, the Teaching Assistant should sign on the first page that the data contained
correspond to the ones stored in the PC and that no plagiarism has been attempted.
Experiment 2: Determination of reaction conversion versus space time in a
continuous-stirred tank reactor (CSTR)
Objective
The objective of this lab exercise is to determine the effect of space time on the reaction
conversion in the liquid phase reaction between sodium hydroxide and ethyl acetate in CSTR.
Materials and Equipment
3 l of a solution of ethyl acetate (concentration is given during the lab)
3 l of a solution of sodium hydroxide (concentration is given during the lab)
CSTR (Parameters of the reactor: L x W x H = 470 x 400 x 380 mm)
Experimental Procedure
The procedure to carry out this practice is:
1. Fill two beakers with 1.5 l distilled water
2. Adjust the overflow on the tank such that the measuring sensor is immersed approx. 30
mm in the liquid with the tank filled.
3. Switch on the unit at the master switch.
4. Switch on the chemical pumps and adjust both to maximum rate till water level in reactor
reaches overflow.
5. Switch off the second pump and adjust the first pump to flow rate of approx. 20%. Find
out volumetric flow rate with 50 ml beaker measuring the volume of water, which passes
per unit time. Do the same at 50% and 100%.
6. Empty the reactor.
7. Prepare glass beakers with 1 l solutions of sodium hydroxide and ethyl acetate.
8. Insert the conductivity measuring sensor in the measuring opening on the lid.
9. Switch on the chemical pumps and adjust both to maximum rate till water level in reactor
reaches overflow.
10. When the liquid level reaches the overflow, switch on the stirrer and adjust to a
maximum speed.
11. Adjust both pumps to flow rate of approx. 20%. At regular intervals of approx. 20-30
seconds, log the conductivity and reaction temperature indicated on the measuring unit
until stable values are reached. Do the same at 50% and 100%.
12. Take note of the results on the table.
13. Switch off chemical pumps and stirrer.
14. At the end of the experiment:
- empty the reactor and rinse out with distilled water
- rinse measuring sensor with water
- operate both chemical pumps with water to clean them
15. Switch off the unit.
Results and Tables
Pumps in % Volumetric Flow Rate (mL/min)
Pumps in % Conductivity (mS/cm) Conversion (%)
1. Determine the reaction rate constant at a different flow rates. What is expected?
2. Estimate the space time in every case.
3. Plot the pump volumetric flow rate versus % capacity. Evaluate the quality of calibration
curve.
4. Plot conversion versus space time. Explain the results obtained. 1. What is a CSTR? Present
the basic design equation.
Questions
1. What is a CSTR? Present the basic design equation.
2. Describe the relationship between residence time, space time, and conversion.
Report structure
Prepare a report containing the following parts at least:
Title
Objective
Materials and Equipment
Experimental Procedure (containing all your actual measurements)
Process Flowsheet
Results and Tables (completed)
Questions (with answers)
Conclusion
References
Before delivery, the Teaching Assistant should sign on the first page that the data contained
correspond to the ones stored in the PC and that no plagiarism has been attempted.
FORMS
STATEMENT OF DUE DILIGENCE
No student will be allowed in the lab without agreeing to and signing the statement below. Please
hand it directly to your lab instructor.
To ensure that research laboratory activities are carried out safely,
I, ____________________ (print name)
am fully aware that safe and correct procedures are an important part of the laboratory
component of research, and I have read and understood the present safety manual.
I understand that I am responsible for conducting myself in a safe manner, becoming aware of
and informed about special hazards of technique, apparatus or chemicals in the chemical
laboratory, and will conform to any additional safety instructions presented orally or in writing
by the instructor or contained in posted instructions or safety memoranda that are distributed.
I understand that although every reasonable precaution is taken to ensure safety in the laboratory,
working with hazardous materials and doing potentially hazardous procedures, is a normal part
of life in the research laboratory.
I also understand that while in the lab I need to wear appropriate eye protection and clothing at
all times, as outlined in the lab manual. I will ask questions about any safety issues that I am
unsure about.
I agree that all accidents or incidents (near misses) must be immediately reported the laboratory
technicians and coordinator.
Furthermore, I understand that I can be dismissed from the laboratory, possibly permanently, for
safety infractions.
Name:
Date:
Signature:
RISK ASSESSMENT FORM
Adapted from the Brunel University and University College of London (UK) Risk Asessment Forms and
includes elements of the BioCOSHH Form published by the Newcastle University Microbiological
Hazards and Genetic Modification Safety Advisory Sub-Committee (UK)
Project/experiment title: Review Date:
Chemical Reaction Engineering Laboratory 09.10.2017
Course (teaching labs)/Researcher name (only for research/project activities) :
Chemical Reaction Engineering
Researcher email address :
[email protected]Supervisor: Stavros G. Poulopoulos
Emergency contact: Stavros G. Poulopoulos
Persons at risk (names): Students, Teaching Assistant
Summary of project/experiment and objectives:
The objective of the first lab exercise is the determination of the reaction constant k and the overall reaction
order, which are necessary for the relevant calculations and the elaboration of the experimental data in the
next lab exercises.
The objective of the second lab exercise is to determine the effect of space time on the reaction conversion in
the liquid phase reaction between sodium hydroxide and ethyl acetate in CSTR.
Location of work/Laboratory number: Block 6 / 6.154
Existing containment Level (BSL):
BSL 1 BSL 2 BSL 3 BSL 4
Specific project hazards (include both likely and unlikely):
Physical (e.g. lifting heavy objects) : Cutting with broken glass equipment.
Chemical (e.g. corrosive acids, fumes) : Sodium hydroxide, very hazardous in case of skin contact (corrosive,
irritant, permeator), of eye contact (irritant, corrosive), of ingestion, of inhalation.
Ethyl acetate, Hazardous in case of ingestion, of inhalation. Slightly hazardous in case of skin contact (irritant,
permeator), of eye contact.
(irritant).
Biological (e.g. pathogens): None
Electrical (e.g. shock, laser) : Highly unlikely
Biosafety Risk Assessment
No biological agents and hazards are involved.
Potential routes of exposure
Select all that
Inhalation Ingestion Injection Absorption Other
apply
Use of biological agents or hazards
Small scale Medium scale Large scale Fieldwork Animals Plants Select all that
Other apply
Frequency of use
Daily Week Monthly Other Select one
Maximum amount or concentration used
Negligible Low Medium High Select one
Levels of infectious aerosols
Negligible Low Medium High Select one
Potential for exposure to biological agents or hazards
Negligible Low Medium High Select one
Who might be at risk
Staff Students Visitors Public Other
Assessment of risk to human health (Prior to use of controls)
Level of risk Effectively zero Low Medium/low Medium High Select one
Current Risk controls (e.g. PPE, fume hood/ventilation etc):
Lab coat Lab gown Surgical scrubs Disposable clothing
Apron Spectacles Goggles Face shield
Gloves Special headwear Special footwear Full face respirator
Disposable mask Filter mask Half face respirator Other (specify below)
Additional controls needed (e.g. adibodies test, vaxination, training, supervision etc) :
None.
Risk Estimation Matrix (after implementation of controls)
Severity of harm Likelihood of harm
High Medium Low Negligible
Severe High High Medium Effectively zero
Moderate High Medium Medium/low Effectively zero
Minor Medium/low Low Low Effectively zero
Negligible Effectively zero Effectively zero Effectively zero Effectively zero
High Risk: Unacceptable under existing control measures, activities must be suspended and requires immediate
action.
Medium Risk: Manageable under risk control & mitigation, requires supervisor/management decision
Low Risk: Acceptable after review of the activities, requires periodic monitoring
Effectively zero Risk: Acceptable with continued data collection and trending for continuous improvement.
All three signatures needed before work can start :
Supervisor: Stavros G. Poulopoulos, Associate Professor Sign:
Lab Technician: Dastan Nurmukhambetov, Lab Sign:
Technician
