skf 4761process control laboratory...lab module: skkk 3721 pollution control & chemical reaction...

LAB MODULE SKKK 3721

POLLUTION CONTROL & CHEMICAL REACTION

ENGINEERING LABORATORY

Name :

Course :

Semester :

Section :

Group :

Lab Instructor :

School of Chemical & Energy Engineering

Faculty of Engineering

UNIVERSITI TEKNOLOGI MALAYSIA

LAB MODULE: SKKK 3721 Pollution Control & Chemical Reaction Engineering Laboratory

Table of Content ITEM PAGE General Lab Safety Procedures 3 Guideline for Lab Proposal 5 Guideline for Lab Report 6 Course Outline 9 Experiment 1: Iodine Reaction 13 Experiment 2: Saponification of Ethyl Acetate and Sodium Hydroxide in CSTR 18 Experiment 3: Cyclone Separator 27 Experiment 4: Ambient Air Quality Measurement 31 Experiment 5: Coagulation & Flocculation 33 Experiment 6: Biodiesel Synthesis 35 Experiment 7: Water Quality Analysis 36


GENERAL LABORATORY SAFETY PROCEDURES

BASIC PRECAUTIONS Awareness is the most fundamental rule of chemical safety. Take time to understand the safety and health hazards of the chemicals in the workplace. Every laboratory worker should take the following precautions:

Assume that unfamiliar chemicals are hazardous.

Review the safety and health hazard data of all chemicals used in the laboratory.

Know the signs and symptoms of overexposure and the physical and sensory characteristics (odour, appearance) of these chemicals.

Know appropriate procedures for emergencies, including the location and operation of all emergency equipment.

Avoid distracting or startling others.

When working with hazardous materials, have a second person nearby, or, at minimum, maintain surveillance by telephone contact.

Avoid leaving experiments unattended.

Never use unlabeled chemicals or chemicals whose labelling is suspect.

Always order or use the least amount of chemical required.

Use appropriate personal protective equipment at all times. Wear proper lab attire for lab works; wearing lab coat and shoes is a MUST.

Use hazardous chemicals in a chemical fume hood, whenever possible.

Maintain equipment and inspect it regularly for proper function.

Use guards and shields where possible. All mechanical equipment should have adequate guarding.

Use safety shields when there is a possibility for explosion or implosion.

Store and handle chemicals in properly in accordance with the chemical manufacturer's guidelines.

Store hazardous waste in a closed, labelled container as provided in the lab.

Avoid pouring chemical waste materials into the sink.

Do not eat, drink, smoke, chew gum or apply cosmetics in the laboratory.

Do not store food or beverages in the laboratory or in a chemical refrigerator.

Do not mouth pipette. Use a mechanical pipette or aspirator.

Do not use chipped or cracked glassware.

Report all accidents, even if they do not result in injury, to the principal investigator, laboratory supervisor and/or technicians immediately.

HYGIENE The following housekeeping and hygiene practices should be implemented at all times to reduce the likelihood of accident or chemical exposure:

Work areas should be kept clean and free from obstruction.

Hands should be washed after every experiment, before touching any non-contaminated area or object, and before leaving the laboratory area.

Access to exits, emergency exits, aisles, and controls should never be blocked.

Emergency exits should be kept unlocked from the inside.

Stairways and hallways should not be used as storage areas.

Work areas should be cleaned at the end of the experiment and at the end of the day. CHEMICAL STORAGE AND HANDLING Many potential hazards are associated with the storage and handling of laboratory chemicals. These hazards may be minimized by understanding the properties of the chemicals and by developing procedures by which they may be handled safely. Simply storing chemicals alphabetically is not


prudent. Flammable, corrosive, explosive, and peroxide forming agents require special precautions. Storing incompatible chemicals together may have disastrous results. The following guidelines are prudent for all chemical storage and handling:

Chemical handling: Use bottle carriers to transport chemicals. Close caps securely. Pour all chemicals carefully. Add acid to water, not water to acid.

Labels: Be sure all labels are securely attached and legible. Keep chemicals in their original containers if possible. Label all secondary containers to avoid unknown chemicals and/or inadvertent reaction. Date all chemicals, which may become unstable over time or are peroxidizable.

Shelves: Do not store chemicals on hard-to-reach shelves. Labels on stored chemicals should be able to be read easily. Shelves should be made of a chemically resistant material and should have a 2-inch lip or side rails.

Incompatible chemicals: Incompatible chemicals should not be stored together. For each chemical, the hazardous nature must be considered individually and in relation to other chemicals in the area.

Excessive storage: Avoid stockpiling chemicals. Purchase only what is needed. Use older stock first. Discard chemicals that are no longer needed or that have expired.

Fume hoods: In general, fume hoods should not be used for storage of chemicals, unless the chemicals are part of the experiment being conducted in the fume hood at that time. The exception is storage in a fume hood, which is specifically designed for that storage, and where experimental procedures are not carried out.

EMERGENCIES Be sure you know the location and method of operation of the nearest eye wash, safety shower, fire extinguisher, spill kit and fire alarm pull station. Be sure that emergency telephone numbers are posted or otherwise accessible.

Spill If flammables are involved, extinguish ignition sources. Clean the spill, only if the spill is manageable, you have been trained and you have appropriate cleanup materials. If you are unable or do not attempt to clean the spill, prevent the spread if possible, evacuate the area, close the lab door, and alert others or sound alarm. Communicate with your supervisor and technicians immediately.

Fire Extinguish the fire if it is small, contained, you have been trained and you have an appropriate fire extinguisher available. If you are unable to extinguish the fire, then pull the nearest fire alarm and evacuate the building via the nearest exit. Communicate with your supervisor and technicians immediately.

Chemical Exposure o Splash to skin or eyes: flush with water at least 15 minutes using a safety shower or eye wash

and seek immediate medical attention. o Injection: control bleeding, wash with soap and water and seek immediate medical attention. o Ingestion: seek immediate medical attention. o Inhalation: stop emission if possible, alert others or sound alarm, get fresh air and seek

immediate medical attention. Communicate with your supervisor and technicians immediately for the occurrence of any emergency cases.


GUIDELINE FOR LAB PROPOSAL

Lab Proposal or lab preparation report is a formal draft of portions of the Final Report. It must be handwritten and submitted at the end of the lab hours during the lab preparation week for the corresponding experiments. It should include roughly the introduction, overall methodology, analysis, experimental plan and anticipated results. Planning for delegation of task (role playing) when the experiment is in progress must also be included. The content of lab proposal attest to your understanding of the experiment, its context in theory, and a suitable approach to performing the experimental work as well analyzing the results. A properly prepared lab proposal will save much time in the later phases of the experiment and will reduce the chances of errors in data collection and analysis. The lab proposal must be handwritten and prepared on the experimental sheet. It must be clear, concise and specific, but its specific contents will depend largely on the actual experimental work that you will be doing. Descriptions with the assistance of charts and/or diagrams, instead of 100% wordy sentences, are very much encouraged. The lab proposal should consist of the following sections: 1. Cover Page The cover page should be prepared on the given standard template. 2. Introduction This section should cover the background of the experiment under investigation. Typically there is a brief explanation on the problem statement, objective of experiment, scope of experiment and the significance of experiment in the context of knowledge and its application. 3. Overall Methodology Overall methodology should outline the planning of the whole learning process in order to accomplish the experiment. Flow chart of overall methodology can be presented in this section. You should also include roughly the experimental procedures and associate the description with suitable illustration. 4. Analysis If there are mathematical equations/correlations needed, specific methods to analysis the results, software to be used, etc. – they should be defined in this section. Propose and explain calculation procedure that you think it will be used later on. If model/simulation/computer program will be used or built, describe what will be done, why you need it and how the model/simulation will be used. 5. Experimental Plan Basically, experimental plan identifies the list of data/information needed and variables to be investigated along with their methods of measurement. In addition, any essential data that can be obtained before doing the experiment must be identified and put in this section. You should also include the outline of team plan in order to accomplish the experiment, and the statement of task delegation among the team members before, during and after the experiment. 6. Anticipated Results Briefly discuss the relevant anticipated results and the manner in which you intend to present them. Prepare sketches of tables or figures with the expected trends and justify them. Discuss why you anticipate these results.


GUIDELINE FOR LAB REPORT

Basically, your Final Lab Report should tell what you did, why you did it, what you learned and the significance of your results. The report does not have to be extremely long. In fact, the key to writing an excellent report lies in presenting concisely your response to the objectives of the project and justifying that response with appropriate documentation. The final lab report should consist of the following sections: 1. Cover Page The cover page should be prepared on the given standard template. 2. Abstract The abstract is the report in miniature. It summarizes the whole report in one, concise paragraph of about 100-200 words. As distinguished from the introduction, the abstract tells the reader what will be done and lays the groundwork. Also, the abstract summarizes the report itself, not the actual experiment. Hence, you cannot write the abstract until after you have completed the report. Before writing the abstract, it is often helpful to summarize each section of the report (introduction, literature review, methodology, results, discussion, and conclusion) in one sentence. Then try to arrange this information into a short paragraph. Remember, the abstract should be a precise and specific summary. 3. Introduction Pertinent background and explanatory information about your experiment must be presented if your audience is to ‘connect the dots’ of later sections of your report. Introduce the objective of experiment, scope of experiment and the significance of experiment as what you have done in your Lab Proposal with the necessary improvement. 4. Literature Review/Theory The literature review and/or theory section is a brief review of relevant ideas from the major field and a more intensive coverage of the experiment at hand – in your own words. Only pertinent articles or textbook materials relevant to the assigned experiment are cited. The underlying physical principles, laws and governing equations relevant to the problem are presented in here. The literature may reveal conflicting views and opinions on the topic; these are included in the review in an unbiased way. State the assumptions and limitations of the theory, if any. Charts, diagrams, and other exhibits may be used in developing and explaining the theory, especially if they aid clarity and conciseness. 5. Methodology This section gives details of how the experiment is accomplished. This is a rewrite – in proper tense, with any needed additions, corrections and improvements – of the Lab Proposal. Assumption and justification involved while doing the experiment and preparing the report may also included. Importance and information on precautious/safety aspect of the experiment may also be highlighted and discussed, if any. This rewrite should now reflect the actual experimental work done by your team, and thus be consistent with the upcoming results and discussion sections. 6. Results The results section delivers the evidence that will help answer the questions raised by the objective and scope of experiment, should prepare readers for the more detailed upcoming discussion, and justify the conclusions that will be drawn later on. Observations, data and calculated results (in consistent units) are often presented best as graphs or charts, particularly if it will be important to illustrate trends. However, tables make sense when you need to present accurate data and specific facts or demonstrate the relationships between numerical


and/or descriptive data. Figures and tables should include – whenever possible – published, theoretical, and/or model/simulation values available from the literature or produced programmatically. Tables of raw experimental data are not placed in this section; they are reported in appendices. Other results that do not relate directly to the upcoming discussion should either be reported in the appendices. Data are often summarized or reduced/condensed for presentation. Reducing the data allows generalizations to be made and trends to be pointed out. Obviously, then, charts and tables must be accompanied by appropriate text. Every figure or table itself is numbered and supplied with a brief but descriptive title or caption. Build graphics and other visual displays so that, with their accompanying text/description, they are self-explanatory. The text must briefly explain how the results were obtained from the experimental data, the associated quantitative uncertainty (e.g., confidence limits, standard error, etc. if necessary), references to appropriate equations or sample calculations, and any critical assumptions or approximations made in obtaining the results. However, best practice in bringing together your exhibits and your words is accomplished by referring readers to graphics explicitly and telling them what trends to notice. 7. Discussion If the results section delivers the evidence, the discussion section makes the case in court. It must answer and reflect to the objective and scope of experiment. In the discussion section, you explain what your experimental results mean by relating them to the concepts and ideas presented in the introduction and literature review/theory sections. There are many questions that could be answered in this section so you should not limit yourself to those offered here as examples. Answer the questions that make most sense for your work.

Do the results agree with theory, with the work of others, with models/simulation? If so, how? If not, why not? Can the disagreement be explained?

What are the most probable sources of experimental error and have these affected your ability to draw conclusions? How might these errors have been reduced or eliminated?

Did your results reveal problems with the experimental plan, method, or equipment? How might these be improved?

Were your assumptions suspect or reliable?

What definite conclusions can you draw from your results? What conclusions are more speculative?

What implications do your results have on theory and/or current industrial practices?

What questions remain unanswered? What questions should be answered next? In this section, you may also criticize the lab experiment and make recommendations or improvement. Such criticisms and recommendations, however, should focus on the lab as a learning process; mere complaints about faulty equipment or amount of time spent are not appropriate. 8. Conclusion Draw conclusion from the results and discussion that answer the objective and scope of experiment. Then go on to explain your conclusions that summarizes and reflects the results and discussion. 9. Nomenclature All symbols and acronyms used in the report and its appendices must be listed and defined in a nomenclature section with the consistent set of units used for calculation/reporting of results. Symbols are arranged in alphabetical order, Latin terms (e.g., a, b, D, Re, Pr, etc.) first, followed by Greek (e.g., α, β, ρ, etc.), and finally subscripts (e.g., i, j, k, etc.). Greek and subscript sets are headed by the titles ‘Greek’ and ‘Subscripts’. In addition to the nomenclature section, introduce these symbols where they first appear using either running text or a list set off from the running text. If a dozen or fewer symbols are used in this report, you may rely on the in-text introduction of symbols and acronyms alone and forego a separate nomenclature section altogether.


10. References The references section includes all references from which material in this report was taken. It does not include materials consulted but not cited. It does include citations listed in any appendix document (e.g., citing of handbooks from which properties data have been taken). A report without ANY cited literature is typically not a credible piece of work. Citing the literature typically strengthens any case you are making in your own reporting. The in-text citations themselves should give the page number(s) relevant to the actual material cited. The in-text citation plus the full reference in the references section make it possible for the reader to find the material. The referencing format should follow the one that is standard for UTM. 11. Appendices Appendices may include raw data, calculations, graphs, and other quantitative materials that were part of the experiment, but not reported in any of the above sections. Refer to each appendix at the appropriate point (or points) in your report. For example, at the end of your results section, you might have the note, See Appendix A: Raw Data Chart.

LAB REPORT SCHEME

Section Marks

1 Cover page

2 Abstract 10

3 Introduction 10

4 Literature review / theory 10

5 Methodology 10

6 Results 10

7 Discussion 30

8 Conclusion 10

9 Nomenclature

10 References 5

11 Appendices

12 Formatting 5


COURSE OUTLINE

Lecturer :

Room No. :

Telephone No. :

E-mail :

Prerequisite : SKL 3223 Chemical Reaction Engineering and SKL3413 ( co requisite)

Synopsis : This laboratory course contains experiments that are covered basis concept in

chemical reaction engineering and pollution control such as kinetic analysis of

reaction, ambient air and water quality analysis. All experiments require students

to apply fundamental laboratory techniques and skills as well as communication

skill. Students, in group will demonstrate a mastery of laboratory techniques and

clearly describe the qualitative and quantitative aspects of the experiments

performed.

LEARNING OUTCOMES

Course Mapping on Bloom Taxonomy of Course Outcome

No. Learning Outcomes Program learning

outcomes

Bloom

Taxonomy

Assessment

1. Conduct the experiment to determine

the reaction rate and order of reaction

of a batch chemical reaction

PO3 C4, P4, A3

Lab Report

2. Analyze experimental data to calculate

rate law and order of reaction.

PO2, PO3 C4, P4, A3 Lab Report


the performance of a cyclone

PO3, C4, P4, A3 Lab Report


the quality of air based on standard

parameters

PO2 PO3, C4, P4, A3 Lab report


the performance of coagulation &

flocculation

PO3, C4, P4, A3 Lab Report

6. Orally present and describe the

procedure of experiment and then

carried out the experiment for biodiesel

production.

PO6 C4, P4, A3 Presentation

Lab Report


the quality of water based on standard

parameters and orally present the

outcomes

PO6 C4, P4, A3 Presentation

Lab Report

STUDENT LEARNING TIME

Teaching and Learning Activities Student Learning Time (hours)

1. Face-to-Face Learning

a. Lecturer-Centered Learning

i. Lecture

b. Student-Centered Learning (SCL)


i. Laboratory/Tutorial

ii. Student-centered learning activities – Active Learning, Project Based Learning

28

12

2. Self-Directed Learning

a. assignment, module, e-Learning

b. Revision

c. Assessment Preparations

3. Formal Assessment

a. Continuous Assessment

b. Final Exam

Total (SLT) 40

TEACHING METHODOLOGY

Independent Study, group work, group report and oral presentation

EXPERIMENT SCHEDULE

EXPERIMENT Topic Topic Outcomes

Experiment 1 Iodine Reaction

Laboratory activity to conduct iodine reaction I, II and III

Data collection of time consumption in the reaction

Data manipulation and analysis to calculate order of reaction , reaction rate constant and Activation Energy

Analysis of temperature effect to reaction rate constant

It is expected that students have the ability

to:

determine rate of a reaction , order of reaction and Activation Energy from collected data

identify some of the factors that control reaction rate

Experiment 2 Saponification Process Of Ethyl

Acetate With Natrium Hydroxide

solution

Laboratory activity on saponification process

Data collection of reactant consumption during the reaction by titration technique

Data calculation to determine order of reaction and reaction rate constant


to:

Prepare Natrium Hydroxide solution for a given concentration

Determine rate of reaction and order of reaction of saponification process


Experiment 3

Cyclone Performance

Study on the effect of inlet

flowrate on the cyclone

performance


to:

Describe in details the

fundamental principle in the

operation of a cyclone

Examine on the effect of inlet

flowrate on the cyclone

performance

Experiment 4

High volume sampler

Study the ambient air

quality sampling


to:

Determine quality of ambient air around the university area and make comparison with Malaysia’s Daily Standard value for suspended solid in the air

Experiment 5

Coagulation & Flocculation

Study on the performance of coagulation and flocculation technique towards turbidity reduction


to:

Analyze wastewater sample and determine the turbidity reduction of the sample

Experiment 6

(3 weeks)

Bio diesel production from Palm oil

Literature review of 5 articles

Methodology presentation

Experimental work

Lab report


to:

Search and summarize the literature on bio diesel

Propose the methodology of bio diesel production

Conduct experiment on bio diesel production

Experiment 7

(3 weeks)

Water Quality Determination

1. BOD5 2. COD 3. Turbidity 4. Nitrogen Content


to:

Interpret and understand a PBL experiment;

Propose the suitable methods based on standard parameters to analyze water sample;

Conduct analysis on the water sample to obtain its quality


REFERENCES : 1. Fogler, H.S., “Elements of Chemical Reaction Engineering”, 4th

Edition, Prentice

Hall,

New Jersey, 2006.

2. Davis, M.E and Davis, R.J, “Fundamentals of Chemical Reaction Engineering”,

Graw-

Hill, New York, 2003

3 Davis, M.L. and Cornwell, D.A., "Introduction to Environmental Engineering",

McGraw Hill, 4th ed, 2007

GRADING

No. Assessment Number % each % total Dates

1 Lab report 7 10 70

2 Presentation 2 10 20

3 Test 1 10 10

Overall Total 100

NOTES:

Students are responsible to submit all lab report on time. Failure to do that will be penalised.

Lab briefing will be given during week 2 of the semester.

Experiment work will start from week 3.

Lab reports should be submitted not later than 1 week after the experimental work.


EXPERIMENT 1

IODINE REACTION

OBJECTIVE OF EXPERIMENT In this experiment, you will study the reaction kinetics and rate laws of “iodine clock reaction”. It is a reaction that proceeds at an easily measured rate at room temperature. SCOPE OF EXPERIMENT

1. To investigate the effects of reactant concentration and reaction temperature on the rate of reaction.

2. To determine the reaction orders and rate constant of iodine reaction. 3. To determine the activation energy and Arrhenius constant of iodine reaction.

DESCRIPTION OF EXPERIMENT Reaction Mechanisms In this experiment, the kinetics of reaction between persulfate S2O8

2- and iodide I

- ions is investigated:

S2O8

2- + 2I

- 2SO4

2- + I2 (1)

persulfate iodide slow sulfate iodine

Rates of reaction are measured by either following the appearance of a product or the disappearance of a reactant. In this experiment, the rate of consumption of the persulfate and iodide ions will be measured indirectly to determine the rate of the reaction. As reaction (1) runs, which is a slow reaction, the amount of iodine (I2) produced from it will be used instantaneously in reaction (2): 2S2O3

2- + I2 S4O6

2- + 2I

- (2)

thiosulfate iodine fast tetrathionate iodide

The iodine produced from the persulfate-iodide reaction (1) is immediately reduced back to iodide by thiosulfate ions (2). A known amount of thiosulfate ions will be added to the reaction vessel which will in turn consume iodine as it is produced. This continues until all the thiosulfate has been converted to tetrathionate, whereupon accumulation/excess of iodine will start to form in the solution via reaction (1). Since the amount of thiosulfate added is known, the amount of iodine produced from reaction (1) can be determined stoichiometrically. When all the thiosulfate is consumed, accumulated iodine starts to form in solution. By measuring the time taken for the known amount of thiosulfate to be consumed, the rate of production of iodine during that time can be calculated. The colour of the accumulated iodine formed might be intense enough that it can act as its own indicator. However, for better results, starch will be added, which produces a deep blue starch-iodine complex: I2 + (C6H10O5)n • H2O (C6H10O5)n • H2O–I2 (3)

iodine starch fast blue complex

Although three reactions are involved, the reaction between persulfate and iodide ions (reaction 1) is the one of interest. The second reaction (reaction 2) is only used to delay the reaction between iodine and starch (reaction 3). In other words, all of the thiosulfate must be consumed before the colour changes. Without the thiosulfate ions present, the iodine molecules produced from the first reaction would slowly build up and the solution would gradually darken, making it difficult to identify a definitive point at which the reaction is over or complete.


In summary, iodide (I

-) and persulfate ions (S2O8

2-) react to produce iodine (I2) and sulfate (SO4

2-) in

reaction (1). This iodine is immediately consumed by the thiosulfate ions (S2O32-

) in a pathway described by reaction (2). As soon as all of the S2O3

2- ions are consumed, the excess iodine

produced in (1) is free to react with starch, turning into the blue complex solution (3). The amount of thiosulfate ions added will determine the amount of iodine has been produced in the time taken for the reaction to turn into blue complex. Rate Equation The rate of reaction at constant temperature and ionic strength can be expressed as the change in concentration of a reagent or product over the change in time and can be equated to the rate law expression:

t

][I =

t

]O[S

][I]Ok[Sdt

]d[I

dt

]Od[S rate

2

82

nm2

82

2

82

It will be necessary to know or measure Δ[S2O8

2-] (the initial change in concentration of S2O8

2- ions),

and Δt, the time elapsed during the change, as well as the initial concentration of S2O82-

and I- ions. A

way to obtain the Δ[S2O82-

] by coupling another reaction (reaction 2) to the one we are studying (reaction 1). Reaction (2) is the reduction of I2 as fast as it is formed by S2O3

2- ion. Only when S2O3

2-

ion is gone, the reaction complete and I2 will accumulate. The variation in concentration of persulfate (a minus sign denotes consumption) and the variation in concentration of iodine (production) are basically given by: Δ[S2O8

2-] = [S2O8

2-]final – [S2O8

2-]initial = 0 – [S2O8

2-]initial = – [S2O8

2-]added

Δ[I2] = [I2]final – [I2]initial but at the beginning of reaction [I2]initial = 0 , so: Δ[I2] = [I2] final Then:

time solution volume

I of moles

t

][I rate 22

The number of moles of iodine produced is given by the amount of thiosulfate added to the reaction vessel: moles of I2 = moles of S2O3

2- = (volume of S2O3

2- added) x (concentration of S2O3

2-)

The stoichiometry of reaction (2) gives:


OS of (moles 1/2

t

][I rate

2

322

)

*The ½ denotes that in a certain period of time, 1 mole of iodine produced is equivalent to 2 mole of thiosulfate consumed. Since the moles of thiosulfate used is known, then the moles of iodine used can be calculated by simply divided the moles of thiosulfate with 2. The we can calculate the rate by:


)OS of tion(concentra added) OS of (volume 1/2

t

][I rate

2

32

2

322


This reaction rate is a measure of how much iodine is produced in the time it takes for the reaction to turn into blue complex (i.e., time taken to react with all of the thiosulfate present). Reaction Orders In this experiment, the initial rate method will be used to find the order of reaction with respect to persulfate (m) and the order of reaction with respect to iodide (n). The method is based on the measurement of the rate of reaction over a period of time. This time period is short enough for the reaction not to have proceeded significantly, but long enough to be unaffected by the time which the solutions take to mix at the start of the reaction. The rate law equation can be written as:

nm2

82 ][I]Ok[S rate

By taking the natural log of both sides, the equation becomes: ln rate = ln k + m ln[S2O8

2-] + n ln[I

-]

For runs with different concentrations of persulfate and a constant concentration of iodide at a constant temperature, ln rate = ln k + m ln[S2O8

2-] + constant

The constant term in this equation is (ln k + n ln[I

-]). The slope of the best fit line of a plot of (ln rate)

versus ln[S2O82-

] will be equal to m, the order of reaction with respect to persulfate. Similarly, for runs where persulfate concentration and temperature are kept constant and the amount of iodide is varied, ln rate = n ln[I

-] + constant

The constant term in this equation is (ln k + m ln S2O8

2-]). The slope of the best fit line of a plot of (ln

rate) versus ln[I-] will be equal to n, the order of reaction with respect to iodide.

Activation Energy (Ea) and Arrhenius Constant (k) Recall the Arrhenius equation: k = A.exp(-Ea/RT) By taking the natural log of both sides, the equation becomes:

Aln T

1

R

E k ln a

A plot of ln k versus 1/T yields a straight line whose slope is -Ea/R and whose y-intercept is ln A, the natural log of the Arrhenius constant. EXPERIMENTAL PROCEDURES You will be provided with the following solutions:

Sodium thiosulfate, Na2S2O3 solution (1M) ~ 6.25/40 g/L

Potassium persulfate, K2S2O8 solution (2.5%) ~ 25g/L

Potassium iodide, KI solution (5%) ~ 50g/L

Starch solution (1%)


First Experiment: Dependence of reaction rate on the concentration of reactants Scope: Determination of reaction orders (m and n) and rate constant (k) Experimental procedures for the first experiment are described according to Table 1 and Table 2. The first experiment must be conducted at similar and constant reaction temperature. Part I: Determination of reaction order with respect to persulfate ion (m)

1. Clean up all beakers and flasks with distilled water. 2. For data set in Table 1, soak a conical flask that contains K2S2O8 solution in a water bath at a

temperature around 35oC – 40

oC. Wait until the K2S2O8 solution has a similar temperature as

the water bath. 3. Fill in 30mL of KI solution into another conical flask. Add certain amounts (refer Table 1) of

Na2S2O3 solution, starch solution and distilled water into another conical flask that contains 30mL KI solution. This particular mixture denotes your reaction medium.

4. Soak the reaction medium in the same water bath. Be sure to stir the reaction medium with a magnetic stirrer until it reaches the water bath temperature.

5. Once the K2S2O8 solution and reaction medium are at the similar temperature (as the water bath), pipette the K2S2O8 solution into the reaction medium. Start the stopwatch at the first drop of K2S2O8 solution into the reaction medium.

6. Stop timing when the reaction medium turns into a deep blue complex colour. Part II: Determination of reaction order with respect to iodide ion (n) Repeat the experiment for the set of data in Table 2, for different amount of KI solution and distilled water, whereas the amount of K2S2O8 solution is kept constant. Second Experiment: Dependence of reaction rate on the reaction temperature Scope: Determination of activation energy (Ea) and Arrhenius constant (k) Repeat the experiment for the set of data in Table 3 at different reaction temperature.


Experiment 1: Iodine Reaction Table 1. Preparation of solutions to determine the reaction order with respect to persulfate ion (m)

Conical Flask Exp. Run #1 #2 #3 #4 #5

Reaction Medium Starch solution (mL) 5 5 5 5 5

Distilled water (mL) 50 45 40 25 15

Na2S2O3 solution (mL) 10 10 10 10 10

KI solution (mL) 30 30 30 30 30

In Pipette K2S2O8 solution (mL) 5 10 15 30 40

Total (mL) 100 100 100 100 100

Time (min)

Table 2. Preparation of solutions to determine the reaction order with respect to iodide ion (n)




Na2S2O3 solution (mL) 10 10 10 10 10

KI solution (mL) 5 10 15 30 40


Total (mL) 100 100 100 100 100

Time (min)

Table 3. Preparation of solutions to determine the activation energy (Ea) and Arrhenius constant (k)




Na2S2O3 solution (mL) 10 10 10 10 10

KI solution (mL) 5 5 5 5 5


Total (mL) 100 100 100 100 100

Reaction Temperature (oC) 35 40 45 50 60

Time (min)


EXPERIMENT 2

SAPONIFICATION OF ETHYL ACETATE AND SODIUM HYDROXIDE IN CSTR OBJECTIVE OF EXPERIMENT In this experiment, you will study the saponification reaction of sodium hydroxide and ethyl acetate in a continuous stirred-tank reactor (CSTR). SCOPE OF EXPERIMENT

1. To carry out the saponification reaction between sodium hydroxide and ethyl acetate in a CSTR.

2. To investigate the operational behaviour of a reaction in CSTR. 3. To calculate the reactant conversion based on the conductivity calibration curve. 4. To verify the reaction order obtained from the hypothesis of the experiment using graphical

technique (concentration vs. time data) and analytical technique (design equation of CSTR); compare the results from both techniques.

5. To determine the rate constant of saponification reaction between sodium hydroxide and ethyl acetate using graphical technique (from concentration vs. time data) and analytical technique (from design equation of CSTR); compare the results from both techniques.

6. Compare the reaction kinetics, rate law and conversion in a batch reactor to the one in a CSTR system for the same reaction.

DESCRIPTION OF EXPERIMENT Reaction Mechanisms The stoichiometry of the saponification reaction between sodium hydroxide (NaOH) and ethyl acetate (EA, CH3OOOC2H5) is:

NaOH + CH3OOOC2H5 CH3COONa + C2H5OH (1)

Sodium Hydroxide

Ethyl Acetate

Sodium Acetate

Ethyl Alcohol

Assume that the initial concentration of sodium hydroxide is equal to the initial concentration of ethyl acetate. The reaction kinetics and rate law of saponification reaction in a CSTR can be determined using conductivity calibration curve. Overall conductivity in a reaction mixture is the constituent of sodium hydroxide and sodium acetate conductivities, which determine the composition of both chemicals, respectively. The conductivity calibration curve represents the conversion-conductivity relationship of the reaction mixture, and provides a mean to get concentration vs. time data. From this graph, conversion of the reactant at 0%, 50% and 100% conversions can be determined based on the conductivity of the reaction mixture at 100% reactant, 50% reactant – 50% product, and 100% product, respectively.


Figure 1. Conductivity calibration curve

Design Equation of CSTR Saponification between sodium hydroxide (NaOH, denotes as A) and ethyl acetate (EA, denotes as B) is basically second order elementary reaction. For a steady-state constant volume isothermal CSTR, the design equation is:

A

Aoo

r

XCV

where V is the reactor volume, X is the reactant and υo is the total volumetric flow rate feeds into the

reactor. For a elementary-bimolecular second order reaction, the rate equation is:

BAA CkC -r

Basically, reactant conversion, X, can be calculated using the following equation:

Bo

B

Ao

A

C

C1X

C

C1X

The design equation of a CSTR also can be written in terms of initial concentrations, reactant conversion, reactor volume and feed flow rate. Thus, we need to use the relations:

AoBoAoBoB

AoA

CC whenX),(1CX)(1CC

X)(1CC

Therefore,

22

AoA X)(1kC -r

If we combine the above equations, we see that

22

Ao

Aoo

X)(1kC

XCV

Conductivity (μS)

Conversion

1.0

0.0


And further simplified to

2

Ao

o

X)(1kC

XV

EXPERIMENTAL PROCEDURES You will be provided with the following solutions:

Sodium hydroxide (NaOH) 0.1M

Ethyl acetate (EA) 0.1M

1. Prepare conductivity calibration curve using three points: i. X = 0.0, use 10mL 0.1M NaOH ii. X = 0.5, use a mixture of 5mL 0.05M NaOH and 5mL 0.05M sodium acetate iii. X = 1.0, use 10mL 0.1M sodium acetate

2. Ensure that all valves are closed. (Note: DO NOT change anything on V4 and V5 as they are recycle streams to the feed tanks)

3. Prepare 9L solution of 0.1M NaOH (8g per 2L H2O) and 9L solution of 0.1M EA (19.6mL per 2L H2O), and pour these solutions into feed tanks T1 and T2, respectively.

4. Switch on pumps P1 and P2, and stirrer S1. Adjust the feed flow rates into the CSTR to be at 40cm

3/min using valves F1 and F2. Start the stopwatch immediately as you switch on the

pumps and stirrer. Measure conductivity and temperature of the reaction medium in the CSTR for every 2 minutes for over 30 minutes.

5. When liquid level inside the CSTR reach 2000cm3 (2L), record the space time, and measure

conductivity and temperature of the reaction medium. 6. Then, flow the reaction medium into the buffer tank by opening valve V3. Continue take

measurement for 10 minutes. 7. Close valves F1 and F2, and stop pumps P1 and P2. Discharge all liquids through valve V4. 8. Repeat the experiment for different feed flow rates: 60, 100 and 120 cm

3/min.

9. Once all experiments are done, discharge all residual NaOH and EA. 10. Clean-up the pilot plant.


Experiment 2: Saponification of Sodium Hydroxide and Ethyl Acetate in a CSTR Table 1. Calibration Data

Calibration Data

0.1M NaOH

0.05M NaOH

+ 0.05M Sodium Acetate

0.1M Sodium Acetate

Conversion

0.0

0.5

1.0

Conductivity (μS)


Experiment 2: Saponification of Sodium Hydroxide and Ethyl Acetate in a CSTR Table 2. Experimental Data: Flow Rate = 40cm

3/min

Time, t

(min)

Conductivity

(μS)

Temp.

(oC)

Conversion

(mol)

CA

(mol/L)

CB

(mol/L)

CB

(mol/L)

CD

(mol/L)

0

2

4

6

8

10

12

14

16

18

20

22

24

26

28

30

CA: concentration of NaOH CB: concentration of EA CC: concentration of sodium acetate CD: concentration of ethyl alcohol



3/min

Time, t

(min)

Conductivity

(μS)

Temp.

(oC)

Conversion

(mol)

CA

(mol/L)

CB

(mol/L)

CB

(mol/L)

CD

(mol/L)

0

2

4

6

8

10

12

14

16

18

20

22

24

26

28

30



Experiment 2: Saponification of Sodium Hydroxide and Ethyl Acetate in a CSTR Table 6. Experimental Data: Space Time

Flow Rate

υo

(cm3/min)

Space Time

τ

(min)

Conductivity

(μS)

Temp.

T (oC)

Conversion

X

40

60

100

120


EXPERIMENT 3

CYCLONE SEPARATOR OBJECTIVE OF EXPERIMENT In this experiment, you will study the effect of inlet velocity towards efficiency and pressure drop of a single cyclone separator. SCOPE OF EXPERIMENT

1. To carry out an experiment of particle capture using a single cyclone separator 2. To investigate the effect of velocity on the efficiency and pressure drop of a cyclone separator

DESCRIPTION OF EXPERIMENT

Cyclone separator is one of the practical centrifugal particle collectors and it is probably the most widely used in the world. As shown in Figure 1, a cyclone consist of a vertical cylindrical body, with a dust outlet it the conical bottom. The gas enters through a rectangular inlet, arranged tangentially to the circular body of the cyclone. The gas spirals around the outer part of the cylindrical body with a downward component, then turns and spirals upward, leaving through the outlet at the top of the device. During the outer spiral of the gas, the particles are driven to the wall by centrifugal force, where they collect, attach to each other, and form larger agglomerates that slide down the wall by gravity and collect in the dust hopper in the bottom. The cyclone separator is usually employed for removing particles 10µm in size and larger. However, conventional cyclones seldom remove particles with an efficiency greater than 90 percent unless the particle size is 25µm or larger.

Very small cyclone have been used to collect small particles from very small gas flows for research and gas-sampling purposes, but the industrial problem is to treat large gas flows. Several practical schemes have been worked out to place large number (up to several thousand) small cyclones in parallel, so that they can treat a large gas flow, capturing smaller particles. The most common of these arrangements, called a multiclone.


Figure 1: Schematic diagram of a cyclone

Equations

1. Cyclone Efficiency

2. Pressure drp

Where,

∆P = Pressure drop, N/m2

Vi = Inlet Velocity, m/s

ρg = air density, kg/m3

3. Inlet Velocity Head


Where,

K = Cyclone configuration constant

De = Outer diameter of a cyclone, m

A = Cross-sectional Area of inlet cyclone, m2

4. Inlet Velocity

Where,

Q = Inlet flow rate

Cyclone Dimension The cyclone system models that are used for this experiment have two cyclones (C1 and C2) with 100mm and 78mm in diameter. The relative dimensions for these cyclones are according to the Swift design, given by: EXPERIMENTAL PROCEDURE The objective of this experiment is to investigate the effect of inlet velocity towards efficiency and pressure drop of a single cyclone separator.

1. Place a clean filter paper inside the captured particle box (S1). This is to avoid any particles from inserting the pump system.

2. Make sure the cyclone separator is in a good condition and its entire component is paired correctly. Check if there is any particle inside the cyclone system.

3. Weight accurately the empty collector bottle (H1). 4. Place the 3-way valve (V3, V4, V5, and V6) in order to get flow rate A (cyclone C1

operation). Refer to Figure 2. 5. Turn on the pump and adjust the glop valve with flow rate of 10m

3/hour.

6. Weight 100gm of the particle sample. Make sure valve V2 is close and pour the entire

particle sample inside the sample container F1.

7. Slowly, release the particles into the cyclone system by opening valve V2.

8. Record the pressure drop (∆P) and pressure gauge (G1) value.

9. Turn off the pump right after the sample container F1 is empty.

10. Open the collector bottle and weight the mass of the particle collected.

De = 0.40D De = 0.40D S = 0.50D La = 1.40D Lb = 2.50D H = 0.44D W = 0.21D


11. Check the filter paper. If you noticed the filter paper is about to clog, replace it with a new one.

12. Repeat steps 2 to 11 with flow rate of 14, 18, 22, and 26m3/hour.

RESULTS 1.0 Plot in the same graph:

(a) ∆P versus ƞ (b) Q versus ƞ

2.0 Plot Vi2 versus ∆P

3.0 Find the K value (cyclone configuration constant) and make a comparison with the K value obtain from Figure 2. State the reason if both of the value is different.

4.0 Discuss the effect of the inlet velocity towards efficiency and pressure drop of a cyclone.

Q (m

3/hour)

∆P (cmH2O)

Win (g)

Wc (g)

Vi (m/s)

ƞ (%)

10

14

18

22

26

* Win = Mass of feed particle ** Wc = Mass of particle collected


EXPERIMENT 4

AMBIENT AIR QUALITY MEASUREMENT

OBJECTIVE OF EXPERIMENT In this experiment, you will study the quality of the ambient air in UTM using a High Volume Air Sampler (HVS). SCOPE OF EXPERIMENT

1. To determine the concentration of suspended solid in UTM’s ambient air and compare it with the standard Malaysia TSP value.

2. To determine whether the quality of the ambient air in UTM is in a safe level. . DESCRIPTION OF EXPERIMENT

An air pollutant is known as a substance in the air that can cause harms to humans and the environment. It may cause respiratory diseases and reducing life expectancy of human. Pollutant can be in form of solid particles, liquid droplets, or gases.

Air pollutants can be classified as either primary or secondary. Primary pollutants are substances directly emitted from a process, such as ash from a volcanic eruption. While secondary pollutant forms in the air when primary pollutants react or interact. The concentration of suspended particle is usually expressed as µg/m

3 which is the mass of suspended particles per meter cube of

volume air. Suspended solid is measured by using a High-Volume Air Sampler (HVS). Large volumes of

air are drawn through a filter by a pump. This procedure is usually done continuously for 24 hours. The Total Suspended Particle (TSP) standard for Malaysia is 260 µg/m

3.

Equation Where, W2 = Weight of filter paper after sampling, g W1 = Weight of filter paper before sampling, g Q = Volumetric flow rate inlet air HVS, m

3/hour

t = Time for sampling, hour 10

6 = Conversion from g to µg

EXPERIMENTAL PROCEDURE Apparatus: High-Volume Air Sampler, filter paper

1 Weight the filter paper (W1) and put it inside the HVS. 2 Close the HVS and turn on the pump. 3 Record the time and the air flow rate. 4 Leave it approximately for 4 hours and record the final weight of the filter paper (W2).


RESULTS & DISCUSSION

1. Calculate the TSP for this experiment. Compare the obtain value with the standard Malaysia STP value. Discuss the differences.


EXPERIMENT 5

COAGULATION & FLOCCULATION

OBJECTIVE OF EXPERIMENT In this experiment, you will study the treatment of waste water using coagulation & flocculation method. SCOPE OF EXPERIMENT

1. To determine the effectiveness of coagulation & flocculation methods towards reduction of turbidity.

2. To investigate the optimal amount of coagulant. DESCRIPTION OF EXPERIMENT All type of water, especially surface water, contains both dissolved and suspended particles. In wastewater treatment operations, the process of coagulation and flocculation are used to separate the suspended solid.

Coagulation involves the addition of chemical (coagulants) during relatively intense mixing to destabilize naturally occurring particles and macromolecules and to precipitate additional particles. An example of coagulant that is often used is aluminium sulfate.

In flocculation, a period of less intense mixing is used to promote the aggregation of destabilized particles into larger flocs that can be removed subsequently by sedimentation or filtration. During coagulation and flocculation, various dissolved ions and molecules may be adsorbed by particles or may be precipitated, depending on the type and concentration of species.

EXPERIMENTAL PROCEDURE

1. Shake well the plastic jar that contains the wastewater sample. 2. Measure turbidity in NTU and pH of the sample. 3. Fill in 1L of sample in six different beakers and label all beakers with number 1-6. 4. Use beaker 1 as the control beaker. 5. Weight the coagulant (Al2(SO4)3 or FeCl3 ) according to these dosage:

Beaker Number Amount of Coagulant (g)

1 0.0

2 0.2

3 0.4

4 0.6

5 0.8

6 1.0

6. Lowered the paddles in each beaker and set the paddles speed at 250rpm. When the

speed is stable, pour the coagulant in side each beaker simultaneously. Leave the mixing for 1-3 minutes (Record the starting time).

7. Change the paddles speed to 30 rpm for 30 minutes for flocculation process. 8. After 30 minutes, remove the paddles and leave the mixture to settle for another 30

minutes.


9. Take a sample from each beaker by using a syringe. Measure the turbidity and pH for each sample.

DISCUSSION 1. Find the optimal amount of coagulant for this experiment 2. Why we need to slow down the paddles speed in Step 7?


EXPERIMENT 6

BIODIESEL SYNTHESIS OBJECTIVE OF EXPERIMENT (3 WEEKS) In this experiment, you will study the lab-scale production of biodiesel from palm oil, methanol and sodium hydroxide. WEEK 1: Seek info on biodiesel production. WEEK 2: Propose an acceptable route to synthesis biodiesel from palm oil, methanol and sodium hydroxide. Then, plan your experimental work in a proposal. Your experimental work should study the effect of certain variables in the reaction. Therefore, prepare at least two samples of experiment. The lab proposal should contain the following items:

background of experiment,

objective of experiment,

scope of experiment,

literature review on lab-scale production of biodiesel,

overall methodology,

apparatus and materials used, experimental procedures,

list of mathematical equations/correlations needed,

identification of data needed, and

anticipated results. In your proposal, concise description with the assistance of charts and/or diagrams, instead of wordy sentences, is very much encouraged. WEEK 3: During lab week, carry out the proposed experiment and record the data needed. In your lab report, discuss the effects of variables being studied on the production of biodiesel.


EXPERIMENT 7

WATER QUALITY ANALYSIS OBJECTIVE OF EXPERIMENT (3 WEEKS) In this experiment, you will analyse the quality of UTM’s lake water sample. WEEK 1: Seek info on type of analysis that can be used for water analysis. WEEK 2: Propose at least 4 types of water analyses for water quality measurement. Then, plan your experimental work in a proposal. The lab proposal should contain the following items:

background of experiment,

objective of experiment,

scope of experiment,

literature review on type of water analysis

overall methodology,

apparatus and materials used, experimental procedures,

list of mathematical equations/correlations needed,

identification of data needed, and

anticipated results. In your proposal, concise description with the assistance of charts and/or diagrams, instead of wordy sentences, is very much encouraged. WEEK 3: During lab week, carry out the proposed experiment and record the data needed. In your lab report, discuss the quality of UTM’s lake water.

skf 4761process control laboratory...lab module: skkk 3721 pollution control & chemical reaction...

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