UNIVERSITI MALAYSIA SABAH
SCHOOL OF ENGINEERING & INFORMATION TECHNOLOGY
CHEMICAL ENGINEERING PROGRAMME

LAB MANUAL

KC 31001 LABORATORY 6

Semester 2 2016/2017

Venue:
Makmal Tindakbalas, Makmal Unit Operasi, Makmal Kawalan,
Makmal Bioproses

Lecturer:
Hafeza Abu Bakar

Lab. Assistants:
En. Freddy, En. Razis, Ms. NorAemi, Ms. Chen Moi Fong

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Contents

No. Titles Pages
1. Laboratory safety 3
2. Laboratory reports and assessment 5
3. Experiments
BP1 Preparation of culture media and isolation of pure culture 8
BP2 Characterization of bacteria and establishing pure cultures 12
BP3 Quantification of cell number 15
CRE1 Kinetic studies in batch reactor 20
CRE2 Isothermal continuous stirred tank reactor (iCSTR) 24
SP1 Determination of adsorption isotherm for citric acid 30
SP2 Solid-liquid extraction (SLE) 36
SP3 Batch distillation on a binary mixture 41
PC1 Liquid/water flow control (WF) 49
PC2 Liquid/water level flow control (WLF) 60

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Laboratory Safety in General

These guidelines are meant for safety awareness in the laboratory. However, specialized
laboratory may require specific safety rules. Good management of laboratory is important to protect
laboratory personnel/users against hazards at work.

1. Laboratory Safety awareness
- Everyone is responsible for his or her own safety and the safety of others while working in the
laboratory.
- Before working with a chemical, assessment must be made of its hazards and risk.
- Be familiar with appropriate protection measure when you are working with the following:
û Flammable substances
û Corrosive and toxic chemicals
û Biohazards
û Radioactive materials
û Compresses gases
- Laboratory should be adequately ventilated.
- Chemical storage areas should be cool, dry, well ventilated and away from sunlight.
- Eating, drinking, and smoking are strictly prohibited in laboratories, as well as stores and
workshops.

2. Personal Protection
- Laboratory coat, safety goggles and gloves (if needed) should be worn all the time in the
laboratory.
- Always assure that you wash your hands before leaving the laboratory.
- Short skirts, shorts and open-toed shoes/sandals should not be worn in the laboratory to avoid
skin exposure.

3. Fire Hazards and hazardous chemicals
- Always store flammable liquids in appropriate safety cabinets/cans.
- Do not store incompatible reagents together, e.g. flammables and acids. Segregate acids and
bases, and corrosive materials from organic and flammable materials.
- Wear appropriate protective equipment such as laboratory coat, apron, gloves and eye protection
gear when you are working with flammable, corrosive and toxic chemicals.
- Ensure that no ignition sources present nearby while working with flammable chemicals.
- All electrical cords should always be in good condition. Electrical outlets should be grounded.
- Do not store ethers for long periods to avoid formation explosive peroxides.
- Corrosive chemicals can burn and irritate tissue. If inhaled or ingested, it may affect lung and
stomach tissue.
- Avoid mixing oxidizing chemicals with other chemicals during disposal.
- Careful when dealing with carcinogens (cancer causing agent). Suspected carcinogens (please
check for a full list): chloroform, benzidine, benzene, methylchloromethyl ether, vinyl chloride,
acrylonitrile, formaldehyde, etc.
- Never use lubricants on valve regulators of compressed gases.

4. Laboratory Housekeeping
- All equipment should be inspected carefully before used.
- Equipment and work bench must be cleaned after use.
- Use non-chromate cleaning solution if possible. Make sure cleaning is done in the fume hood if
sulphuric acid glass cleaner is used.

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. . Keep laboratory floor dry at all times.Always check that flames and compressed gas supplies are shut off when not in use and end of day. (ii) solvent spills – apply activated charcoal and mix thoroughly until material is dry. Perform artificial respiration if victim is not breathing.Avoid experimental work in an unoccupied space/building if possible. move the victim out for fresh air. . tie up and label.Contact the laboratory personnel or University safety officer immediately when emergency happens. give water.All laboratory personnel/users must be familiar with the location and uses of the safety devices in and around the laboratory. .Upon inhalation of hazardous chemicals.Upon ingestion of chemicals. do not give fluids. CPR might be needed. . name of researcher/student and contact number. stating the experiment. place in fume hood. .For chemical spills: (i) acid spills – apply neutralizer or add water if necessary and check mixture with indicator for neutralization. If unconscious. Transfer mixture into plastic bag. Any spills must be immediately attended to. 6. Emergency Procedures . Contact laboratory personnel for disposal. If nauseated. for example: ü Safety shower ü Fume hood ü Fire extinguisher ü First aid kit ü Eye wash station ü Fire alarm .Always place a note should any unattended experiments must be carried out. After Hours/Long Hours Experiment . 4     . 5. if victim is awake.

5     . every group should submit only one full report. The lab report should be submitted to my room (Bilik No 56.Laboratory Reports and Assessment General Guidelines 1. result. Late report submission without reasonable reasons will cause mark deductions. 4. they should reschedule the time with the lab technician and please inform me on the date. The date will be notified later. Lab report is due in a week for each completed experiment. Every member of the group has to submit a short technical report for all five experiments. Please BE PREPARED mentally and physically and go through the manual before entering the lab. Whoever unable to attend or run the experiment with his/her group (with reasonable excuse and proof of absence) at scheduled time. 2. Students should have studying the theory of the experiments and also preparing the required tables for noting down the observations. 6. There will be a presentation on the project after the report is submitted. However. 3. Get your laboratory observations and calculation recorded in a logbook. The short report should emphasize more on abstract. Attendance is compulsory. As for the mini project. if the group does not have sufficient time to finish the experiment. The report is due in 2 weeks. Late submission will affect your total marks. Some of the groups will perform the same experiment on the same day. discussion and questions given. he/she should join other group to complete the experiment. Please inform the lecturer/ instructor about the matter as soon as possible. All experiments are carried out in groups. 7. 5. Students are encouraged to be on time or earlier. Block A). The raw data and preliminary analysis counter signed by the instructor.

It might be useful to think in terms of writing one sentence to summarize each of the traditional report divisions: objective. and well labeled. Please show the process flow diagram in the report for better undertanding of the experiment 5. easily read. Graphics need to be clear.” Together these acquaint the reader with the problem you are setting out to solve. Abstract This section summarizes the whole report in one. not as they were supposed to happen. results are dominated with calculations.Guidelines for Report Writing Laboratory report should contain the followings: 1. Discussion is the prominent section in a report. Using clear paragraph structure. Title page Please provide the essential information at the front cover of the report such as: • Group number • Name & Matric number of the student • Group members’ names • Name of experiment • Date of experiment • Name of the instructor/ lecturer • Name of the lab assisstant • Venue 2. It should be a precise and specific summary. explain all steps in the order they actually happened. A sample calculation is sufficient in the report and let the remainder in the appendix. analyse and interpret results that you obtained from the experiment. You may have to define the terms used in stating the subject and provide background such as theory or history of the subject. • Analyze experimental error: Was it avoidable? Was it a result of equipment? If an experiment was within the tolerances. and the plan of development of the report. 3. You can use the explanation below to help you write the discussion part. concise paragraph of about 100-200 words. the objective. Emphasize the objective (which states the problem) and the analysis of the results (including recommendations). • Interpretation: What is the significance of the results? What ambiguities exist? What questions might we raise? Find logical explanations for problems in the data. Nevertheless. method. • Compare expected results with those obtained. Experimental procedure This section describes the process in chronological order. Avoid the temptation to copy a whole paragraph from elsewhere in your report and make it do double duty. the significant results should be in verbal/ write in sentences form. You should be able explain. discussion. • Analysis: What do the results indicate clearly? What have you found? Explain what you know with certainty based on your results and draw conclusions. Introduction The introduction of a technical report identifies the subject. It shows that you really understand the experiment that you completed. the purpose is the “why”. conclusions. tables and figures. Result and discussion Generally. and the plan is the “how. graphs. It also should provide the reader with any background information which the reader will need before you can launch into the body of your paper. you can still account for the difference from the 6     . The subject is the “what”. 4.

Conclusion The conclusion states the knowledge comes out of the report and experiment result. If the flaws result from the experimental design explain how the design might be improved. • Analyze the strengths and limitations of your experimental design 6. etc) • IEEE style Please provide any resources that you refer to complete the report such as laboratory manual or any other outside reading. Appendices Appendices may include raw data. the two most common referencing standards are: • Author-Date style (Chicago style. 8. 7. Evaluation System Assessment Method Marks Laboratory reports 50% Laboratory Log Book 5% Attendance / TeamWork 5% Mini Project and Presentation 40% Overall Total 100% 7     . Reference In engineering. Questions Answer all questions from the manual and insert them in a section of your report before conclusion part. 9. APA 6th. calculations. graphs. ideal. It can be a short and concise conclusion. and other quantitative materials that were part of the research.

Normally. A broth medium is one in which the components are dissolved in water. Generally. (iii) Insert inoculating loop into culture tube and remove loopful of ture. The liquid agar is then poured into sterile petri dish and is allowed to solidify. Handling method is designed to keep the culture pure and to prevent pollution. autoclave is usually used for sterilization. use the lid as a shield by slightly raising it enough so the loop can be inserted but agar surface still protected from contaminants. Most bacteria can grow well at pH of 7. In microbiology laboratory.1 THEORIES AND EXPLANATIONS 1. a temperature of 121oC for a period of time (approximately 20 minutes) is used to heat- sterilize bacteriological media. (iv) flame the lip of tube and replace closure. normal transferring a culture from one vessel to another involves: (i) sterilizing inoculating loop by flaming. bacteria occur in nature as mixed populations. BIOPROCESS PRINCIPLES LABORATORY EXPERIMENT 1 PREPARATION OF CULTURE MEDIA AND ISOLATION OF PURE CULTURE       1. To study individual bacteria. The most useful method is the streak plate method. 8     . various microorganisms need to be isolated into pure cultures consisting of a single type of species.1 Aseptic technique Aseptic is important while working with microorganism to prevent contamination of culture and spread of microorganisms into the environment.1. Do not lay caps or lids on table top to avoid exposing to contamination. (ii) remove the closure and briefly flame the lip of culture tube before inserting sterile loop.0 INTRODUCTION Cultivation is an important technique used to isolate culture and determine microorganisms in microbiology. in which a mixed culture is spread or streaked over the medium surface so that individual cells are separated from one another. Addition of agar results in a solid medium. In both cases. Do not allow tube closures or Petri dishes lids to touch anything. Any medium for cultivation of bacteria must provide basic nutritional requirements. 1. NOTE: Keep all culture covered with caps or lids. Most methods for obtaining pure cultures rely on dilution technique. Single cells will be entrapped and grow into colonies. Another method to produce pure cultures involves diluting a fraction of a mixed culture through a series of cooled liquid agar such that fewer cells exist. Generally. pH of a medium may need to be adjusted to an optimum value to permit microbial growth (referring to the number of cells not the size of the cells). There are two types of medium: defined or synthetic medium and complex medium. When transferring colonies from Petri dish.

invert the plates to prevent water condensate from spreading bacteria over agar surface. (iii) Sterilize the loop after inoculating each section of plate. (ii) Allow the loop to touch the agar surface lightly and slide gently over the surface. 1.   Figure 1.2 Correct method to hold the loop. Transfer culture using aseptic technique without contaminating the culture or exposing yourself to them 4. Isolate single colony for your next experiment by doing streaking on agar plates 9     . Once again.2 below)).2 Streak plating The streak plating technique isolates individual bacterial cells (colony-forming units) on the surface of an agar plate using a wire loop.2 OBJECTIVE In this experiment. Prepare a broth medium and agar medium 2. 1.1. (iv) Use petri dish cover to prevent contamination into the media and (v) when incubating. Figure 1. you will learn to: 1.1 Three times streaking method. The following rules are important for consistent results: (i) Allow the loop to cool before using it for inoculation (Note: Hot loop may kill the microorganism). Use autoclave to sterilize the prepared medium and required labwares 3. (Note: Do not dig the loop into agar! Hold the loop parallel to the agar surface to minimize gouging (see figure 1. the idea is to obtain isolated colonies after incubation of the plate. The streaking patterns shown in the figure below result in continuous dilution of the inoculum to give well separated surface colonies.

1. 8. Insert the sterile loop and remove a loopful of culture. Place the streaked plate into a 37 ◦C incubator and incubate for 48 hours. 7. Try not to touch the sides of tube. Nutrient broth and agar will be prepared in advance by lab demonstrators.4. 3. Flame the tube lip again and replace the tube cap.4 PROCEDURE 1. Use your free hand to pick up the tube containing the culture.1 Preparation of medium and sterilization 1. 2. 6. Place the loop containing the inoculum into the tube. Examine the plates and describe its appearance. 9. Remove the loop and cross streak the agar surface three to four times and continue streaking into a second adjacent area. Remove the tube cap and flame the lip in Bunsen burner flame.5 ml Cotton Aluminium foil Sterile petri dish Bunsen burner 1. Cover the agar plate with its lid. Gently shake it to disperse the culture. 1. Allow the wire to cooled for a few seconds (Do not wave the loop in air).2 Sampling analysis: 1.4. 10     .2 MATERIAL AND APPARATUS Nutrient Apparatus Equipment Peptone Microscope slides PH meter Ethanol 95% Conical flasks (250 ml) Balance MRS Broth Graduated cylinder (1L) Autoclave MRS Agar Beaker (500 ml) Incubator Gram stain Crystal Loop Oven Violet Beaker (250 ml) Spectrophotometer Gram stain iodine Pipette (100 microlitre) Gram stain Safranin Pipette (1000 microlitre) Pipette tips (100 microlitre) Pipette tips (1000 microlitre) Microcentrifuge tubes 1. 5. 4. Insert the wire of inoculating loop into Bunsen flame until it is red and glowing. Flame the inoculating loop.

5 EXPERIMENTAL RESULTS Observe plates. Did you obtain isolated colonies on the agar plates which were streaked? If you did not obtain isolated colonies. 10. 1. size and color of representative colonies from the streaking results. What is subculturing? 4. Describe the morphology. 5.6 QUESTIONS 1. When and why do you need to apply isolation of pure culture? Support your reason(s) with three examples. Keep the plates in the fridge for next experiment. What is the difference between streak plate and spread plate method?       11     . 1. what changes should you make in your technique to ensure isolated colonies? 3. What can you notice in the control plate? 2.

called cultural characteristics. The outer leaflet of the outer membrane is composed largely of a molecule called lipopolysaccharide (LPS). The space between the plasma membrane and the outer membrane is called the periplasmic space. Gram-positive cell walls have a thick peptidoglycan layer beyond the plasma membrane. These differences. In 1883 Hans Christian Gram invented an important differential staining method called the Gram Stain. This staining procedure differentiates microbes into two basic groups: Gram positive microbes and Gram negative microbes.0 INTRODUCTION When grown on a variety of media. They have a thin peptidoglycan layer and an outer membrane beyond the plasma membrane.pdf) 2. BIOPROCESS PRINCIPLES LABORATORY EXPERIMENT 2 CHARACTERIZATION OF BACTERIA AND ESTABLISHING PURE CULTURES       2. These acids are also very important in the body’s ability to recognize foreign bacteria. Spanning the outer membrane are porin proteins that enable the passage of small molecules. the bacteria are first fixed to the slide by the heat fixed smear. This renders the slide safe and keeps the bacteria stuck to the slide so that simple or complex staining and washing procedures can be carried out without washing them off of the slide. In the Gram stain. In most microbiological staining procedures. Characteristic polymers called teichoic and lipoteichoic acids stick out above the peptidoglycan and it is because of their negative charge that the cell wall is overall negative.edu/~makemson/MCB3020Lab/Ex2GramStain. Differential stains render one type of microbe one color and other types of microbes another color. Lipoproteins join the 12     .fiu. are used as the basis for separating microorganisms into taxonomic groups. In this procedure living. microorganisms will exhibit differences in the macroscopic appearance of their growth. Gram-negative cell walls are more complex. (source: http://www2. LPS is an endotoxin that is important in triggering the body’s immune response and contributing to the overall negative charge of the cell. potentially pathogenic bacteria are smeared on the glass slide and allowed to dry before the slide is heated so that the bacteria are killed and stuck (coagulation of surface proteins) to the slide. Gram-positive cell walls stain blue/purple with the Gram stain.1 THEORIES AND EXPLANATIONS Most bacteria can be divided into two groups based on the composition of their cell wall: 1. 2. Gram positive organisms retain the crystal violet-iodine and appear blue/purple whereas Gram negative cells loose the primary dye complex during the challenge rinse (acetone or alcohol) and are stained by the safranin which makes them pink.

touch the slide 2 seconds after heating. Pick up a single colony using the aseptic technique to the slide and mix with water. Do not overheat the slide.4 METHODOLOGY OF OPEN REFLUX METHOD 2.1 Gram stain CELL COLOUR REAGENT Gram Positive Gram Negative Crystal violet PURPLE PURPLE Iodine PURPLE PURPLE Alcohol PURPLE COLOURLESS Safranin PURPLE RED 2. Prepare one smear for each microorganism. outer membrane and the thin peptidoglycan layer.1 Identification of bacteria 1. Smears require only a small amount of the bacterial culture. For agar culture. 2. 2. Spread the suspension over an area of circle. Do not blow on slide or wave it in the air. label one end of slide with microorganism to be stained.3. Become familiar with the chemical basis of the Gram stain and the performance of the procedure for differentiating between the two principal groups of bacteria (gram-positive and gram-negative). ii. it should be warm but not hot enough to burn.2 OBJECTIVE In this experiment. iii. Prepare the bacterial smears for the microscopic visualization of bacteria 2. Smear preparation i. place a small drop of water at the top center of slide. Allow the smear to heat dry by passing the slide through a bunsen burner flame intermittently. Observe the growth of colonies on the agar plates. Gram-negative cells will stain pink with the Gram stain. Table 2.3 MATERIAL Refer to Bioprocess principles laboratory experiment 1. Note: Remember to hold the clean slides by their edges.4. 2. 13     . 3. Characterize bacteria using gram staining and microscope 3. Place the slides on the staining rack and flood each smear with crystal violet. On the underside of slide. you will learn to: 1.

6. After 1 minute. 9.6 QUESTIONS 1. What color does your specimen appear under microscope? Is it gram positive or negative? 6. wash the crystal violet from each slide with distilled water and drain off excess water.4. Swirl the medium to make sure the colony is well dispersed.5 EXPERIMENTAL RESULTS Show and describe your Gram stains. What features of your Gram stain exemplify the Gram stain theory? If there are features of the Gram stain that are not as expected. What is a differential staining? What are the advantages of differential staining procedures over the simple staining technique? 5. 5.2 Establishing pure culture 1. counterstain. 11. mordant. wash the iodine from each slide with distilled water. 7. 1. Tilt each slide and decolorize with ethanol until alcohol draining from the slide appears colourless. 2. Why is it important of obtaining pure cultures? 4. Wash the slide briefly and drain off the excess. 8. 10. 9. Which is the most crucial step in the performance of the Gram staining procedures? Justify your answer. 12. Examine the slides. pick up a loopful of single colony from the agar plate and inoculate into the prepared broth medium. Store the culture in fridge for next experiment. Why must fresh bacterial cultures be used in a Gram stain?       14     . Flood each smear with iodine. Describe the growth of each culture on the streak plates. what possible sources or error may be responsible? 7. 2.) 8. 4. 2. Cite the purpose of each of the reagents in a differential staining procedure. (Define the followings: primary stain. about 15 seconds. Describe the color of the smear. decolorizing agent. 4. After staining for 1 minute. Incubate the broth medium in an incubator shaker at 37 ◦C and 150 RPM for 24 hours. Using aseptic technique. View the slides under microscope to observe the cell morphology. What is a pure culture? How do you prove a culture is pure? 3. 2. 3. Counterstain the smear with safranin for 20 to 30 seconds. Wash the slide briefly with distilled water and blot dry.

turbidimetric measurements.1 Serial dilution from stock solution Quantification of the cell numbers is important in researches.01 M. there are numerous occasions when it is necessary to either estimate or determine the number of bacterial cells in a broth culture or liquid medium (a. 15     . Usually the dilution factor at each step is constant. A ten-fold serial dilution could be 1 M. including injured or starved cells.1 Preparation of dilutions utilizing sterile nutrient broth blanks.1.k. cell mass determination. Figure 3. For accurate enumeration of bacterial numbers. resulting in a geometric progression of the concentration in a logarithmic fashion. The methods include standard plate counts. BIOPROCESS PRINCIPLES LABORATORY EXPERIMENT 3 QUANTIFICATION OF CELL NUMBER       3. The culture- independent techniques are important as it has been established that the bacterial diversity in any given environment is severely underestimated when assessed by means of culture-based technique. a series of dilutions are performed in order to gradually reduce the concentration of the solution from that of the stock solution.0 INTRODUCTION In the study of microbiology. Determination of cell numbers can be accomplished by a number of direct or indirect methods. it is important to use culture-independent techniques. direct microscopic counts. Since measuring small volumes of solution is prone to error.1 THEORIES AND EXPLANATIONS 3. This can be done by series of dilution. and 0. and measurement of cellular activity.a bacterial enumeration). 0. 3.001 M and so on. 0. visual comparison of turbidity with a known standard.1 M.

determine the dry cell weight 4. it is critical that each colony comes from only one cell. from the knowledge of the dilution used. is the time necessary for dilutions. then incubating the plates under proper conditions so that colonies are formed. A viable cell count is usually done by diluting the original sample. plating aliquots of the dilutions onto an appropriate culture medium. 16     . This method of enumeration is relatively easy to perform and is much more sensitive than turbidimetric measurement.1. Actually an axenic culture will be made from a clone (colony). we call these pure cultures even though we have no technical proof of that.3. The viable titer is determined by and counting colonies (expressed as Colony Forming Units or CFUs) per volume plated and multiplying by the dilution factor. However. the total number of viable cells is usually reported as colony-forming units (CFUs) rather than cell numbers. After incubation. For accurate determination of the total number of viable cells.2 OBJECTIVE In this experiment. A pure culture is defined as the progeny from one cell. quantify cell viability using plate count method 2.3 MATERIAL Refer to Bioprocess principles laboratory experiment 1. as well as the time needed for media preparation. since one is never sure that all such groups have been broken apart. platings and incubations. isolated colonies will be examined for the types of cells and one will be restreaked to obtain a pure culture. This method only counts living cells because dead cells do not reproduce to form colonies. the original number of viable cells can be calculated. Proof of pure culture involves showing that all the colonies on the restreak are identical and Gram staining these to demonstrate all the cells in the resulting colonies are identical and the same as those on the original plate. A major disadvantage. you will learn to: 1. Assuming that one cell could have given rise to the colony.2 Standard plate count A viable cell is defined as a cell which is able to divide and form a population (or colony). 3. however. so chains and clumps of cells must be broken apart. the colonies are counted and.1) Later. Use Hemacytometer to determine the total cell 3. determine the optical density of broth medium containing cell suspension 3. Viable titer = (CFU/volume plated) x Dilution factor (3. 3.

1 ml of sample from no. Cover the opening with para-film and gently shake to mix.1 Determination of viable cells: Plate count method 1. 3. Pass 10 ml of broth medium through the filter. Switch on the spectrophotometer and adjust the wavelength to 600 nm. Fill an empty cuvette with 3ml of distilled water. Load the cuvette containing sample and wait until a stable reading has been achieved.1 ml of sample from tube no. 3. Carefully remove the filter paper which contains the cell paste and dry in an oven at 95 ◦C for 24 hours. 2. 6. Label the tubes from 1 to 8.8.4. Shake well and remove 0. Total cell count can be determined by using a Hemacytometer.9 ml of peptone water in each of the tubes. 1 and pipette onto the surface of agar. Remove 0. 4. Determine the dry cell weight of cells. Cautiously remove 8 sterile microcentrifuge tubes and fill them with 0.4 Determination of total cell 1. 8.1. Incubate the agar plates at 37 ◦C for 48 hours before counting. 4. 4. Use it as a reference. Fill an empty cuvette with 2. 5. 3. 2. 2. Sterilize a spreader with ethanol and flame and cool it at the side of agar before spreading the pool of liquid sample. Invert the plate and label. 7.4. Remove 0.4.2 Determination of optical density 1. Weight a dry filter paper.3. Load the filter paper into the filtration unit. Allow it to warm-up for 15 minutes.3 Determination of dry cell weight 1. Repeat this process up to tube no. 3.3 ml of sample from broth medium and pipette into the cuvette to make up 3 ml. Record the reading. 6. 1 and pipette into tube no.4 PROCEDURE 3. 2 to tube no. Repeat the spreading process for tube no. Withdraw 0.7 ml of distilled water.1 ml of sample from the broth medium and pipette into tube no. 3. 3. 17     . Load the reference cuvette into the sample chamber and set to zero. 2. 5.4. 5.

3.5 EXERIMENTAL RESULTS

Calculate the viable titer for each plating medium.

Dilution number Number of colony Cell number

3.6 QUESTIONS

1. Are all the bacteria counted by this procedure? Is this an overestimate or
underestimate of the actual number of viable bacteria in soil? What are
possible reasons that the CFU underestimates the number of bacteria?
2. Why can a standard curve be used only to estimate cell concentration of a
fresh culture of the same species grown in the same media? For instance
why can’t it be used for other species, or same species grown in other media?
Why can’t it be used on older cultures?
3. If the stock culture you were given was old, would you expect the
heterotrophic plate count to be higher or lower? Why?
4. Which method would you use (heterotrophic plate count or
spectrophotometer) if you had enumerate 200 different samples? Why?

 
 
 
   

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Appendix 01: Colonial Morphology
 
Both colonial and cellular morphology are characteristic of each species of bacteria and are
sometimes useful in the identification of an unknown microorganism. When a bacterium grows on a
solid agar surface, the number of cells increase until a visible mass of cells, called a colony, appears.
It is usually inferred that each colony arises from the division of a single cell. The most useful
culture characteristics are morphology, size and pigmentation of the colony. The figures presented
below illustrate some of the morphological characteristics of bacterial colonies and provide helpful
terminology for the description of colony morphology.
 
 

 
Figure A.1 Morphological characteristics of bacterial colonies.

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CHEMICAL REACTION ENGINEERING LABORATORY EXPERIMENT 1

KINETIC STUDIES IN BATCH REACTOR
(Saponification of Ethyl Acetate)

1.0 INTRODUCTION

The design of a chemical reactor calls for prior information regarding (a)
the order of reaction and (b) the value of the reaction rate constant which gives
the reaction rate equation. This information is to be obtained invariantly through
laboratory- scale experiments conducted at constant temperature. The
equipment used is generally of batch type in case of homogeneous reaction, and
of flow type in case of the homogenous or heterogeneous reactions. The present
experiment is very typical of the kinetic method that is normally used for simple
homogeneous reaction.
This experiment can be divided into two parts: (i) to find the reaction
order and the rate constant at constant temperature, (ii) to determine the
activation energy for saponification of ethyl acetate. Reaction rates depend on
the composition and the temperature of the reaction mixture. Every chemical
reaction occurs at finite rate and, therefore, can potentially serve as the basis for
a chemical kinetic method of analysis. On the other hand, activation energy is
the energy barrier that has to be overcome for a reaction to happen.

1.1 THEORIES AND EXPLANATIONS

The saponification id ethyl acetate in dilute aqueous solution can be
written as:

CH3COOC2H5 (l) + NaOH (l) = CH3COONa (l) + C2H5OH (l)
(1.1)

Because that the reaction saponification of Ethyl Acetate is a single
reaction, let A be NaOH and B be CH3COOC2H5, the rate equation can be defined
as

–rA = k CA.CB
= k f (CA)
= k CAn
(1.2)

when one mole of A reacts with one mole of B (refer to eq. 1.1)

20  
 

3) The graph of log [dCA/dt] vs log [CA] is a straight line.3 MATERIAL 1. and the order of the reaction. –rA = k CAn log [-dCA/dt] = n log [CA ] + log k (1. k. A = frequency factor E = activation energy R = Ideal gas constant T = temperature Rearranging the Arrhenius equation. NaOH(aqueous. The Arrhenius equation: K=AeE/RT (1. n can be directly obtained by finding the intercepts and the slope from the graph of log [dCA/dt] versus log [CA]. evaluating all terms in the equation including the derivative dCi/dt. pure 10ml 2.2 OBJECTIVE 1. To verify that the saponification of ethyl acetate in dilute aqueous solution is a second order reaction. a dozen conical flaks(250ml) 21     . we can use the differential method.4) where k = rate constant. and testing the goodness of fit of the equation with the experiment. plot the graph of log [dCA/dt] vs log [CA ]. 2. To report the value of the reaction rate constant. Phenolphthalein indicator 5. HCL (aqueous. Batch reactor (1 litre beaker) 6.05M) 1 litre 3. The rate constant. 0. we can find the slope or tangent at point for the suitably selected concentration values by using mirror method.5) 1. The slope of these points dCA/dt is the rates of reaction at certain compositions. In determining the rate constant of the reaction. Then. To find the activation energy of the reaction of saponification of ethyl acetate in dilute aqueous solution 1. ! ! ln ? = − ! ! − ln ? (1. Ethyl Acetate. 3. The differential method of analysis deals with the differential rate equation to be tested. t.1M) 500ml 4. By plotting the graph concentration CA versus time.0.

Explanation: Note that when a sample of reaction mixture is transferred into the conical flask containing HCl. the experiment helps to find the alkali concentration (CA) in the reactor as a function of time (t). Back-titrate the contents of twelve conical flasks with aqueous NaOH from the burette using phenolphthalein as indicator (appearance of first shade of pink color is the end point of titration). 2.10. Place 1 litre of NaOH solution in a clean 1 litre beaker. 22     .3.4.1 Ascertain the order of reaction: 1. pipette 10ml of the reaction solution mixture into each one of the labeled conical flasks.7. 3.4.1 M solution in the reactor itself and saponification reaction is now on. The ethyl acetate forms a 0. Transfer 10ml of 0. Place the reactor on a magnetic stirrer and start stirring vigorously. stop-watch 1. 7.2 Determining the activation energy of saponification: Repeat steps 1-6 in section 1. 6.11. 7. 5. Keep a clean and dry 10ml pipette handy.8. By means of a clean and dry measuring pipette. At the reaction times 1.2.9. The experiment should be carried out at room temperature.12 minutes.1M HCl solution into each of twelve conical flasks.4. which serves as the reactor. pipettes 9. which are serially labeled. the alkali in the reaction mixture gets neutralized and so the saponification reaction stops. In other words. 1.4 METHODOLOGY 1.6. transfer exactly 10ml of ethyl acetate into the reactor and start the stop watch simultaneously.1.4.5. In this experiment conduct the experiment at 40 ̊ C and 50 ̊ C instead of the room temperature. Note: The stopwatch must not stop until all the twelve samples are transfer. 4. measuring pipette(5ml) and burettes 10ml and 25ml 8. Back-titration of the contents of this flask therefore helps in determining the amount of unreacted NaOH present in the reaction mixture at the time of its removal from the reactor.

∆V. Draw the conversion vs time graph. (min) Vinitial Vfinal mL 1. (ii) 40 ̊ C.. Evaluate the rate constants when temperature changes.1. 23     . 5. Find the order of reaction and rate constant using a. 3. and (iii) 50 ̊ C. Readings of Burette Volume of Time.t (mL) NaOH used. Perform the mass balance. Saponification reaction conducted at T = ____ ̊ C. Justify the differences found in comparison. For each case.6 QUESTIONS 1. Using Arrhenius equation. calculate the conversion. E and frequency or pre-exponential factor. Integral method Compare the result of the two methods. k0. calculate activation energy.5 EXPERIMENTAL RESULTS Record the following at (i) room temperature. 4. Differential method b. 2.

the tank is fitted with the auxiliary equipment necessary to maintain the desired reaction temperature and pressure conditions. an equal volume of the reactor contents is displaced through an overflow pipe situated near the top of the vessel. a steady continuous feed of reactants is pumped into the vessel and since there is usually negligible density change on reaction.0 INTRODUCTION Continuous stirred tank reactors (CSTR) may consist of one or more cylindrical tanks. Normally the tanks are arranged with their axes vertical. 2. In normal operation. CHEMICAL REACTION ENGINEERING LABORATORY EXPERIMENT 2 ISOTHERMAL CONTINUOUS STIRRED TANK REACTOR 2. The well-stirred tank reactor is used almost exclusively for liquid phase reactions.1 Single continuous stirred tank reactor. although instances of gaseous reactions have been reported. ethyl acetate and sodium hydroxide are introduced at the respective volumetric feed rate of vA and vE. In addition. The stirring of the contents of each tank is affected by an agitator which is mounted on a shaft inserted through the vessel lid.1 THEORIES AND EXPLANATIONS The stoichiometric equation of the saponification of sodium hydroxide (A) and the ethyl acetate (E): CH3COOC2H5 + NaOH CH3COONa + C2H5OH (2. although this is not essential. 24     .1) The reactants. Figure 2.

8) The CE and CA at the exit stream is taken as those exiting in the vessel using the result from the calculation of the equation 2. and 2. is called space time τ Residence time.6) v + vA Total volumetric flow rate = E time (2.11) 25     .3) And vin = vout (2.4.5) v Volumetric flow rate of Ethyl Acetate = E time (2.2) The ratio of the reactor volume.3. V.10a) d [C E ] d [C A ] = =0 dt dt (2. over the total inlet volume flow rate. v. The flow rate for input.7) Volume of the liquid in the reaction vessel is constant at V. 2. vin = vA + vE (2. At the beginning of the experiment. τ = V / v (2.4) v Volumetric flow rate of sodium hydroxide = A time (2.8 we get.9) dCA (C A )in − (CE ) out = − KCE C A dt τ (2. the equation is given by: d [n e ] d [C E ] =V = vin (CE) – vout (CE) – VkCECA dt dt (2. d CE (CE )in − (CE ) out = − KC E C A dt τ (2. moles of Ester and Alkali changes with respect to time.

12a). τ is the space-time of experiment. CAα and CEα.14b) The conversion of the ethyl acetate and sodium hydroxide can be evaluated from equation (2.13) For the special case (CA)in = (CE)in k τ (CEα)2 + (CEα) – (CE)in = 0 (2. CE α = (CE)in . ! !! (!!! !!! )/!!! (!!! !!! ) ! !! = !!! = !!!! therefore ? = !!!! (2.k τ (CE)α (2.16) !"#$%&  !"  !"#$%&! !! ?= = !!!  !"!#$  !"#$%&'()*  !"#$  !"#$ !! !!! (2. k τ (CE α)2 + (CEα) {1 – k τ [CE. Vmixture = Vtotal – VNaOH(exact) – VHCl (2.14c) to find the rate constant.15) Before using equation (2.in – CA.14a) or the equation (2. we need to find the CA.14b) to determine the conversion if rate constant . CAo.12) CA α = (CA)in . CAO is the concentration of the Sodium Hydroxide which before reacted with the Ethyl Acetate.14a) OR k τ (CAα)2 + (CAα) – (CA)in = 0 (2.12a) Eliminating (CAα) from (2.in]} – (CE)in = 0 (2.k τ (CE α)(CAα) (2. After a certain passage of time CA and CE reaches constant value.14b) to k τ (CA) 2 + (CA) – (CAo) = 0 (2. for CSTR. Also. k. and the τ .14c) where CA is the concentration of the Sodium Hydroxide which had reacted with the ethyl acetate in the continuous stirred tank reactor.3a) 26     . We can write the equation (2.12) and (2. value is known or to determine the k value if experimental conversion is known. k.

1M. Sodium Hydroxide.17) and (2. Start the stirrer. 2. NaOH (aqueous.4 METHODOLOGY OF OPEN REFLUX METHOD 1. reactor) 2. 4. 2. titration) 4. 2. 0. !"#$%&'(  !"  !"#$  !"  !""# (!"#$%&'()*  !"#$  !"#$  !"  !"#$) ! !! ! ! ?!! = !"#$%  !"#$%&'()*  !"#$  !"#$ = !! !!! (2. NaOH (aqueous. (2. Isothermal Continuous Stirred Tank Reactor 8. Magnetic stirrer 14. Ethyl acetate (0.3).5L/hr. Measuring calibrated cylinder (1000mL) 2. introduce the streams into the vessel. We find the average of the CAs which we find before.1 M strength of Ethyl Acetate. then substitute that value of the average of CA into the equation (2. 0. Hydrochloride acid. Water vessel 12. Distilled water (H2O) 6. Sodium hydroxide.14c). Digital stop watch 13. titration) 5. Then we can find the rate constant.3 MATERIAL AND APPARATUS 1. k. Adjust the flow rates of the Ethyl Acetate and the Sodium Hydroxide to the required level. Once the flow rates are adjusted to the known levels.2 OBJECTIVE To determine the rate constant for the given reaction at ambient temperature. HCl (aqueous. 0.05M. 3. and 0. Burettes 50 cm³ 11. 7 conical flasks ( 250 ml) 9. Phenolphthalein indicator 7.18) Substitute the equation (2.1 M of Sodium Hydroxide. Fill the reservoir with the 0. 27     .05 M.14c).1 M. reactor) 3. Measuring pipette ( 5ml ) 10.17) !!" !!!"#$ !"#$% (!!!! )!"#$ ?! = ????????  ??  ???? = !!"#$%&' !!"#$%&' (2. by solving this equation. NaOH. 2.18) into the equation (2.

2. final V(exact) (ml) CA (mol/L) (min) (ml) (ml) 2. Back–titrate the contents of the seven conical flasks with aqueous NaOH from the burette by using phenolphthalein as indicator. What is the rate constant for CSTR? 28     . 16 and 30th minutes by pipette each of them out into the prepared and labeled conical flasks. 8. 12. t = 0. vA= _____ L/hr Volumetric flow rate of Ethyl Acetate. t VNaOH. Note: The end point of the titration is indicated by the appearance of the first shade of pink colour. 6. stop the experiment. Volumetric flow rate of Sodium Hydroxide. 5. vE = _____ L/hr Total volumetric flow rate. Collect the sample for the time. 1. Vr = _____ mL Time. Note: Do not stop the stop-clock until all the twelve samples are transferred. 6. 4.5 EXPERIMENTAL RESULTS Find the values of (CA)α and tabulate the observations. 7. initial VNaOH. 2. 10.5 QUESTIONS 1. The contents which in the vessel are stirred and the reaction is allowed to complete until the Ethyl Acetate has reacted. Once a constant value of concentration is reached. (vA + vE) = _____ L/hr Total reactor volume. 8.

(show the graph) 5. 4. Draw the conversion vs time graph. 3. why and when will you choose to use CSTR for your production? 6. Calculate the substances conversion. Perform mass balance for the saponification of ethyl acetate and sodium hydroxide in isothermal CSTR system. 29     . Formulate a model for the system of CSTR’s which should describe the change in concentration due to changes in inlet flow rate. In terms of conversion. 2. Compare the conversion in a batch reactor with the conversion in the CSTR’s for the same reaction time.

the quotient of the real ( γ ) and the maximum adsorption molality is defined as degree of coverage Θ . A + B ↔ ABads (1.ads . mA (1. The quantity of absorbed substances is a function of the type of system investigated and the partial pressure and the concentration of the substance in lab at a constant temperature. substantial adsorption enthalpies.1. monolayer of the adsorbed substance).2) In cases of monolayer formation.ads referred to the surfaces area of or the mass mA of the adsorbing agent.1 THEORIES AND EXPLANATIONS 1. 30     .3) The correlation between the adsorption molality and the free equilibrium concentration of B at constant temperature is described by great numbers of adsorption isotherms of limited validity. a number of superimposed adsorption layers) and chemisorptions (chemical bonds. 1. where γ =adsorption molality. The extent of adsorption is expressed by the quality of adsorbent nB. very low adsorption enthalpies. γ Θ= γ max (1. SEPARATION PROCESS LABORATORY EXPERIMENT 1 DETERMINATION OF ADSORPTION ISOTHERM FOR CITRIC ACID 1. It is the equilibrium relationship between concentration in liquid phase and concentration in substance particles adsorption in certain temperature.0 INTRODUCTION In this experiment adsorption isotherms operation is introduced.1 Equilibrium relation for adsorbents: adsorption isotherms Attractive forces between the exposed particles cause gases or dissolved substances B attach themselves (absorbate) reversibly to the surfaces of solid phases A (adsorbing agents) (adsorption). The term adsorption is used to describe the attachment of gases or dissolved substances to the surface of a solid.1) Depending on the strength of the interactions one can differentiate physiosorption (weak Van der Waals forces. n γ = B .

k des = rate constant of the adsorption and desorption. β = system-dependent constants 31     .eq = K ' C B .5c) γ γ MAX K C B.eq (1. In contrast. dC B For the case of an established adsorption.3).4) where C B = concentration of B in the solution k ads.5) Where C B = equilibrium concentration of B in solution. 1 1 1 1 = × + (1. dt dC B − = k ads c B (1 − Θ) − k des Θ dt (1.eq (Henry’s isotherm).eq γ max 1 Consequently. the adsorption molality tends toward a concentration in depending limiting value γ max at very high equilibrium concentrations ( KC B . k des This simplified for very low equilibrium concentrations ( KC B . dt Langmuir’s adsorption isotherm follows: γ max KC B . eq >1) γ = γ max (1.5a) Thus.eq γ = 1 + KC B .eq γ max k Freundlich’s empirically determined adsorption isotherm for many systems γ = αC Bβ. the graph plots of as a function of the reciprocal γ 1 1 equilibrium concentration gives a straight line with slope and the C B.eq (1. − dC B From kinetic consideration of the adsorption rate . k K= ads = constant. ( − = 0 ) with definition (1.5b) In the region of validity of the isotherm (4) the correlation between adsorption molality and equilibrium concentration can be linearized by simple rearranging.6) where α . respectively. the adsorption molality γ should be linearly correlated with C B .eq < 1 ) to:- γ = γ max KC B .eq (1.

To determine whether isotherm adsorption occur for liquid-gases adsorption systems.O ) and equilibrium concentrations ( C B . 1. . whose logarithmic expression is as followed: lg γ = β lg C B . system volume = 0.7a) 3V0VK c NaOHVNaOH .25L VS = 100mL. To investigate which isotherm rule (Henry.2 OBJECTIVE 1.eq ) × Vs γ = B .5c) and (1.eq + lg α (1. (1.O = NaOH NaOH .eq present case. all results are straight line. the adsorption molality γ can be determined from following correlation.2).eq ) ).5a).6a) This form allows a simple graphic evaluation and thus the determination of the constants α and β .7b) 3V1 From this. lg(C B.0 st (1. as functions of 1 the corresponding equilibrium concentrations ( C B. c V V cB. CNaOH.1 of citric acid solution when the tribacity of the absorbed material (citric acids) is considered by applying the following relationships.6a). plot the expressions of the adsorption molality ( γ . can be calculated from the volume of the volumetric flack Vk=250ml and the volumes of NaOH of known concentration. Freundlich or Langmuir isotherm adsorption) that this adsorption system is valid.8) mA mA Where Vk = 250mL=0. which are required for the evaluation. n (C B .1 c B . γ which correspond to the relationships (1. lg γ ).3 MATERIAL 32     .1L MA=3 mass of adsorbing agent = 0.003kg 1. . The initial ( C B .eq . In the C B.eq ). 1 Therefore. 3. which is derived from equation (1. To estimate the equilibrium concentration balance of citric acid after stirring the solution with different starting concentration and activated carbon.ads = (1.0 − C B .eq = (1. 2.

500 g 23 Distilled water. 100 ml 22 Activated carbon.5 M NaOH and fill it into another 500 ml volumetric flask. 5 litres 1.54 g dissolved in distilled water. 100 ml 1 12 Graduated pipette. 250 ml 6 8 Volumetric pipette.5 M citric acid with 52. 250g 20 NaOH. Chemicals and apparatus Units 1 Retort stand 1 2 Burette clamp 1 3 Magnetic stirrer with stirrer bar 3 4 Laboratory balance 1 5 Burette. seal the flask mount and set onto the magnetic stirrer. 25 ml 1 10 Volumetric pipette. Fill them into the 500 mL volumetric flasks and top up with distilled water until calibration mark. 100 ml 1 16 Funnel 1 17 Circular filter paper 1 18 Stopper 6 19 Citric acid. 50 ml 1 6 Volumetric flask. Top up with distilled water until calibration mark. 2. Repeat for other five Erlenmeyer flask. 500 ml 4 7 Volumetric flask. Prepare 0. Prepare 2 sets of 0. granulated. 3.5 M citric acid (Vst) listed in table 1 into a separate clean 250 ml volumetric flask and top off to calibration mark. 1M 21 Phenolphthalein indicator.00g activated carbon into a clean Erlenmeyer flask. After that. 10 ml 1 9 Volumetric pipette.4 PROCEDURE 1. No. 50 ml 1 13 Erlenmeyer flask. 250 ml 6 14 Pipettor 1 15 Beaker. 50 ml 1 11 Volumetric pipette. 4. 5. Add 3. 33     . Pipette each volume of the 0. Pour 100 ml each of the six concentration series solution into separate 250 ml Erlenmeyer flasks containing the activated carbon.

5 50. Then find the respective logarithms and reciprocals for CB. Find CB. 8.0 62.0 10.0.0 187. repeat the titration process with 10 ml of the 0.5 10. 6.0 12. Table 1.5 M NaOH and in similar manner.0 50.0 25. Vo = __________ ml VNaOH.0 10.0 25.5 25. 9.0 62. Vst (ml) V1 (ml) 250.eq and γ.1: Volumes of stock solution for the preparation of the concentration series (Vst) and the sample volumes after filtration (V1) for the determination of the equilibrium concentration of citric acid.5 25. Add the filtrate solution with 3 drops of phenolphthalein.0 25.0 50.eq and γ .5 10.0 125.5 EXPERIMENTAL RESULTS Record the following. Tabulate the data.6 QUESTIONS 1.0 187. 7. CB.0 12.5 M solution of citric acid (Vo). 34     . Titrate the respective sample volumes (V1) given in the table 1 with 0.0 1.5 50.0 1.0 125. Include any relevant observation. Repeat the titration process. Stir the content of the flasks vigorously for 30 minutes and filter the suspensions stirring.o= ________ ml Burette Readings (ml) Volume of Vst (ml) V1 (ml) Initial Final NaOH 250.0 25.

Discuss and conclude your findings. Determine the slope of the regression lines of (i). (ii) Freundlich. What is the major difference in Henry. 35     . 2. Determine the adsorption constant (k) and the maximal adsorbed substance amount of citric acid per gram of activated carbon. Freundlich and Langmuir isotherm adsorption? Under what circumstances that they are applicable/not applicable? 6. 5. (ii) and (iii). and (iii) Langmuir isotherm adsorption theory. 4. Plot the correlation between the of the equilibrium concentration CB.eq and the adsorption molatity γ using (i) Henry. 3.

etc).e. Leaching is widely used in chemical industries where mechanical and thermal methods of separations are not possible or practical. the contact time should be independent of the flow rate 36     . is carried out in this experiment. At very high flow rate. no flooding of the extraction chamber.0 INTRODUCTION Solid-liquid extraction (leaching) is the process of removing a solute or solutes from a solid by using of liquid solvent. The efficiency of extraction varies with the contact between solid and solvent. transfer the solute to the liquid phase). SEPARATION PROCESS LABORATORY EXPERIMENT 2 SOLID-LIQUID EXTRACTION 2. samples weight from valve 2 and 3 will be taken. followed by putting the bag into the extraction chamber. physical state of solids. It can be used in both simple batch system or in a semi-continuous system such as the Bollman extractor. The rate of extraction depends on many factors such as type of solvents. but the overall operation of the plant would be uneconomic as the throughput would be very low. In the case of a free-draining solid. and the nature contact between solvent and solid (contact time. production of a concentrated solution of a valuable solid material are typical industrial examples of leaching. The extraction of the corn/soybean/nut oil from the maize/soybean/nuts using the extracting solvent. (ii) the diffused solvent dissolves the solutes (i. Leaching process consists of three parts: (i) diffusion of the solvent through the pores of the solid. 2.1 THEORIES AND EXPLANATIONS Solid-liquid extraction by percolation of solvent downward through a fixed bed of solid is a common method of operation. i. In this experiment. Extraction of sugar from sugar beets. Along the experiment. The experiment started once the extractor is stabilized. oil from oil bearing seeds. At first 2 kg of maize (corn)/soybean/nuts is poured into extraction bag.e. sufficient contact would occur to allow penetration of solvent into the cells and diffusion of solute out again. An optimum can occur between these two extremes. Murphee efficiency will be high as the system will have the opportunity to approach equilibrium. hexane. At very long contact times. contact will be limited and extraction efficiency will be impaired. The solvent hexane is poured into the solvent charge. (iii) transfer of the solution from porous solid to the main bulk of the solution. solvent and solid are fixed and it is left to determine how the extraction proceeds with time. For cellular solids case.

1) x= (ρ / ρ o ) − 1 Where ρ=density of mixture ρs=density of hexane ρ0=density of soya bean As for amount of solute content in effluent. Weighting machine 6. 2.e. Then we calculate the area under the curve. we can get it by plotting the graph of density of effluent vs time. It is expected the profile of extraction to be exponential with time but the practical systems has to be done to confirm the model. but is expected to reduce throughput (i. the amount extracted per unit time).2 OBJECTIVE 1. To compare methods for estimating the amount of material extracted (to compare the amount of oil that is extracted from the corns). Hexane 4. since it will always be just the time taken for solvent to percolate through the column. Erlenmeyer flasks 5.3 EQUIPMENT AND MATERIAL 1. the composition of the effluent can be calculated by using equation (2. 2. The value of the area will be multiply by the solvent flow rate to get the amount of solvent. 1 − (ρ / p s ) (2.e. For this experiment. the rate of solvent input). Maize (Corn) / Soy bean / nuts 3. QVF Teaching system: CTS 6 Solid Liquid Extractor 2. To demonstrate the characteristics of an extraction by downward percolation through a fixed bed at two solvents’ flow rates. it is not expect to alter the efficiency.1). 2. reducing the flow rate (i. Stop watch 37     . The amount of effluent should be inversely proportional to the reboiler. Therefore.

9. Then every 5 minutes until 30 minutes have elapsed then at T= 45. Record the final volume in the reboiler.2. 2. FI1. 1. weight 2 kg of blended corn and pour it into the extraction bag. 2. into the solvent charge. Adjust the heat input to give a flow rate of approximately 500 ml/min. 7. DO NOT start up without the permission from your supervisor/lab assistants. 4. 10. 5. Record the collection of this sample as T=0. Sample reboiler contents and effluent every 2 minutes for the first 10 minutes.5 and begin the solvent transfer to the extraction vessel. 15 minutes after solvent has begun to pass through the product cooler. approximately 28 litre of hexane. Take a sample of the first effluent. When a steady value for FI 1 has been determined. Lastly. 12. record its value and the values indicated by TI 1 and PI 4 [steam heating]. Carefully take a sample from the reboiler. Take down the volume of the hexane. measure the flow rate. 11. Weight of solid charge = ____ kg Solvent charge = ____ L FI 1 = ____ ml/min TI.5 EXPERIMENTAL RESULTS Record the following data. 3.1 (Initial) = ____ 0C TI 1 (Final) = ____ 0C TI. 14.6 PROCEDURE CAUTION: Read all operating instructions FIRST to ensure that you fully understand all safety precautions and operating instructions.2 (Initial) = ____ 0C TI 2 (Final) = ____ 0C PI 4 = ____ bar FI 2 = ____ L/min FI 3 = ____ L/min Final volume in reboiler= ____ L (at ____ 0C) 38     . Determine the density for each of the samples taken. Place the extraction bag into the extraction chamber. 13. 6. Fill the solvent. 60. Record the final temperature indicated by TI 1. 8. Close valve V. shut down the extractor and leave it to cool. Before the extraction is started. 90 minutes.

Why is the effluent composition not zero at time zero? 39     . 7. Draw a labeled diagram of the equipment. density of effluent vs time 5. 3. 10. 9. 8. 6. calculate the amount of solute in the reboiler. Use this graph to estimate the amount of solute extracted during the course of the experiment. Alternatively calculate each composition. Plot a graph of loge [composition] vs time for the effluent.6 QUESTIONS 1. Using the final density of the reboiler contents and the corrected final volume. Plot a calibration curve of density vs. Plot a graph of a. Use the calibration graph to convert the data for density of effluent to effluent composition [kg solute/kg solvent]. Use the transformed data to plot a graph of effluent composition vs time. Weight of density bottle (empty) = _____ g Volume of the sample = ____ cm3 Time Weight of sample for Weight of sample for (min) sample point V2 (g) sample point V3 (g) 0 2 4 6 8 10 15 20 25 30 45 60 90 120 2. solute composition. Tabulate the density (kg dm-3) and composition (kg solute/kg solvent) of V2 and V3 at their respective time. 4. 2. density of reboiler content vs time b.

between the two extractions. Explain why the change in density for the reboiler contents appears to be less in rate and magnitude than for the effluent. Comment on the shape of the composition versus time cuves. 11. b. Explain briefly why the effluent density increased during the course of the experiment while the density of the reboiler contents decreased. Suggest the efficiency of the extraction. 17. by composition-time curve or reboiler composition. Carry out mass balance analysis. 12. Comment on the shape of the loge [Composition] versus time graphs. 16. 14. 13. Comment on the agreement or otherwise between the estimates of the amount of oil extracted obtained: a. 40     . 15. What are the effects of contact time on the extraction of corn oil? 18.

gasoline. SEPARATION PROCESS LABORATORY EXPERIMENT 3 BATCH DISTILLATION ON A BINARY MIXTURE       3. the area available for gas dispersers (bubble cap.0 INTRODUCTION Distillation is the main process involved in petroleum refining. perforations) decreases.1. the minimum allowable capacity to determine the effectiveness of dispersion and contacting of the phases.1 THEORIES AND EXPLANATIONS 3. and heavy distillates or residuum category (fuel oil.2 Useful calculations for binary distillation 3. The fractioning column of LS-32205 consists of equally-spaced plates using a liquid downcomer which is important in determining the stability and transfer efficiency of the system. The most common gas disperser for cross-flow plates has been the bubble-cap. wax and tar).2. The products of oil processing are usually grouped into three categories: light distillates (liquefied- petroleum gas. The column operates as an enriching section. As the downcomer area increases. or (ii) constant overhead composition. 3. 3.  The plate-column capacity is determined by the maximum allowable capacity to avoid increasing pressure drop which leads to flooding and on the other hand.1) !" where V is the volume of component (cm3).1.1 Convert data to mole fraction !" Number of mol of component. varying overhead composition. A batch of liquid is charged to the reboiler and the system is first brought to uniform operation under total reflux. naphtha). which is extensively used in the laboratory and in small production units. This device has a built-in seal which prevents liquid drainage at low gas flow rates.1. Mw is the molecular weight of the component (g/mol). lubricating oils. Then a portion of the overhead product is continuously withdrawn in accordance with the established reflux policy. The progress of batch distillation can be controlled either by (i) constant reflux.1 Batch distillation Batch distillation is the process of separating a specific quantity of a liquid mixture into products. varying reflux. ρ is the density of component (g/cm3). ? = (3. 41     . middle distillates (kerosene and diesel).

2792× ∙ ℃ + 0. Determine the ethanol composition with the refractive index Composition (mol) Feed (XF) 0. Hence the latent heat of feed is.1.2792 Distillate (XD) 0.5℃ − 80℃ = 2.!"# = 0. λF is the latent heat of vaporization of the substance. ̊ C Heat capacity of mixture is.water=158.5 ̊ C for a feed of xF=0. ?!.!"# ∆? + λ! (3.8?? 74. Feed input is given at T=80 ̊ C.5?? ?!. ? ?= (3. !"!"! ×!. ̊ C.656 = 40.58 + 0. 158. ?! ????  ????????   % = ×100% (3. hence.2792×38.4) ?= λ! where CP is the heat capacity of the mixture (J/mol.5℃ + 40. = = 0. CP.163 Reflux ratio.2 McCabe-Thiele method (example calculation steps) For a given set of results as followed.157 40.K). ?!"!!"#$ = ×100% = 3.!"!#!"#!!!"# 3.58 KJ/mol. ∆? = 82.685??/???? ∙ ℃ ??? ??? From T-x-y diagram the feed dew point is 82.2) ?! + ?! Taking the example of 10 V/V% ethanol in ethanol-water mixture.2.656 KJ/mol.1715 mol !"!/!"# !"!"! ×!!/!"! Number of mol of 90 ml distilled water = = 5 mol !"!/!"# !. Given the heat capacity of ethanol and water. KJ KJ λ! = 0.24 (mol fraction).07×10! ??/???? kmol kmol Therefore.!"!#!"# Mol fraction of ethanol in mixture.685?? ∙ ℃×2.07×10! ??/???? 42     . Mole fraction is the percentage of component X exits in the mixture in unit mol.3) ? Ratio value of q obtained to determine the q line equation which required to draw the q line on the McCabe-Thiele diagram.8 KJ/kmol.!"#!/!"! Number of mol of 10 ml ethanol.5℃ Latent heat of water is 40.07×10! ??/???? ?= ???? = 7.312% !. CP. △T is the temperature difference between dew point of feed at feed input ( ̊ C). while the latent heat of ethanol is 38.7208× ∙ ℃ = 98.4 KJ/kmol. 98.45 Bottom (XB) 0.7208×40.ethanol=75.

Under no circumstances should the chemicals be allowed to flow into the main drains. 3.3 Chemical safety and precaution Ethanol is volatile and will evaporate quickly.2 OBJECTIVES AND AIM Objectives: 1. binary mixture (ethanol and water) 3.5) ?= ?− ? ?−1 ?−1 ! Top operating line (TOL) equation is given as ? 1 ?= ?+ ? (3. 200 ml ethanol (for refractive index calibration) 5. Refractometer 4. Beakers 43     . The q-line equation is given as ? 1 (3. To draw temperature profile for the column 3. Aim: 1. To calculate tray efficiency using McCabe Thiele’s graphical method 4. Syringe 7. Distilled water (for refractive index calibration) 6. To investigate the effects of a constant reflux ratio on product composition at top and bottom. Avoid exposing this chemical to the atmosphere for extended period of time. Dispose all unused chemicals in an appropriate manner after the experiment. Work in a well-ventilated area. 2. Stir rod 8. To perform batch distillation on a binary mixture using a bubble cap distillation column. To study a bubble cap tray in action 3.3 EQUIPMENT AND MATERIAL 1. To calibrate a refractive index graph for binary mixture 2. For details refer to the MSDS of each chemical. LS-32205 Bubble Cap Distillation Unit 2.6) ?+1 ?+1 ! 3.1.

Drop a few drops of distilled water onto the sampling area such that the refractometer lens is well immersed.1 Obtaining refractive index calibration data 1. wipe the sampling area. 44     . Figure 3. Switch on the refractometer.4. 4. 3. draw 10 ml component A (distilled water) and pour into a 100 ml beaker (A).4 PROCEDURE 3.1 The schematic diagram for bubble cap distillation unit. 5. Measure the refractive index of component A and jolt down the refractive index shown on the refractometer. 3. Use a clean dry cloth. Pour away the component A (distilled water) on the refractometer. 2. Using a syringe.

Temperature sensors and digital temperature display j. Repeat 6-8 for another 9 times until the mixture contain up to 90 ml of component B (ethanol). Top and bottom product tank h. 9. Water jet vacuum with pressure gauge i.5. Sampling ports e. repeat step 1-9 by switching to 10 ml of component B (ethanol) in beaker (B) and mix with up to 90 ml component A (distilled water) intermittently to get the refractive index. 4.4.2 Experimental set up and checking 1. Feed tank and feed valves f. 10. Drop a few drops of mixture from beaker (A) onto the sampling area such that the refractometer lens is well immersed. Bubble cap distillation column b. 2. Connect the unit to a 415 VAC 3 phase 50 Hz power supply and switch on the power supply. Open valve V9. 3. 7. Measure and record the refractive index. Check that the binary mixture to be distillated has been poured into the reboiler. Pour away the sample. draw 10 ml component B (ethanol) into previous beaker (A). 3. Reflux unit (Reflux divider and reflux valve) c. wipe the sampling area. Attach the inlet hose from the condenser unit to a cold water supply and the outlet hose to a drain. 5. Dosing pump g. Upon completing step 9. 11. 8. 3. NOTE: Do not open valves v8 and v11 when the experiment is running. Open valves V8 and V11 if initial vacuum suction is required. Record the refractive index according to the concentrations as shown in Table 3. 5.2 bar. Ensure that all hand valves on the unit are closed except the one on the water inlet valve V9. Using a clean syringe. Identify the components of LS-32205 bubble cap distillation unit: a. 45     . Switch ON the main power switches on the unit. 6.4. Reboiler/evaporator and two condenser units d. Keep an eye on the pressure gauge. Stir the mixture using a stir rod. section 3. Start the cooling water supply. Use a clean dry cloth. close V8 and V11 when the vacuum pressure reaches 0.1. Control Panel 2.3 Constant reflux 1. Close all the valves on this unit. Collect 10 ml sample in the reboiler to test the refractive index. 4. 3.

13. place it in a beaker filled with cold water. T15 to 95 ̊ C by pressing UP and DOWN button. Open valve V12 on the Top product tank. Tabulate all the data as shown in table 3. Turn on the reboiler heater ON/OFF switch located on the Control Panel.5.2 in section 3. it will begin to show condensate collection. NOTE: Please take note of the temperature change on T11. leave the column at total reflux (100%) for another 10 minutes to allow the system to stabilize. 17. when T11 reaches about 80 ̊ C. To quickly cool down the reboiler’s sample. 8. 9. Once the top product appears in the divider vessel. The reflux controller indicates percentage of condensate returning to the column. 6. record all the temperatures and draw 10 ml sample each from the top product tank (DV3) and the reboiler tank (DV1). 3. Turn on the reflux switch and set the reflux to 100%. Then. for around 20 minutes. Set the power of the reboiler to maximum using the power regulator. 11. NOTE: High power setting is required in order to supply sufficient energy to warm the system up in the initial startup. Table 3. empty the top product vessel and measure its volume to get the product output rate of the system.1 Refractive index calibration table A (ml) B (ml) Mol fraction A Mol fraction B Refractive index 0 10   10 0   10   10   20   10   30   10   40   10   50   10   46     . 7.5 EXERIMENTAL RESULTS 3. 12. 10. Set the feed flow to zero since this is a batch process. 15. At every intervals of 10 minutes.1 Refractive index calibration Record the refractive index from section 3. 16.1 into the table below.5. Change the reflux control to a desired value (80%). Set the temperature of reboiler. All alcohol samples can be reused after the experiment. Measure and note down the refractive index of each sample at constant room temperature. 18. as long as they are uncontaminated. Wait for the vapor to condense in the glass condenser. 14.4. Take 6 set of readings. Record all the temperatures as the initial experiment point.

3.2 Batch distillation (constant reflux) result tabulate table Reflux (%) 100% Constant reflux: _____% T1 (̊ C) T2 (̊ C) T3 (̊ C) T4 (̊ C) T5 (̊ C) T6 (̊ C) T7 (̊ C) T8 (̊ C) T9 (̊ C) T10 (̊ C) T11 (̊ C) T12 (̊ C) T13 (̊ C) T14 (̊ C) T15 (̊ C) 47     . The curve obtained is the ethanol water refractive index calibration. Operating condition: Binary mixture of ________ / _________ (____V/V %) Feed’s refractive index = ___________@_______ ̊ C Heater Set temperature = __________ ̊ C Heater Power = 2kW Table 3.5.2 Effects of a constant reflux ratio on product composition Tabulate all data for batch distillation (constant reflux) as shown in the table below. 60   10   70   10   80   10   90 10   10   20   10   30   10   40   10   50   10   60   10   70   10   80   10   90 Plot the refractive index curve for ethanol (graph of refractive index against mol fraction ethanol).

ii. Top product Refractive index Composition(mol%) Bottom product Refractive index Composition(mol%) i. Plot the VLE data for ethanol water binary mixture using McCabe Thiele diagram. What is the definition of an equilibrium stage? 4. 3. You can refer the calculation steps in section 3. iii. Discuss your findings.1. Can you perform the energy balance and find the heat loss for the distillation column? 8. Discuss the difference of a bubble cap distillation column compared to sieve plate and valve plate columns.6 QUESTIONS 1. 2. What is (are) affecting the performance of the distillation column? Suggest ways to improve the performance of a distillation column. When should/shouldn’t batch distillation been applied? 3. Where in the column is the temperature highest? 5. Plot the mol percent product against time graph for top and bottom products. 6.2. How does a constant reflux ratio affect the top and bottom product composition? How (do you think) would the reboiler heating and feed condition influent the degree of separation? 7. Calculate the number of steps from top product to reach the bottom product composition which indicates the number of equilibrium stages. 48     . Plot the T-x-y diagram of ethanol water for the temperature composition relationship. What are the assumptions behind McCabe-Thiele’s graphical method? Determine the overall column efficiency.

1. The next objective is to observe the change of output when a different value of PID is used for the same set point input. and PS = constant.4) 49     . PROCESS CONTROL LABORATORY EXPERIMENT 1 LIQUID/WATER FLOW (WF) CONTROL 1.1 PID Theories The Proportional – Integral (PI) control ! ?! (1. (ii) the set point is increased and decreased using a step function at a fixed PID in a closed loop. we get the following transfer function. The aim of the experiment is to control the flow rate by using a PID single loop flow control. 1. (1. Taking Laplace transform and rearranging. This experiment is to observe and obtain the response of the controlled variable.3) ? =   ?! ? + ?! ?! + ?! ?? where KC = gain.2) = ?! (1 + ) ?(?) ?! ? The Proportional – Derivative (PD) control ?? (1. PV when (i) the process is run under an open loop condition by changing the manipulated variable values (% of valve opening). and pS = constant.1 THEORIES AND EXPLANATIONS 1. τD = detention time. we use water to simulate a liquid phase flow process. ?(?) 1 (1. we get the following transfer function.0 INTRODUCTION In this experiment. Taking Laplace transform and rearranging.1) ? =   ?! ? + ? ?? + ?! ?! ! where KC = gain. τI = integral time.

This is the Controlled Flow (CF) stream. an orifice plate 50     .6) = ?! (1 + + ?! ?) ?(?) ?! ? In proportional mode. The range of error to cover 0% to 100% controller output is called the proportional band. ?(?) 1 (1. Pipeline Controlled Flow (CF): P21-FT21-CF1-FCV21-T21 .5) ? =   ?! ? + ? ?? + ?! ?! + ?! ?! ! ?? Taking Laplace transform and rearranging. because the one-to-one correspondence exists only for errors in this range. .Manual valves CF2 and WF2 are shut.2 Model WF922 description The process consists of two pipelines of 1” each.1.The interconnecting manual valve MVX and the pump P20 discharge manual discharge valve MF are shut. P22B.Water is pumped from tank T21 by one or two pumps P22A. 2. circulating water around a tank T21 as follows:- NORMAL OPERATION 1. a Control Valve FCV21 and back into tank T21. each value of error has a unique value of controller output in one-to-one correspondence. over some range of errors about the setpoint. linear relationship exists between the controller output and the error. 100 (1. Pipeline Wild Flow (WF): P22A/B-FI22-FE22/FT22-WF1-T21 . For the two-position mode had the controller output of either 100% or 0%. . . The proportional band (PB) of a proportional controller depends on the inverse of the gain. via a Variable Area Flowmeter (Rotameter) FI22. a smooth. a manual valve CF1.Water is pumped from tank T21 by pump P21 via a Vortex Flowmeter FT21. ?(?) = ?! (1 + ?! ?) ?(?) The Proportional – Integral – Derivative (PID) control ! ?! ?? (1.7) ?? = ?! 1.

FE22 with a Differential Pressure (DP) Flow Transmitter FT22. Pipeline Wild Flow (WF): P21-FT21-WF2-T21 • However. note that the flowmeter signals to the PID flow controller (FIC21) must also be interchanged so that FE22/FT22 becomes the CF which is the process measurement (PV) signal to the PID flow controller (FIC21). Wild Flow (WF) x R = Controlled Flow (CF) • R is the instrument ratio factor • there must be a Control Valve at the Controlled Flow (CF) pipeline. whilst FT21 becomes the WF to be multiplied by the instrument ratio factor R. Pipeline Controlled Flow (CF): P22A/B-FI22-FE22/FT22-CF2-FCV21- T21 ii. SV is R x WF and MV is the controller output to the control valve. The CF pipeline must have a closed loop in flow control. . • The Control Valve FCV21 is always at the CF pipeline. an external selector switch is provided at the panel and its two position are: 51     . the flow pipeline circuits are interchanged and become:- i. so that there is a closed flow loop around the CF pipeline.g. setting the setpoint (SV) of FIC21. PV = CF. a manual valve WF1 and back into tank T21. This is the Wild Flow (WF) stream. In this case the PV is the variable to be controlled i. 4- 20 mA representing the flowrates expressed in the same engineering units) at both the WF and the CF pipelines. the interconnecting manual valve MVX and the manual discharge valve MF of pump P20 are all shut. Manual valves CF2 and WF2. . One WF pipeline can set more than one CF pipeline but each CF pipeline must have its own flow closed loop with its own PID flow controller and control valve. with its PV.e. • To interchange the flowmeter signals to FIC21. . • the instantaneous WF is multiplied by the instrument ratio factor R (i.  For Ratio Control. NOTE THAT PUMP P20 IS OFF AND NOT USED. SV and MV. There is no PID controller for the WF pipeline. • there must be flowmeters with linearised signal transmission (e.e. INTERCHANGE OPERATION If manual valves CF2/WF2 are opened but CF1/WF1 are shut. R x WF) and this signal becomes the instantaneous remote setpoint (SV=R x WF) cascaded to the PID flow controller controlling flow at the CF pipeline.

For panel operation and control. Controller FIC21 is configured for Ratio control using one PID (PID1). PV = CF. SV and MV. Set the PID values of proportional band (PB). CF2/WF2 Shut • Controller Selector Switch Position 1: “FT21=PV=CF” The recorder FR21 displays: Red pen/Channel 1 : FT21 Green pen/Channel 2 : FT22 The CF pipeline must have a closed loop in flow control. SCADA/DDC selector switch should be at the ‘PANEL. There is no PID controller for the WF pipeline. the PANEL. One WF pipeline can set more than one CF pipeline but each CF pipeline must have its own flow closed loop with its own PID flow controller and control valve.   1. PID1. select Position 2: “FT22=PV=CF”. Operate and read the Chart Recorder. Otherwise. Aim: Learn how to 1. SV1 and MV1 throughout. if a DCS is connected. NOTE: Since only ONE PID is used i.e. 4. This 52     . the PV. SV is R x WF and MV is the controller output to the control valve. operation and control is only from the control panel. with its PV. 3. The NORMAL OPERATION is for FT21 to be the Controlled Flow CF. Adjust Manipulated Variable (MV) and Set Point Variable (SV). integral time (τI) and detention time (τD).2 OBJECTIVE AND AIM Objective: To control water flow using PID controller. SV and MV are understood to mean PV1.e. 1. Move between Manual (M) and Auto (A) control mode. In this case the PV is the variable to be controlled i.3 EQUIPMENT Model WF922 flow ratio process control training unit Control System and Instrumentation The processes can be operated and controlled from the control panel or the DCS (Distributed Control System). Thus • CF1/WF1 Open. 1: “FT21=PV=CF” 2: “FT22=PV=CF” For FT22 to be the CF. SCADA’ position. 2.

Instrument Description Label Variable Area This flowmeter is for local indication only FI22 Flowmeter or and has no transmitting output. Field-Mount Instruments: Transmitters. Control Valve. Rotameter. E for the measuring element. All instruments and controls are Tag-named as follows:- • the first letter describes the process variables such as F for flow. CV is for control valve pneumatically operated and SV is for electrically operated ON/OFF solenoid valve. If the Positioner is integral with the IP converter. it is further represented as PP. please refer to a separate manual for the instrument specifications etc. I for indicator. A for Alarm and V for valve. 53     . • the Tag ends in digits differentiating different instruments of the same process variables and functions. For more details. P for pressure and T for temperature. the integral unit is represented as EP i. Note that for SCADA operation. Orifice plate It is a flow element for 1” nominal pipe. T for transmitter of the measurement sensor. selector switch is at the front cubicle beneath the Instrument control panel.e. IP + PP. The letters CY represent such a control accessory. The instruments mounted at the field (plant) are asterisked (*) in (c) and further detailed below. Gauges. a DCS with a SCADA configuration must be connected. L for level. For more specific details. etc . If a pneumatic Positioner is used at the control valve. C for control (ON/OFF or PID). R for recorder. PID throttling control valve requires an IP converter (CY) which converts a 4-20 mA signal proportionately into a 3-15 psi signal. S for switch (ON/OFF). FE22 Differential It measures the pressure drop (h) across FT22 Pressure (DP) the tapping points of the orifice for a Transmitter 3 calibrated flow range of 0-6 m /Hr. please refer to your instructor on Typical Notation/ Symbols. H and L refer to High and Low alarm (annunciator) limits when used with A (alarm). • the subsequent letters described the functions.

Liquid filled and complete PG22 with snubbers to minimise pressure pulsation. If the selector switch is at Position 1. PP Positioner pass. Vortex Flowmeter Calibrated Range: 0-6 m3/Hr FT21 Control Valve Control Valve. Analog display in the form of horizontal coloured bar or pen. Equal % characteristics. at Position 1) or FT22 (during INTERCHANGE OPERATION. Calibrated Range 0-6 m3/Hr • Green pen (Channel 2): FE22/FT22. FCV21 Air to Open (ATO). then: • Red pen (Channel 1): FT21. Calibrated Range 0-6 m3/Hr * Note that the Red pen (Channel 1) is always for CF and the Green pen (Channel 2) is always for WF. Controller Chart Recorder Two analog inputs with pen/bar graph and FR21 selective display in engineering units. Solenoid valve Normally open (NO) SV21 Pressure Relief Safety instruments to vent excess pressure PRV20. CF is either FT21 (during NORMAL OPERATION. Pneumatic Pneumatic Positioner for FCV21 with By. Valves. Current-to-Air Converts 4-20 mA to 3-15 psig FCY21 Converter proportionately. PRV21. valve FCV21. 1”. Temperature Measure temperature TG21 Gauge Pressure Gauges Measuring pressure drop across the control PG21. at Position 2). in the system. PRV22A/B Panel-Mount Instruments Instrument Description Label Single Loop Configured for Ratio control using only one FIC21 Multifunction PID (FIC21. PID1).chart paper are to be read as follows: 54     .

For SCADA operation. A PANEL. THE GENERAL FUNCTIONS AND FEATURES DESCRIBED HERE CAN ALSO BE ENGINEERED INTO THE TOTAL TRAINING SYSTEMS. engineering units = Actual readings. if additional communication hardware modules and software are preconfigured in a DCS and the panel controller. engineering units The chart drive is set for fast speed (500 mm/Hr). Any of our process plants can be operated and controlled from either the panel control centre OR the DCS control centre. This selector switch must be in the “PANEL. The same DCS can also be configured with the panel controllers to become a SCADA (Supervisory Control and Data Acquisition) system. in the sense that the DCS receives signals directly from the plant and it controls (PID. The recorder chart drive is started by pressing ON the RCD button with the front swing cover opened. The DCS is configured in Direct Digital Control (DDC) mode. * IF OTHER MAKE OF DCS IS USED INSTEAD. by switching this selector switch accordingly. The panel control systems can be by-passed and be taken over by the DCS (in DDC) mode by switching over the hard-wiring so that all measurement signals from the field are connected directly to the DCS and all control outputs to the field are directly from the DCS. This selector switch must be in the “DDC” position. 55     . SCADA/DDC selector switch is provided at the front cubicle for this switch-over. THE DCS ENGINEERING AND CONFIGURATION OF SUCH MAKE OF DCS WILL BE OUTSIDE OUR CURRENT SCOPE OF WORK. • Analog display in % x Maximum (calibrated range). Distributed Control System (DCS) The *Yokogawa CENTUM CS1000 is a Distributed Control System (DCS) used in Direct Digital Control (DDC) mode. the control functions (PID or ON/OFF) are still done at the panel controllers but the DCS Operator Stations are used for the operators interface with the process. ON/OFF) the plant directly. SCADA” position for SCADA operation. The chart speed is regularly printed on the chart paper. HOWEVER.

set at the “PID1” page or panel. FAL(CF) : Flow of the Controlled Flow stream (CF) drops below the preset Low flow limit. The dedicated alarm window remains lit as long as its process variable is still in the alarm condition. SCADA/DDC selector switch • Pumps Start-Stop pushbuttons for P20. Instrument Control Panel Note the following: • Controller. NORMAL OPERATION. A buzzer will come on and the respective alarm window [FAH(CF). Pressing the Acknowledge button will silence the buzzer sound. Recorder. set at the “PID1” page or panel. Annunciators. PH1. INTERCHANGE • Instrument wiring termination and power supply and wiring: The Instrument panel can be opened from the back to access the Instrument terminations. Front Cubicle Beneath the Instrument control panel is another cubicle with the following at the front of the cubicle:- • Switch for incoming mains 415V/50Hz/3 phase. P22B 56     . 2: “FT22 = PV = CF”. P22A. PLI. • PANEL. • A 1-2 position selector switch for 1: “FT21 = PV = CF”. The front cubicle below the Instrument panel can be opened from the front. The Test button is to test if the Annunciator alarm window lights are working. Annunciators The Annunciators are:- FAH(CF) : Flow of the Controlled Flow stream (CF) exceeds the preset High flow limit. The alarm window light will go off when the process variable is restored to normal. P21. FAL(CF)] will lit up when the above abnormal or alarm conditions occur.

6. B22A. B22B open.3% to open the control valve FCV21 fully. Trace the piping system from the tank overflow pipe to its final discharge. • The bottom manual drain valve of tank T21 is always shut.g. B22B can be shut later after the respective pump has started pumping. 4. Switch controller FIC21 to Manual (M) mode with its MV = +100% e.4 PROCEDURE 1. 5. press the acknowledge button to silence the buzzer. discharge and by-pass valves are fully opened. P22B) suction. • The manual discharge valve MF at the discharge of pump P20 is fully shut. SCADA” position. SCADA/DDC selector switch should be in the “PANEL. Tank T21 should be filled with water up to almost the level of its lower overflow pipe. MF. P21. B21. for NORMAL OPERATION.1 Getting started 1. Instrument air supply (IAS) is required to operate the control valve system. it need not be readjusted frequently. Once set. MVX. P22A. Switch On the following pumps with the manual by-pass valves opened:- Pump P21: Manual by-pass B21 open. Quickly check the various manual valves as follows:- • All pumps (P20. Rationalise the cause of the alarm condition.1. The PANEL. FCY21/PP/FCV21. 106. 2.4. • The interconnecting manual valve MVX is fully shut. Refer to the earlier section “annunciators” and rationalise the cause of the alarm condition. Check that the pressure is in accordance to the pressure indicated at the air pressure regulator (IAS). The panel instruments all lit up. • The manual by-pass valve around the control valve FCV21 should be always shut but its two adjacent manual valves should be always opened. • Model WF922 is connected to a common drain system for draining outside the building. Turn on the main power supply switch at the front cubicle. 2. Check that pump P20 is OFF and its manual discharge valve MF is fully shut. 3. 7. Whenever any annunciator is activated. Shut fully CF2/WF2. The pump by-pass valves B20. Main power supply (415V/50Hz/3 phase) is preconnected to the Model plant. Open fully CF1/WF1. Switch the selector switch to Position1: “FT21 = PV = CF”. P22B: Manual by-pass B22A. Pumps P22A. 57     .

0. Start the recorder FR21 by pressing its RCD button with the front swing cover opened. B21.g. PH1 should be set at 4.e. • In Manual (M) mode.0 so that the flow ratio R = 1. 2. 58     . Also note the PH1 and PL1. PL1 at 1. 106. 1. TI1 = 10 secs.2 m3/Hr. The recorder chart drive should be stopped (press RCD) when its chart recording is not required.2 Training: PID SINGLE LOOP FLOW CONTROL (NORMAL OPERATION): FT21-FIC21-FCY21/PP/FCV21 1. PL1 values once they are set at these values. • Shut the interconnecting manual valve MVX. Shut the pumps manual by-pass valves. PH1 and PL1 are used to set the High and Low flow alarm limits (in m3/Hr) of the process variable PV.4. GW1=0. of pump P20. Access the instrument ratio factor R at the PARAMETER page or panel at CGN1.0 3. The flow single loop is:. GG1=1.3%. • Open manual discharge valves of the pumps P21. which is the controlled flow CF. 9. • Shut the manual discharge valve MF. values. Access the PID tuning panel or page at PID1 and change the PID values to the following first (I) trial PID values.6 m3/Hr. Restore the pipelines and control to NORMAL OPERATION position i. B22A. • Change the setpoint SV to 3. Set CGN1 to 1. Stop the chart drive. FIC21 (PID1): PB1 = 150%. • Controller selector switch is in Position 1: “FT21=PV=CF”.FT21-FIC21-FCY21/PP/FCV21 2. Shut fully CF2/WF2. TD1 = 0 secs. • Open fully CF1/WF1. (60%) • Switch to Auto (A) mode for single loop flow control. Check the chart speed (500 m/Hr) which is regularly printed on the chart. 8. P22A. Do not change these PH1. The PID flow controller is FIC21 (PID1) and the controlled variable PV is FT21. B22B. 4. Be familiar with the controller as follows:- • Display FIC21 and change from Auto (A) to Manual (M) mode and vice versa. PID Controllers setup 1. P22B. manually stroke the control valve FCV21 fully opened with MV = +100% e.0 m3/Hr.0%. Check that the control valve FCV21 is fully opened. Controller FIC21 is configured for Ratio control using one PID (PID1).

7. Switch FIC21 to Auto (A) Mode. 3. Write down the setpoint (sv) and pid values on the recorder Chart paper besides its response. Check the chart speed which is regularly printed out on the chart. GG1 = 1. 4. 59     . Set the setpoint SV = 1. ON. With the controller FIC21 still in Manual (M) mode at MV=100%. • Check that the adjacent upstream/downstream manual valves of FCV21 is fully Opened but its manual by-pass valve is fully shut.0%.0 5. Manually adjust MV so that PV approaches SV. 9.e. or continues to Oscillate even after 3 cycles. These chart recordings constitute the results of your experiment and should be kept for your report. Switch ON only pump P21 and shut its manual by-pass valve B21. 8. set its first (I) Trial Linear PID values as follows:- FIC21(PID1) : PB1 = 150%. and not By- passed. Observe the response of FT21 at the red pen until it is almost Steady at the setpoint to within ±0. 6. 1. TD1 = 0 sec : GW1 = 0.8 m3/Hr. • The Positioner (PP) at FCV21 must be CONNECTED i. TI1 = 10 secs.02 m3/hr. The recorder FR21 chart drive should be at fast speed (500 mm/Hr) with RCD ON.5 EXPERIMENTAL RESULTS Attach the recorder chart paper(s) with clearly marked details.

τD = detention time. It is usually applied in reaction process control and storage tank control.2) = ?! (1 + ) ?(?) ?! ? The Proportional – Derivative (PD) control ?? (1. PROCESS CONTROL LABORATORY EXPERIMENT 2 LIQUID/WATER LEVEL FLOW (WLF) CONTROL 2. and PS = constant. we get the following transfer function. τI = integral time.1) ? =   ?! ? + ? ?? + ?! ?! ! where KC = gain.1 THEORIES AND EXPLANATIONS 2. 60     .1. The purpose of this control is to control the level of the tank at its desired value. Level conductivity probes are used to detect water level.0 INTRODUCTION Level control is very important in chemical industry. The liquid flow is measured by the differential pressure across an orifice. which may eventually lead to unwanted incident or explosion. and the water level of the tank is measured through the differential pressure (DP) level transmitter. The model WLF922 uses water to simulate a liquid phase level and flow process.3) ? =   ?! ? + ?! ?! + ?! ?? where KC = gain. Taking Laplace transform and rearranging. and pS = constant. ?(?) 1 (1.1 PID Theories The Proportional – Integral (PI) control ! ?! (1. 2. Failure to control the level of a system may cause the tank to overflow or dry up.

?(?) (1. multiplied by the liquid density. Taking Laplace transform and rearranging. It works on the principle that the hydrostatic pressure at any point in a column of the liquid depends on the level of the liquid column above this point. a DP transmitter is also the most common level measuring device in industrial process plant. This works on the fluid mechanics principle that the liquid volumetric flowrate (F) is proportional to the square root of the pressure drop (h) across an orifice flow element. The proportional band (PB) of a proportional controller depends on the inverse of the gain.4) = ?! (1 + ?! ?) ?(?) The Proportional – Integral – Derivative (PID) control ! ?! ?? (1. The range of error to cover 0% to 100% controller output is called the proportional band.e.1. the hydrostatic pressure is a measure of the level. because the one-to-one correspondence exists only for errors in this range. we get the following transfer function. each value of error has a unique value of controller output in one-to-one correspondence. An open tank system requires one wet 61     .1) ! This equation is only true if the flowrate is high enough to be called turbulent flow. If the tank liquid density is constant. 100 (1. linear relationship exists between the controller output and the error. For the two-position mode had the controller output of either 100% or 0%.7) ?? = ?! 2. i. over some range of errors about the setpoint. a smooth.6) = ?! (1 + + ?! ?) ?(?) ?! ? In proportional mode.5) ? =   ?! ? + ? ?? + ?! ?! + ?! ?! ! ?? Taking Laplace transform and rearranging. On the other hand. ! ? = ? = ? ℎ if the density is assumed constant (2.2 Open Tank Flow and Level Measurement The most common industrial flowmeter is the orifice plate with a DP transmitter. ?(?) 1 (1.

The low pressure chamber is opened to the atmosphere. The top space of T31 is pressurised with air from the pressure regulator AR31 to about 2. T31 as an Open or Closed Tank The top vent (V) and overflow drain (D) manual valves are opened to operate T31 as an Open tank (so that the top space of T31 is at atmospheric pressure).1.5 psig is equivalent to about 1760 mm Water level at ambient temperature.0 psig. The DP transmitter therefore measures H (tank level) × D (density of tank liquid) × g (gravity). as monitored by the pressure gauge PG31. If the density (D) of the tank liquid is constant. Note that a pressure of 2. note that when T31 is pressurised as a Closed tank. the inflow rate will be slightly reduced but its outflow will be increased slightly. The PID single inflow control loop is: FE31/FT31- FIC31-LCY31/PP/LCV31. However. Excessive pressure will cause the pressure relief valve PRV31 to vent. the measured DP is a measure of the tank level H. using the two wet legs technique. cancelling the pressure at the top space of the open tank.5 to 3. The level transmitter LT31 is installed to measure the tank level. 2. and vice versa operating T31 as a Closed tank. Level Process as Self Regulating (SR) or Non-Self Regulating (NSR) The first thing to note in controlling a level process (or any process) is to check whether it is Self Regulating (SR) or Non-Self Regulating (NSR). the outflow of T31 is by 62     . leg connecting the tank bottom to the high pressure chamber of the differential pressure transmitter. Measurement and Control of Level in tank T31 The PID single level control loop is: LT31-LIC31-LCY31/PP/LCV31.3 Model WLF922 description The process consists of a level tank T31 and a collection tank T32 connected with the appropriate pumps and piping system for the study of:- Measurement and Control of Flow into T31 from T32 Water is pumped by pump P32 from tank T32 into T31 and is referred to as the INFLOW. For Self Regulating Single Capacity Level Process.

• LIC31. • FIC31. Flow Single Loop.Flow (secondary) Cascade: LT31-LIC31-FIC31-LCY31/PP/LCV31 (FE31/FT31) Selector switch in Position 2: CASCADE LIC31- FIC31. Two outflow gravity pipes are provided each with its own manual valve. LIC31 in Auto (A) or Manual (M) mode. PID1. Level Single Loop. the outflow also decreases. Level (primary) . FIC31 is the slave or secondary. 63     . Only one pipe is to be operated as the outflow. SCADA/DCS selector switch at the front cubicle to the “PANEL. The second manual valve remains shut. LIC31/FIC31: Single Loop Programmable Controller. The outflow is dependent on the level. The Self Regulating process is able to control its own level and unlikely to overflow or run dry. Switch the PANEL. SCADA” position for Panel operation. When the inflow increases. Flow PID Controller • In Cascade mode. LIC31 is the master or primary. when the inflow decreases. PID. FIC31 in Cascade (C) mode. PID2. Level PID Controller • FIC31-Loop 2. Similarly. gravity from the tank bottom discharge pipe. the level also increases which therefore increases the outflow. Three control strategies can be operated as described earlier in (c). Configured for:- • LIC31-Loop 1. FIC31 in Auto (A) or Manual (M) mode. Such self regulating mechanism makes the control of a Self Regulating process easier to control. PID1. PID2. • LIC31/FIC31. Loop 2: FE31/FT31-FIC31-LCY31/PP/LCV31 Selector switch in Position 2: CASCADE LIC31- FIC31. Panel-Mount Instruments The panel-mount instruments are listed below. Loop 1: LT31-LIC31-LCY31/PP/LCV31 Selector switch in Position 1: LIC31.

0 m3/Hr. engineering units. Calibrated Range 0-3 m /Hr Analog display in % x Maximum (calibrated range). 64     . ETC. engineering units = Actual reading. Control output of LIC31 (MV1) becomes the remote setpoint (SV2) of FIC31. FT31 Differential Pressure (DP) Flow Transmitter Calibrated for 0-3. CONTROL VALVE.0 m3/Hr.e. Calibrated Range = -800 to 0mm Water Gauge (WG) Transmitted to LIC31. The chart drive is set for fast speed (500 mm/Hr). Open (to atmospheric pressure) or Closed (pressurised). press C) and the Selector switch must be in Position 2. two analog inputs with pen/bar graph and selective display in engineering units. • Red pen (Channel 1): Level. with square root function Transmitted to FIC31 LIC31 PID controller (PID1. Calibrated Range 0-800 mm WG 3 • Green pen (Channel 2): Flow. LFR31 : chart recorder. Note that only FIC31 can be Cascaded (i.076 mm for 0-3. The instrumentation mounted at the field (plant) are further detailed below: LT31 Differential Pressure (DP) Level Transmitter Measures level of tank T31. Air-to- PP Open (ATO) Pneumatic Positioner (PP) for LCV31. LIC31 in Auto (A) mode. GAUGES. with By-pass. FIELD-MOUNT INSTRUMENTS: TRANSMITTERS. Orifice d = 11. radius *ID-½D taps connected to FT31. LCV31 1” Control Valve with Equal % characteristics. Selector: Position 1) configured in the panel-mount Single Loop Programmable Controller LIC31/FIC31 FIC31 PID controller (PID2. The recorder chart drive is started by pressing ON the RCD button with the front swing cover opened. FE31 1” Orifice plate. Selector: Position 2) configured into the panel-mount Single Loop Programmable Controller LIC31/FIC31.

The annunciators LAH32.SV2 respectively when the selector switch is in Position 2. 2. 65     . PRV33 LFR31 Chart recorder.2 OBJECTIVE Objective: To control water level using PID controller. Aim: Learn how to 1. engineering units = Actual reading. The chart drive is set for fast speed (500 mm/Hr). LS32 Conductivity Level Switch PG31. Adjust Manipulated Variable (MV) and Set Point Variable (SV). Calibrated Range 0-3 m3/Hr Analog display in % x Maximum (calibrated range). Calibrated Range 0-800 mmWG • Green pen (Channel 2): Flow. PRV31. PRV32. REMARKS: The PV. Pressure Relief Valves. FAL31: Inflow to T31 measured by FE31/FT31 is below the preset Low alarm limit.SV1 and PV2. LAH31. Move between Manual (M) and Auto (A) control mode. The Low alarm limit is set at PL2 at the “PID2” page. PG32 Pressure Gauges SV31 Solenoid valve. SV in the main display pages (faceplates) of LIC31 and FIC31 become PV1. normally open (NO). LAH32: Tank level at T32 exceeds the High level limit (shortest probe) of the Level Switch LS32. two analog inputs with pen/bar graph and selective display in engineering units. LCY31 Current-to-Air Converter Converts controller output from 4-20 mA into a proportional pneumatic signal of 3-15 psig to stroke the control valve LCV31. LAH31: Tank level at T31 measured by LT31 exceeds the FAL31 preset High level alarm limit. • Red pen (Channel 1): Level. engineering units. 2. The High alarm limit is set at PH1 at the “PID1” page.

• the subsequent letters described the functions. a DCS with a SCADA configuration must be connected. E for the measuring element. T for transmitter of the measurement sensor. Set the PID values of proportional band (PB). H and L refer to High and Low alarm (annunciator) limits when used with A (alarm). PID throttling control valve requires an I/P converter (CY) which converts a 4-20 mA signal proportionately into a 3-15 psig signal. C for control (ON/OFF or PID). integral time (τI) and detention time (τD). The letters CY represent such a control accessory. R for recorder. 4. it is further represented as PP.4 PROCEDURE 66     .e. P for pressure and T for temperature. Operate and read the Chart Recorder. The selector switch is at the front cubicle beneath the Instrument control panel. If the Positioner is integral with the I/P converter. if a DCS is connected. the PANEL. 2. If a pneumatic Positioner is used at the control valve. operation and control is only from the control panel. SCADA” position. 3. S for switch (ON/OFF). All instruments and controls are Tag-named as follows:- • the first letter describes the process variables such as F for flow. Otherwise. 2. Note that for SCADA operation.3 EQUIPMENT Model WLF922 level flow process control training unit CONTROL SYSTEM AND INSTRUMENTATION The processes can be operated and controlled from the control panel or the DCS (Distributed Control System). For panel operation and control. • the Tag ends in digits differentiating different instruments of the same process variables and functions. A for Alarm and V for valve. I for indicator. L for level. IP + PP. the integral unit is represented as EP i. SCADA/DCS selector switch should be at the “PANEL. CV is for control valve pneumatically operated and SV is for electrically operated ON/OFF solenoid valve.

2. • Model WLF922 is connected to a common drain system for draining outside the building. Trace the drain piping system from the tank T32 overflow pipe to its final discharge. Quickly check the various manual valves as follows:- • Locate the Inflow pump P32. discharge and by-pass valves are fully opened. 2. open the by-pass manual valve B33 of pump P33 to divert any flow back into T32. 67     . open fully its manual suction valve but shut fully its two manual parallel discharge valves. thus operating only one gravity discharge pipeline at the bottom of tank T31. 4. leading to the drain. located next to the preset Air Regulator AR31.1 Getting started 1. For pump P33. open fully its manual suction and by-pass valve but make sure its manual discharge valves MV-T and MV-D are fully shut. Tank T32 should be filled with water up to and just below the level of the shortest level probe (not visible) of the Level Switch LS32 which is slightly below the tank (T32) overflow pipe outlet. Also shut the manual valve MV-D at the discharge of pump P33. 3. • Operate T31 as an Open tank with the top vent (V) and overflow drain valves fully opened. To operate Model WLF922 independently. 4. For the Outflow pump P31. • The manual by-pass valve around the control valve LCV31 should be always shut but its two adjacent manual valves should be always opened. For Independent Operation. The second manual globe valve at the second gravity discharge pipe must remain shut. • Operate T31 as a Self Regulating process. Top up the water later whenever necessary. Shut the interconnecting pipeline from Model WLF922 to Model WT922 at the appropriate manual valves MV-T. Check that its manual suction. • The bottom manual drain valve of T32 is always shut.4. The pressurising air inlet to T31 is isolated at its inlet manual valve (with the valve handle at 90° to the air supply inlet tubing). pump P31 must be OFF. Open only the manual GATE valve at the gravity discharge pipe at the tank bottom. For a Self Regulating process. Shut the two manual discharge valves of Outflow pump P31. Compressed air is required to operate the control valve system LCY31/PP/LCV31. the panel-mount selector switch for P33 must be in the Manual or “OVER-RIDE P33” position. one of which is at the strainer inlet.

SV1 is its setpoint and MV is manipulated variable or control output to the control valve. • The air regulator (AR31) for pressurising tank T31 is preset to about 3. Rationalise the Cause of the alarm condition. To be switched ON during operation.e Level of T31. SV1 are displayed as PV. The panel instruments all lit up. SCADA” position for Panel Selector switch operation. Note PV1. Note the following switches and pushbuttons but do not switch ON any pump yet. 68     . Whenever any annunciator is activated. Loop 1). press the Acknowledge button to silence the buzzer. 5a. Use the drain/bleed valve at the bottom of the air regulator (IAS). in which case the bottom gravity discharge pipes of T31 must be all shut. 5b. Pump P33 : Leave it in ‘OVER-RIDE P33’ position for the time being. There is no need to adjust this pressure (IAS) too frequently. • Do not pressurise T31 yet. SV1. PV1. Pump P31 : Do not use unless T31 is to be operated as a Non-Self Regulating process. Turn on the main power supply switch at the front cubicle.0 psig and need no adjustment. MV. Main power supply is pre-connected to the Model plant. Shut the pressurising air inlet manual isolation valve (with the valve handle at 90° to the air supply inlet tubing) located next to AR31 near the top of tank T31. Pump P32 : Pumping inflow from T32 to T31. In Position 1. Loop 1) Switch to Position 1 (LIC31): Single Level Loop LIC31 (PID1. Any higher pressure will cause the pressure relief valve PRV31 to open. PID Controller 1. • Check that the pressure is in accordance to the pressure indicated at the air pressure regulator (IAS).SV for LIC31 PV1 is process variable i. control output to the control valve. • It is good practice to purge the air regulator (IAS) to remove any condensed water. Check that the two manual discharge valves of pump P31 are shut. SCADA/DC : Switch to “PANEL. Controller LIC31/FIC31 is configured with PID controller: LIC31 (PID1. PANEL.

do not by-pass it. Operate tank T31 as a SELF REGULATING LEVEL 1. 69     . Check that LCV31 is about 60% opened. 3. The recorder chart drive should be stopped (press RCD) when its chart recording is not required. LFR31 by pressing the RCD button ON. Instrumentation 1. adjust MV = 25%. Check the recorder chart speed (500mm/Hr) which is regularly printed out on the chart. 2. adjust MV = 60%. The ‘STC’ should be in the “DISP” (Display) mode. (Press the blue push button located at the bottom right side of the controller LIC31/FIC31.) Note the A (Auto) and M (Manual) pushbuttons. Change to the Self-Tuning page (STC1. 2. Start pump P32 and then shut its manual by-pass valve B32. if necessary. Shut the two manual discharge valves of pump P31. 2. 3. With LIC31 in Manual (M) mode. Do not operate P31. Switch OFF the recorder chart drive. Make sure ‘STC’ is not in ‘ON’ mode. Make sure only the manual GATE valve at the gravity discharge pipe at the bottom of tank T31 is opened. With LIC31 in Manual (M) mode. Set the 1-2 Selector switch to Position 1 to operate LIC31 and display LIC31. with the front swing cover opened. from LIC31 4. The Positioner (PP) should be connected and used throughout. to select the display of LIC31. Check that LCV31 is about 25% OPENED (see the indicator scale at the valve stem). The second gravity discharge pipeline and its manual globe valve must remain shut. but USE THE Positioner (PP). Chart recorder 1. Press M and leave LIC31 in Manual (M) mode. With the 1-2 Selector switch in Position 1. 2. Also note that the control valve LCV31 is Air-to-Open (ATO).e. In Manual (M) mode. Loop 1 accordingly. Start the recorder. 4. manually stroke the control valve LCV31 with MV = 50%. Check that the controller Selector switch is in Position 1. Display LIC31 at the controller. Make sure the Positioner (PP) is connected to LCV31 i. Check the Positioner (PP) manual By-pass switch at LCV31/PP. display LIC31. 3.

2. Note the rising water level at tank T31 at its level sight glass. 70     . set MV = 75%. 2. 3. Loop1): PB1 = 30%. Start pump P32 and watch the level (PV1) increases. Set the first (I) trial PID values at the ‘PID1’ page or panel as follows:. Make sure the overflow drain manual valve at the top of tank T31 is fully opened for water to overflow back into T32.4. 4. TD1 = 0 6.5 EXPERIMENTAL RESULTS Attach the recorder chart paper(s) with clearly marked details. TI1 = 25secs. 6. Operate tank T31 as a Self Regulating Open tank process 2. Set the second first (II) trial PID values at the ‘PID1’ page or panel as follows:. Set the setpoint (SV1) of LIC31 to 400 mm. 8. 7. TI1 = 15secs.2 Training: Study level control using loop LT31-LIC31-LCY31/PP/LCV31 1. Check that the stem position of control valve LCV31 is about 75%. display LIC31 faceplate at the controller. switch LIC31 to Auto (A) mode and observe the Level (red pen) response at the recorder LFR31. TD1 = 0 Repeat steps 6-8. 5.LIC31 (PID1. With LIC31 in Manual (M) mode. With the controller Selector switch in Position 1. 5. Shut the pump by-pass valve B32. When the level is near to the setpoint SV1. Loop1): PB1 = 10%. 9. Press the RCD pushbutton with the front swing cover opened.LIC31 (PID1.