DKK3761

Engineering Lab IV DKK3761

Faculty of Chemical & Natural Resources Engineering

DKK3761

ENGINEERING LAB IV

Name

Matric No.

Group

Program

Section

Date

Sem. I - Session 2010/2011

1


Vision

To be a center in producing professionals in the area of chemical and natural resources engineering,

with emphasis on industrial practices and applications.

Mission

To provide for the study of chemical and natural resources engineering in an industrial context

through outstanding education, research, and development.

Program Educational Objective (PEO)

PEO 1: Our graduates will demonstrate effective communications, leadership and teaming skills

PEO 2: Our graduates will demonstrate the foundation and breadth to obtain, apply, and transfer

knowledge across disciplines and into emerging areas of chemical engineering and

related fields

PEO3: Our graduates will demonstrate the foundation and depth for successful chemical

engineering careers in industry, academia, or government

PEO 4: Our graduates will demonstrate that they have a sense of responsibility are ethical in the

conduct of their profession, and have an appreciation for the impact of their profession on

society.

Program Outcomes (PO) for Laboratory

The students are expected to attain the following;

PO1 Ability to acquire and apply knowledge of science and engineering fundamentals.

PO2 Acquired sufficient technical competence in chemical engineering and related disciplines.

PO3 Ability to assist and solve chemical engineering and related problems under supervision.

PO4 Ability to communicate effectively, in verbal and written forms, with both technical and

non-technical groups.

PO9 Ability to function effectively as an individual and in a group with a capacity to be a leader

in sub professional level.

2


CONTENTS

PAGE

A. Teaching Plan 4

B. Laboratory Report Format & Evaluation 5

B1. Laboratory Report Format

B2. Report Evaluation

B3. Laboratory Front page

C. Occupational Safety & Health (OSH) 11

C1. FKKSA Occupational Safety & Health

C2. General Laboratory Safety Procedures

C3. Chemical Safety Data Sheet (CSDS) for Ethylene Glycol

C4. Chemical Safety Data Sheet (CSDS) for Ethanol

C5. Emergency Notification & Response

D. Experiment 23

Exp 1: Tray Dryer Unit

Exp 2: Climbing Film Evaporator Unit

Exp 3: Absorption Column Unit

Exp 4: Thin Film Evaporator Unit

Exp 5: Rotary Evaporator Unit

Exp 6 Sieve Tray Distillation Unit

Exp 7: Short Path Distillation

Exp 8: Pressure Swing Adsorption

3


A. TEACHING PLAN

4


LABORATORY REPORT FORMAT & EVALUATION

B1. Laboratory Report Format

1. Front page

2. Abstract

3. Introduction

4. Literature Review

5. Experiment Objective

6. Methodology

7. Result and Discussion

8. Conclusions & Recommendations

9. References

10. Appendices

B2. Report Evaluation:

Part A : 55%

(Inclusive of Front Page/Format; Abstract; Introduction; Literature Review; Experiment

Objective; Methodology; Conclusions & Recommendations; References; Appendices; Grammar

& Spelling; Timeliness)

Part B : 45%

(Inclusive of Result and Discussion/Questions)

5


Report Evaluation For Part A

Instruction: Please assess each item using the given scales. Fractional marks will be given for each category.

Item AssessedUnacceptable

(1)Acceptable

(2)Good

(3)Very Good

(4)Excellent

(5)Score

Organization and Format

Not follow FKKSA laboratory report format. Not well organized. Contents show lack of knowledge.

Partially follow FKKSA laboratory report format. Contents show enough of knowledge but still a few concept and ideas are loosely connected.

Follow FKKSA laboratory report format of writing; all needed sections present. Well organized. Contents show enough knowledge of subject.

Follow FKKSA laboratory format of writing; all needed sections present. Well organized and easily followed. Contents show full knowledge of subject.

Follow FKKSA laboratory report format of writing; all needed sections present. Tables and figures are correctly drawn and numbered. Excellent organized and easily followed. Contents show full excellent knowledge of subject.

Keywords: Front page, Content, Page No., Total page >8, Arrangement

Abstract Several major aspects of laboratory report are missing. Incomplete description of experiment.Student displays a lack of understanding about how to write an abstract.

Abstract misses one or more major aspects of laboratory report.

Abstract contains most major aspects of laboratory report.Abstract may be too technical and only understood by specialist in the discipline.

Abstract contains all major aspects of laboratory report i.e. main purpose of the experiment, its importance, methodology/ approach, most significant results or findings, main conclusions and/or recommendation.

Abstract contains references to all major aspects of laboratory report i.e. main purpose of the experiment, its importance, methodology/ approach, most significant results or findings, main conclusions and/or recommendation.General audience easily understands abstract.

Keywords: Introduction, Objective, Method, Result, Conclusion, Suggestion, 1 page

6



(1)Acceptable

(2)Good

(3)Very Good

(4)Excellent

(5)Score

Introduction Very little background information or information is incorrect OR, does not give any information about what to expect in the laboratory report

Some introductory information, but still missing some major points. OR, gives little information

Introduction is nearly complete, missing some minor points.

Introduction is complete and well written but theory may not be backed up to concise lead-in to the laboratory experiment.

Introduction is complete and well written; provides all necessary background principles and theory for the experiment. Present a concise lead-in to the laboratory experiment.

Keywords: Related Theory, Principles, Process Background

Literature Review Poor understanding of topic experiment, inadequate information or very little information regarding experiment topic.No external literature review.

Acceptable understanding of topic, adequate information evident, sources cited.Insufficient literature review or may contain unrelated materials.

Good understanding of topic, adequate information evident, sources cited.Sufficient literature review.

Good understanding of topic, adequate information evident, sources cited.Sufficient and relevant literature review.

Complete understanding of topic, topic extensively well-informed and variety of sources are cited.Literature review contains information relevant and directly related to experiment topic.

Keywords: Experiment Topic Information

Experiment Objective

No objective or objective missing the important points.

Objective is partially defined.

Objective is relevant but not elaborated.

Objective is clear, relevant and elaborated but missing some point on relevant explanation.

Objective is precise, clear, relevant and well elaborated with relevant explanation.

Keywords: Objective Elaboration

7



(1)Acceptable

(2)Good

(3)Very Good

(4)Excellent

(5)Score

Methodology Missing several important explanations of materials and/or methodology. Not sequential. Most steps are missing or are confusing. Some procedural components generally described but are not replicable.

Materials and methodology nearly complete but still missing some important experimental details. Others may have difficulties following procedures; some steps are understandable; but most are confusing and lack detail. Can replicate experiment if reader makes some inferences.

Materials and methodology are explained with sufficient detail; some lack detail or are confusing. Mostly easy to follow. Description of procedure makes it likely that the work can be reliably replicated.

Materials and methodology are complete. Mostly easy to follow. Description of procedure can be replicated.

Materials and methodology are complete and adequately detailed. Logical and easily followed. Description of procedure is complete, ensuring that it can be replicated.

Keywords: Experiment Procedure, List of Equipment

Conclusions and recommendations

No conclusions or conclusion missing the important points. No recommendation given to improve the experiment.

Conclusions regarding major points are drawn, but many are misstated, indicating a lack of understanding.Conclusion is too general. Several recommendations have been given but they are too general and not contributing to the experiment’s improvement.

All the important conclusions are drawn could be better stated.Conclusion is related to general interest. Several recommendations have been stated and they are partially contributed to the experiment’s improvement.

All the important conclusions have been made.Conclusion is precisely stated.Conclusion and recommendation relates the study to general interest and other studies that have been conducted.

All the important conclusions have been clearly made. Conclusion is precisely stated and relates the study to general interest, other studies that have been conducted. Recommendations given are significantly contribute to the experiment’s improvement.

Keywords: Experiment Summary, Recommendation

8



(1)Acceptable

(2)Good

(3)Very Good

(4)Excellent

(5)Score

References Some citations in text are not available in list of reference.

A few citations in text are not available in list of reference.

All citations in text are available in list of reference but list of reference is less than 3.

All citations in text are available in list of reference and list of reference is more than 3.

All citations in text are available in list of reference. List of reference is more than 3 and variety source.

Keywords: Book Reference, Journal Reference, Website Reference

Appendices Appendices not available in laboratory report.

Only a few appendices available in laboratory report.

Appendices available in laboratory report but poorly constructed

Appendices available in laboratory report in structured manners

Appendices available in laboratory report in structured manners, clearly and precise

Keywords: List of Formulas, Tables, Figures, Calculation

Grammar and Spelling

Numerous spelling and/or grammar errors. Transitions confusing and unclear.

Still many spelling and/or grammar errors. Few or weak transitions, often wanders and jumps around.

Occasional grammar/spelling errors. May have a few unclear transitions.

Occasional grammar/spelling mistakes. Spell checked and proofed throughout. Good sentence and paragraph structure and transitions.

Minimal to no spelling mistakes. Spell checked and proofed throughout. Good sentence and paragraph structure and transitions.

Keywords: Language

Timeliness Laboratory report handed in more than one week late

Up to one week late Up to three days late Handed in one day late

Laboratory report handed in on time

Keywords: Punctuality

Total Assessment Marks (55%)

9

Engineering Laboratory IV DKK3761

B3. LABORATORY REPORT FRONTPAGE

ENGINEERING LABORATORY IV

(DKK3761)

2010/2011 Semester 1

Title of Experiment :

Date of Experiment :

Date of Submission :

Instructor’s Name :

Group of Member :

Name ID

1.

2.

3.

4.

5.

Group No. :

Section :

Marks :

FACULTY OF CHEMICAL AND NATURAL RESOURCES ENGINEERING

10

Part A 55

Part B 45

TOTAL 100


UNIVERSITI MALAYSIA PAHANG

C. SAFETY, HEALTH & ENVIRONMENT (SHE)

C1. FKKSA SAFETY, HEALTH AND ENVIRONMENT POLICY

In our mission to disseminate knowledge, stimulate teaching and learning, and

inculcate soft-skills, the FACULTY OF CHEMICAL AND NATURAL RESOURCES

ENGINEERING is fully committed in practising Safety, Health and Environment with

the aim of achieving the highest standards of Occupational Safety Health and

Environment (SHE) and prevent from incidents, injuries, ill-health and pollution to

air, water, land and noise from our activities.

In line with UMP OSH policy, FKKSA will preserve the Safety, Health and

Environment of its employees, students and related parties in accordance with

safe system of work and SHE best practices.

It is our policy to:

Provide our employees, students and related parties with sufficient information

and effective training related to Safety, Health and Environment.

Comply with all the relevant legislations, regulations and procedures in the

conduct of the operation.

Achieve zero lost time injury record by having a competent Safety, Health and

Environment Management Team and a self-motivated trained workforce.

Nourish Safety, Health and Environment as our highest core values in

organisational goal.

Review SHE management systems periodically or continuously in order to

achieve safe system of work and SHE best practices.

Establish systems and procedures to maintain the laboratory and pilot plant

facilities as scheduled and to implement safe system of work.

The SHE policy shall be subjected to periodical review to cater for likely variations in

the course of the operations and shall be made available to all interested parties.

“THINK SAFETY, ACT SAFELY, STAY HEALTHY”______________________________

11


Assoc. Prof. Zulkafli HassanDean of FKKSA

Dated: Nov 2009C2. General Laboratory Safety Procedures

DO

Know the potential hazards of the materials used in the laboratory. Review the Chemical Safety Data

Sheet (CSDS) and container label prior to using a chemical.

Know the location of safety equipment such as emergency showers, eyewashes, fire extinguishers, fire

alarms, spill kits and first aid kits.

Review emergency procedures to ensure that necessary supplies and equipment for spill response and

other accidents are available.

Practice 5S to minimize unsafe work conditions such as obstructed exits and safety equipment, cluttered

benches and hoods, and accumulated chemical waste.

Wear personal protective equipment when working with chemicals. This includes eye protection, lab

coat, gloves, and appropriate foot protection (no sandals). Gloves should be made of a material known to

be resistant to permeation by the chemical in use.

Wash skin promptly if contacted by any chemical, regardless of corrosivity or toxicity at least 15

minutes.

Label and store chemicals properly. All chemical containers should be labeled to identify the container

contents (no abbreviations or formulas) and hazard information. Chemicals should be stored by hazard

groups and chemical compatibilities.

Use fume hoods when processes or experiments may result in the release of toxic or flammable vapors,

fumes, or dusts.

DON’T

Eat, drink, chew gum, or apply cosmetics in areas where chemicals are used and stored.

Perform unauthorized experiment.

Store food in laboratory freezer or ovens.

Drink water from laboratory water sources.

Use laboratory glassware to prepare or consume food.

Smell or taste chemicals.

Pipette by mouth.

Leave potentially hazardous experiments or operations unattended without prior approval from

the lab instructor.

Use chipped, cracked or dirty glassware.

Work alone in the laboratory after office hour.12


Dispose chemical waste into sink drains.

Immerse hot glassware in cold water. The glassware may shatter.

Look into a container that is being heated.

13


C3. Chemical Safety Data Sheet (CSDS) for Ethylene Glycol

ETHYLENE GLYCOL

ICSC: 0270March 1999

1,2-Ethanediol1,2-Dihydroxyethane

CAS No: 107-21-1RTECS No: KW2975000EC No: 603-027-00-1

HOCH2CH2OHMolecular mass: 62.1

TYPES OFHAZARD /EXPOSURE

ACUTE HAZARDS / SYMPTOMS

PREVENTION FIRST AID / FIRE FIGHTING

FIRECombustible. NO open flames. Powder, alcohol-resistant foam,

water spray, carbon dioxide.

EXPLOSION

EXPOSURE PREVENT GENERATION OF

MISTS!

InhalationCough. Dizziness. Headache. Ventilation. Fresh air, rest. Artificial respiration

may be needed. Refer for medical attention.

SkinDry skin. Protective gloves. Remove contaminated clothes.

Rinse skin with plenty of water or shower.

Eyes

Redness. Pain. Safety goggles. First rinse with plenty of water for several minutes (remove contact lenses if easily possible), then take to a doctor.

Ingestion

Abdominal pain. Dullness. Nausea. Unconsciousness. Vomiting.

Do not eat, drink, or smoke during work.

Rinse mouth. Induce vomiting (ONLY IN CONSCIOUS PERSONS!). Refer for medical attention. If no medical personnel are available and the patient is conscious, ingestion of alcoholic beverage may prevent kidney failure.

SPILLAGE DISPOSAL PACKAGING & LABELLING

Collect leaking and spilled liquid in sealable containers as far as possible. Wash away remainder with plenty of water. Personal protection: filter respirator for organic gases and vapours.

Xn SymbolR: 22S: ()2

EMERGENCY RESPONSE SAFE STORAGE

NFPA Code: H1; F1; R0 Separated from strong oxidants, strong bases. Dry. Ventilation along the floor.

IMPORTANT DATA

Physical State; AppearanceODOURLESS, COLOURLESS VISCOUS HYGROSCOPIC LIQUID

Routes of exposureThe substance can be absorbed into the body by inhalation and through the skin.

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http://www.ilo.org/legacy/english/protection/safework/cis/products/icsc/dtasht/symbols/xn.htm

http://www.ilo.org/legacy/english/protection/safework/cis/products/icsc/dtasht/_icsc02/icsc0270.pdf

http://www.ilo.org/legacy/english/protection/safework/cis/products/icsc/dtasht/info1.htm


Chemical dangersOn combustion, forms toxic gases. Reacts with strong oxidants and strong bases.

Occupational exposure limitsTLV: 100 mg/m³ (Ceiling value); A4 (not classifiable as a human carcinogen); (ACGIH 2004).MAK: 10 ppm, 26 mg/m³; Peak limitation category: I(2); skin absorption (H); Pregnancy risk group: C; (DFG 2004).

Inhalation riskA harmful contamination of the air will be reached rather slowly on evaporation of this substance at 20°C.

Effects of short-term exposureThe substance irritates the eyes and the respiratory tract. The substance may cause effects on the kidneys and central nervous system, resulting in renal failure and brain injury. Exposure could cause lowering of consciousness.

Effects of long-term or repeated exposureThe substance may have effects on the central nervous system, resulting in abnormal eye movements (nystagmus).

PHYSICAL PROPERTIES ENVIRONMENTAL DATA

Boiling point: 198°CMelting point: -13°CRelative density (water = 1): 1.1Solubility in water: miscibleVapour pressure, Pa at 20°C: 7Relative vapour density (air = 1): 2.1Relative density of the vapour/air-mixture at 20°C (air = 1): 1.00Flash point: 111°C (c.c.)Auto-ignition temperature: 398°CExplosive limits, vol% in air: 3.2-15.3Octanol/water partition coefficient as log Pow: -1.93

NOTES

The occupational exposure limit value should not be exceeded during any part of the working exposure.Card has been partly updated in October 2005. See sections Occupational Exposure Limits, Emergency Response.

15


C4. Chemical Safety Data Sheet (CSDS) for Ethanol

ETHANOL

ICSC: 0044

Ethyl alcohol

CAS No: 64-17-5RTECS No: KQ6300000UN No: 1170EC No: 603-002-00-5

CH3CH2OH / C2H6OMolecular mass: 46.1

TYPES OFHAZARD /EXPOSURE

ACUTE HAZARDS / SYMPTOMS PREVENTION FIRST AID / FIRE FIGHTING

FIRE

Highly flammable. NO open flames, NO sparks, and NO smoking. NO contact with strong oxidants.

Powder, alcohol-resistant foam, water in large amounts, carbon dioxide.

EXPLOSION

Vapour/air mixtures are explosive. Closed system, ventilation, explosion-proof electrical equipment and lighting. Do NOT use compressed air for filling, discharging, or handling.

In case of fire: keep drums, etc., cool by spraying with water.

EXPOSURE

InhalationCough. Headache. Fatigue. Drowsiness.

Ventilation, local exhaust, or breathing protection.

Fresh air, rest.

SkinDry skin. Protective gloves. Remove contaminated clothes. Rinse and

then wash skin with water and soap.

EyesRedness. Pain. Burning. Safety goggles. First rinse with plenty of water for several

minutes (remove contact lenses if easily possible), then take to a doctor.

IngestionBurning sensation. Headache. Confusion. Dizziness. Unconsciousness.

Do not eat, drink, or smoke during work.

Rinse mouth. Refer for medical attention.

SPILLAGE DISPOSAL PACKAGING & LABELLING

Ventilation. Remove all ignition sources. Collect leaking and spilled liquid in sealable containers as far as possible. Wash away remainder with plenty of water.

F SymbolR: 11S: (2-)7-16UN Hazard Class: 3UN Pack Group: II

SAFE STORAGE

Fireproof. Separated from strong oxidants.

IMPORTANT DATA

Physical State; AppearanceCOLOURLESS LIQUID, WITH CHARACTERISTIC ODOUR.

Physical dangers

Routes of exposureThe substance can be absorbed into the body by inhalation of its vapour and by ingestion.

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The vapour mixes well with air, explosive mixtures are easily formed.

Chemical dangersReacts slowly with calcium hypochlorite, silver oxide and ammonia, causing fire and explosion hazard. Reacts violently with strong oxidants such as nitric acid, silver nitrate, mercuric nitrate or magnesium perchlorate, causing fire and explosion hazard.

Occupational exposure limitsTLV: 1000 ppm as TWA; A4 (not classifiable as a human carcinogen); (ACGIH 2004).MAK: 500 ppm, 960 mg/m³; Peak limitation category: II(2); Carcinogen category: 5; Pregnancy risk group: C; Germ cell mutagen group: 5; (DFG 2004).

Inhalation riskA harmful contamination of the air will be reached rather slowly on evaporation of this substance at 20°C.

Effects of short-term exposureThe substance irritates the eyes. Inhalation of high concentration of vapour may cause irritation of the eyes and respiratory tract. The substance may cause effects on the central nervous system.

Effects of long-term or repeated exposureThe liquid defats the skin. The substance may have effects on the upper respiratory tract and central nervous system, resulting in irritation, headache, fatigue and lack of concentration. See Notes.

PHYSICAL PROPERTIES

Boiling point: 79°CMelting point: -117°CRelative density (water = 1): 0.8Solubility in water: miscibleVapour pressure, kPa at 20°C: 5.8Relative vapour density (air = 1): 1.6

Relative density of the vapour/air-mixture at 20°C (air = 1): 1.03Flash point: 13°C c.c.Auto-ignition temperature: 363°CExplosive limits, vol% in air: 3.3-19Octanol/water partition coefficient as log Pow: -0.32

NOTES

Ethanol consumption during pregnancy may adversely affect the unborn child.Chronic ingestion of ethanol may cause liver cirrhosis.The flash point of 50% water solution is 24°C.Card has been partly updated in April 2005. See section Occupational Exposure Limits.

17


C5. Emergency Notification & Response

18


19


20


21


22


EXPERIMENT 1: TRAY DRYER UNIT

OBJECTIVE

1. To determine effect of heating level on the drying rate

2. To calculate water loss through the relationship of relative humidity and enthalpy.

INTRODUCTION

Drying is usually the final step in a series of operations, and the product from a dryer is

often ready for final packaging. Water or other liquids may be removed from solids mechanically

by presses or centrifuges or thermally by vaporization. Drying can be defined by reducing the

moisture content from an initial value to some acceptable final value. Most industrial dryers handle

particulate solid during part of or all the drying cycle, although some, of course, dry large individual

pieces such as ceramic ware or sheet of polymer. The solid to be dried may be in many different

forms, such as flakes, granules, crystals, powders, slab or continuous sheets, and may have widely

differing properties. The liquid to be vaporized may be on the surface of the solid, as in drying salt

crystal ; it may be entirely inside the solid , as in solvent removal from a sheet of polymer; or it may

be partly outside and partly inside.

EQUIPMENT/APPARATUS/MATERIAL

1. Tray Drier Unit

2. Rice

3. Air velocity measurement device

4. Analytical Balance

EXPERIMENTAL PROCEDURES

1. Remove drying plates from support frame.

2. Tare scale to zero.

3. Insert drying plates individually into support frame, read off and note the weight of the

individual drying plates on the digital scale.

4. Spread material (rice) to be dried in a thin layer on the drying plates.

5. Insert drying plates in support frame and note total weight.

6. Switch on fan and set the speed.

7. Measure flow speed with manual anemometer and note it.

8. Set heating level to 2 (1000 Watt) and switch on heater.

9. Start drying experiment, commence time measurement using stopwatch. Collect the data for 5

minutes intervals and drying experiment is complete when either (whichever come first):

23


The total mass m of the material to be dried is no longer falling

The collected data are constant

10. Repeat step 1 to 9 for next 2 different heating level (1 (500 Watt) - 6 (3000 Watt)).

11. Shutdown the equipment.

12. While performing the experiment, the following measured data is recorded at regular intervals

and entered in the working sheet.

Air temperature, T1 before material to be dried

Relative air humidity, F1 before material to be dried

Air temperature, T2 after material to be dried

Relative air humidity, F2 after material to be dried

Total mass, m of material to be dried and drying plates

Use the attached Mollier diagram to determine the loading X for the relevant air states

RESULTS

Table Experimental Data 1

Heating Level :

Air Speed :

Time,t

min

Air Temp.,

T1

Air Humidity,

F1

Air Temp.,

T2

Air Humidity,

F1

Mass, m

0

5

10


Heating Level :

Air Speed :

Time,t

min

Air Temp.,

T1

Air Humidity,

F1

Air Temp.,

T2

Air Humidity,

F1

Mass, m

0

5

10

24


GUIDE FOR DISCUSSION

1. Plot the mass of material to be dried versus drying time. Explain the plotted graph.

2. Find the X value and complete the table.


Time,

t

min

Air

Temp.,

T1

Air

Humidity,

F1

X

Air

Temp.,

T2

Air

Humidity,

F1

X

Mass, m

0

5

10


Time,

t

min

Air

Temp.,

T1

Air

Humidity,

F1

X

Air

Temp.,

T2

Air

Humidity,

F1

X

Mass, m

0

5

10

3. List 5 types of dryer which commonly used in industrial.

25


26


Psychrometric Chart and Air Characteristics

Figure 1: Psychrometric Chart


EXPERIMENT 2: CLIMBING FILM EVAPORATOR UNIT

OBJECTIVE

1. To analyze the influence of steam pressure and column pressure to the evaporation process

at a constant inlet flow rate.

2. To explain the effect of evaporation process on product characteristics in terms of

composition, viscosity and heat-transfer coefficients.

INTRODUCTION

The objective of evaporation is to concentrate a solution consisting of a nonvolatile solute

and a volatile solvent. Evaporation is conducted by vaporizing a portion of the solvent to produce a

concentrated solution of thick liquor. Normally, in evaporation, the thick liquor is the valuable

product and the vapor is condensed and discarded. Most evaporators are heated by steam

condensing on metal tubes. When a single evaporator is used, the vapor from the boiling liquid is

condensed and discarded. This method is so- called single-effect evaporation.


1. CTS4 Climbing Film Evaporator

2. Steam supply

3. Vacuum pump

4. Stop watch

5. Digital balance

6. Beakers

7. Glass rod

8. Portable conductivity meter

9. Water supply


1. Prepare standard salt solution and get its conductivity by using conductivity meter.

2. Prepare 20L salt solution with concentration 25g/L and feed in the feed vessel.

3. Start the vacuum operation so that the liquid from the feed vessel can be sucked into the

vessel column.

4. Flow the cooling water to cool down the steam in the condenser.

5. Set the feed flow rate FI 1 at 0.3 L/min and vacuum pressure at 0.4 bar.

6. Set the steam pressure at 0.5 bar.

7. Record the temperature change at the top and bottom of evaporator column for every 5

minutes until 30 minutes. Then, stop the operation by closing the vacuum valve and steam

pressure valve.

8. Repeat steps 6 to 7 for steam pressure 1 bar(g).


RESULT

Experimental Data

Steam

Pressure

(Bar)

Time

(s)

T1

(0C)

T2

(0C)

Volume

(mL)

Conductivity

(mS)

V3 V5 V3 V5

0.5

0

5

10

15

20

25

30

1.0

0

5

10

15

20

25

30


1. Give two reasons why we must operate the column pressure under 1 atm or at vacuum condition.

2. For standard solution, plot a graph for conductivity versus concentration of salt solution and give

your explanation of the relationship between concentration and conductivity.

3. Plot three graphs for different steam pressure where the time versus concentration of salt solution

taken from valve, V3.

4. Explain the effect of steam pressure and column pressure (fixed) of constant inlet feed flow to

the evaporation rate.

5. Compare the salt solution concentration taken from valve V3 and valve V5, and give the

relationship between composition, viscosity and heat-transfer coefficients.

6. Give all safety precautions that need to be taken before, during, and after running this

experiment.

Chemical Engineering Laboratory II BKF3751

EXPERIMENT 3: ABSORPTION COLUMN UNIT

OBJECTIVE

1. To determine the effect of air flow rate and water flow rate on flooding point in an absorption

column.

2. To explain the relationship between water and air flow rate changes and their effect on

pressure drop, P of an absorption column.

INTRODUCTION

Absorption column is one of the separation techniques that involve liquid and vapor. One or

more component of a gas mixture can be separated when a certain liquid flow through it counter-

currently. The liquid absorbs the component(s) and mass transfer process which separates the

component(s) from gas mixture occurs. Packed material is used to increase the contact surface area

in absorption process which enhances the efficiency and shortens the duration of the process.


1. Packed Absorption Column

2. Air Compressor

3. Water and Air

4. Stop watch


1. Check and make sure the valves for right column for sadle pack are opened.

2. Set the water flow rate at 2.5 L/min.

3. Set the air flow rate at 100 L/min. Start the stop watch and leave it for 5 minutes. Make sure the

water and air flow rate are always constant.

4. After 5 minutes, take the data for pressure drop, P from Digital P Meter.

5. Repeat Steps 3 and 4 by increasing air flow rate by 10 L/min until the flooding point is

observed.

6. When the flooding point is achieve, read the P from Digital P Meter and reduce the air flow

rate back at 100 L/min

7. Repeat Step(s) 3 to 7 for water flow rate at 3.0 L/min respectively.


8. Then, maintain the air flow rate at 50 L/min and, read the pressure drop every 2 minutes at

different water flow rates range from 2.0 to 3.5 L/min with an increment by 0.5 L/min

RESULT

Table 1

Water flow rate, W

(L/min)

Air flow rate, G

(L/min)

Pressure Drop, P

(cm H2O)

Time

(every 5 minutes)

2.5

3.0

Table 2

Air flow rate, G

(L/min)

Water flow rate, W

(L/min)

Pressure Drop , P

(cm H2O)

Time

(every 2 minutes)

50

2.0

2.5

3.0

3.5


1. Plot a graph log P versus log air flow rate for each water flow rate (refer table 1). Find the

relationship between P and air flow rate.

2. Plot graph log P versus log water flow rate for fixed air flow rate (refer table 2). Find the

relationship between P and water flow rate.

3. Describe the following terms:

4. “Flooding point”, “flooding velocity”, and “loading point”.

5. Discuss your data and results obtained from the experiment.

6. List down 5 application of this process that is used in petrochemical industries?

7. Explain roughly one of the applications that are listed above?



EXPERIMENT 4: THIN FILM EVAPORATOR UNIT

OBJECTIVE

1. To demonstrate the separation of ethanol from water using the thin film evaporative

process

2. To determine effect of heating temperature and vacuum pressure on the separation

efficiency.

INTRODUCTION

The thin film evaporation unit is a complete evaporation system including feed input,

heating and vacuum generation for continuous plant operation. The unit is designed to evaporate

materials in the pressure range of atmospheric down to 8 mbar. The lower the pressure, the lower

the temperature required to effect evaporation, thus lowering the chances of damaging the product.

The thin film evaporator adopts a rotating film system, where molecules are continuously

evaporating from a film which is spread by a rotating wiper.


1. BP215 Thin Film Evaporator

2. Stop watch

3. Beakers

4. Refractometer

5. Cooling Water Supply

6. Ethanol

7. Measuring Cylinder

8. Water


1. Prepare a set of mixtures containing ethanol and water within a specified range of composition

between pure water and pure ethanol. Determine refractive index (RI) for each mixture using a

refractometer.

2. Prepare 15L of ethanol-water mixture at a composition at composition 20:80 v/v. Obtain a

sample from the feed liquid at valve V2 and analyze the sample to determine its actual initial

composition.

3. Perform the general start-up procedures with the following default settings:

metering pump P1 : 60% stroke, 60 stroke/min

heating thermostat T1: 100°C

vacuum controller PIC-1 : 400 mbar

4. Allow the unit to run for about 5-10 minutes to achieve steady state. Steady state is reached

when the distillate temperature doesn’t change significantly over time.


5. Record the distillate temperature.

6. Measure the distillate and bottom product flow rates.

7. Collect the product from both distillate and bottom product vessels B2 and B3. Analyze the

collected liquid to determine its compositions

8. Repeat the experiment by reducing the vacuum pressure down (Range 400 – 200 mbar).

9. Return the vacuum pressure to default. Repeat the experiment by increasing the heating

thermostat up (Range 100 – 120 oC).

RESULT

Initial Feed Composition :

P1 : 60% stroke, 60 stroke/min

N

o.

Heating

Temp.oC

Vacuum

Pressure

mbar

Distillate Bottom Product

TempoC

Flowrate

mL/min

RI Composit

ion

Flowrate

mL/min

RI Composi

tion

1 100 400

2 100

3 100

4 400

5 400

6 400


1. Plot the calibration curve of RI vs ethanol composition.

2. Plot a graph of distillate temperature, bottom and top composition and percentage feed

vaporized vs. vacuum pressure and heating thermostat temperature.

3. Compare between the distillate temperature, bottom and top composition and percentage feed

vaporized at different heating thermostat temperature and vacuum pressure.

4. Calculate the separation efficiency at different operating conditions

5. Compare the separation efficiencies between different operating conditions to determine the

effect of temperature and pressure.



FEED RATE SETTING DIAGRAM FOR FEED PUMP


EXPERIMENT 5: ROTARY EVAPORATOR UNIT

OBJECTIVE

1. To provide hands on experience and enhance the understanding on the principles of the

binary (ethanol-water mixture) separation process using rotary evaporator.

INTRODUCTION

A rotary evaporator or rotavap, is a device used in chemical and biochemical laboratories for

the efficient and gentle evaporation of solvents. The main components of a rotary evaporator are a

vacuum system, consisting of a vacuum pump and a controller, a rotating evaporation flask which

can be heated in a heated fluid bath, and a condenser with a condensate collecting flask. The system

works because lowering the pressure lowers the boiling point of liquids, including that of the

solvent. This allows the solvent to be removed without excessive heating.

Evaporation under vacuum can be performed in a standard distillation rig. However, the

rotary evaporator has a key advantage. As the evaporating flask rotates, the liquids are forced to the

outside of the flask with the centrifugal motion. This creates a larger surface area of the liquids and

hence allows for quick, gentle evaporation.

Rotary evaporators are highly effective at removing the majority of organic solvents during

the extraction process. The remainders of the solvents are usually removed using a high-vacuum

line.


1. Rotadest R50 Rotary Evaporator

2. Stop watch

3. Beakers

4. Refractometer

5. Cooling Water Supply

6. Ethanol

7. Measuring Cylinder

8. Water


1. Prepare a set of mixtures containing ethanol and water within a specified range of composition

between pure water and pure ethanol. Determine refractive index (RI) for each mixture using a

refractometer.

2. Prepare 5L of ethanol-water mixture at a composition 20:80 v/v.

3. Perform the general start-up procedures with the following default settings:

http://en.wikipedia.org/wiki/Distillation

http://en.wikipedia.org/wiki/Boiling_point

http://en.wikipedia.org/wiki/Condenser

http://en.wikipedia.org/wiki/Pump

http://en.wikipedia.org/wiki/Vacuum

http://en.wikipedia.org/wiki/Solvent

http://en.wikipedia.org/wiki/Evaporation

http://en.wikipedia.org/wiki/Biochemical

http://en.wikipedia.org/wiki/Chemical


a. Bath temperature T1C-1 : 80°C

b. Rotation speed SI-1 : 25 rpm

c. Vacuum controller PIC-1 : 350 mbar

4. Open valve V5 to collect the distillate in receiving vessel B2

5. Once all temperature readings are constant, close valve V3 and open valve V4. Observe the

flow of distillate from condenser W2 through liquid cooler W3 into receiving vessel B2

6. Start the timer once liquid starts to enter vessel B2.

7. Record the distillate temperature every 5 minutes.

8. After 5 minutes, collect the product from receiving vessel B2 and measure its volume. Analyses

the collected liquid to determine its composition using refractometer.

9. Combined all the collected distillate in a container and at the end of the experiment, measure its

overall volume and composition.

10. Repeat the previous step by switching back and forth between both receiving vessels B2 and B3

every 5 minutes until they are no more flow of distillate observed in the unit.

11. Stop the experiment and switch off vacuum pump P1, heating bath W1 and rotary sphere drive

M1. Lower the heating bath by opening the pressure release valve below the hydraulic jack.

12. Wait for the concentrate in rotary sphere B1 to cool down before collection. Determine the

volume and composition of the concentrate.

RESULT

Initial Feed Composition :

TimeMinut

e

Distillate Temperature

oC

Distillate Volume

mL

RI Distillate Compositio

nVol %

Distillate Flow RatemL/min

Volume of Ethanol in Distillate

mL5

10

Volume and Composition of Concentrate:


1. Plot the calibration curve of RI Vs ethanol composition

2. Plot a graph of distillate temperature, composition, flowrate vs. time. Discuss the findings


3. Calculate the overall separation efficiency of rotary evaporator.

Efficiency = Total amount of ethanol in distillate X 100% Initial amount of ethanol in rotary flask

Chemical Engineering Laboratory III BKF3781

EXPERIMENT 6: SIEVE TRAY DISTILLATION

(Batch Distillation At Total Reflux)

OBJECTIVE

1. To determine the height equivalent theoretical plates (HETP) at total reflux.

2. To determine the effect of liquid and vapor loading on the HETP at total reflux.

INTRODUCTION

The principle for sieve tray distillation is the same as for normal distillation: when a liquid mixture

is heat so that it boils, the composition of the vapor above the liquid differs from the liquid

composition. If this vapor is then separated and condensed into a liquid, it becomes richer in the

lower boiling component(s) of the original mixture. This is what happens in a sieve tray distillation

column. A mixture is heated up, and routed into the distillation column. On entering the column, the

feed starts flowing down but part of it, richer in lower boiling component(s), vaporizes and rises.

However, as it rises, it cools and while part of it continues up as vapor, some of it (enriched in the

less volatile component) begins to descend again.

Figure 1: Chemical engineering schematic of Sieve tray Binary Fractional Distillation tower. A binary distillation separates a feed mixture stream into two fractions: one distillate and one bottom

fractions.

Figure 1: shows a simple continous fractional distillation tower for separating a feed stream into

two fractions, an overhead distillate product and a bottoms product. The “lightest” products (those

with the lowest boiling point or highest volatility) exit from the top of the columns and the

“heaviest” products (the bottoms, those with the highest boiling point) exit from the bottom of the


column. The overhead stream may be cooled and condensed using a water-cooled or air-cooled

condenser. The bottoms reboiler may be a stream-heated or hot oil-heated heat exchanger, or even a

gas or oil-fired furnace. In a continous distillation, the system is kept in a steady state or

approximate steady state. Steady state means that quantities related to the process do not change as

time passes during operation. Such constant quantities include feed input rate, output stream rates,

heat and cooling rates, reflux ratio, and temperatures, pressures, and compositions at every point

(location). Unless the process is disturbed due to changes in feed, heating, ambient temperature, or

condensing, steady state is normally maintained. This is also the main attraction of sieve tray

distillation, apart from the minimum amount of (easily instrumentable) surveillance; if the feed rate

and feed composition are kept constant, product rate and quality are also constant. Even when a

variation in conditions occurs, modern process control methods are commonly able to gradually

return the sieve tray process to another steady state again.


1. Sieve Tray Distillation Unit

2. Refractometer

3. 5L of binary mixture (ethanol-

water).

4. Beakers.


1. Ensure all valves are closed.

2. Prepare a mixture of ethanol and water at desired composition (for instance 5 L mixture

containing 2 L of ethanol and 3L of filtered water).

3. Record initial volume and refractive index of the liquid mixture.

4. Open the charge port cap and charge the reboiler B1 with the ethanol-water mixture. Close the

charge port cap.

5. Make sure all the valve are properly close except V4, V5, V11, V12 and V14.

5. Turn on the main power on the control panel.

6. Open the main cooling water valve V11. Let the cooling water flow into the condenser (W2).

7. Switch on the cartridge heaters W1a & W1b and set the heater power controller to 1.0 kW and

allow the reboiler temperature reach approximate 85oC.

8. Ensure the reflux control is 0 position. (total reflux)

9. As the top column temperature sensor TT 112, reach steady state, record the temperature.


10. Set the reflux control to position 1 (Total distillate offtake). Open valve V9 and collect 10 ml

sample distillate using conical flask. Close valve V9 and set the reflux control to position 0. ( Total

reflux).

11. To collect bottom product sample, adjust the overflow U-tube to a suitable level to let the

product overflow into the product tank, B5 after passing through the product cooler, W3. Open

valve V3 and collect 10 ml of sample bottom product using conical flask.Close valve V3.

12. Measure the refractive index of the samples and record the value into data table.

13. Measure the distillate flow rate as follows:

a) Set the reflux control to position 0 (Total reflux)

b) When the distillate start flowing into the phase separator, start the timer.

c) As distillate reach 200 ml on the measure tank (overflow), stop the timer.

d) Determine the flow rate of the distillate.

14. For different liquid and vapor loading, adjust the heater power settings in W1a and W1b

according table below:

Heater Power(kW)1.001.502.00

15. Wait for approximately 15 to 30 minutes and allow the distillation unit to achieve new steady

state. Repeat steps 9 to 13.

16. Switch off heater power and allow the system to cool down to ambient temperature.

RESULT

Heater W1, W2 Power (kW)

Distillation Bottom Product HETP (mm)Temp (oC) RI Mole

FractionTemp (oC) RI Mole

Fraction

1.001.502.00



1. Using the X-Y equilibrium diagram for ethanol-water system, mark the top and bottom

compositions on the diagram and determine the theoretical number of plates in the distillation

unit using the McCabe-Thiele method. Refer to Appendix D.1 for a step-by-step guide.

2. Calculate the height equivalent theoretical plates (HETP) by dividing the effective column height

with the number of theoretical plates.

3. Plot a graph of HETP vs. Heating Power and observe the relationship.

REFERENCE:

Christie J. Geankoplis, Transport Process and Unit Operations, 3rd Edition.

Figure 2: Process Flow Diagram for sieve tray unit

Calibration Curve for Ethanol in Water


EXPERIMENT 7: SHORT PATH DISTILATION

OBJECTIVE

1. To investigate the effects of stirrer speed and evaporator temperature on the efficiency of

separation.

INTRODUCTION

This Short Path Distillation is a thermal separation process for thermal sensitive products.

Short residence time and low evaporation temperature will cause a minimum thermal stress to the

distilled product. Typical applications are high molecular organic compounds particularly from the

field of chemistry, pharmaceutical and food industry. Distillation is one of the most important

thermal separation methods.

Short path distillation is a continuous separation process working under vacuum conditions.

Evaporation takes place from a heated wiped film. Caused by the pressure drop between the place

of evaporation and the vacuum system the operating pressure in typical wiped film evaporators with

external condenser is limited to some millibars.

The considerably lower pressure in the short path evaporator is obtained by the short

distance for the vapours on their way from the evaporator surface to the condenser. In addition,

the cross section area of flow is equal to the evaporator surface, so that there is only a minor

pressure drop between evaporator and condenser


1. Mix the ethylene glycol and water with a ratio of 7:3 at total of 1 litre in a beaker. Then stir the

mixture homogeneously.

2. Check that all valves are initially closed except the valves HV02, HV04, HV05, HV11 and

HV12. Ensure that the cold trap is filled with dry ice.

3. Remove valve HV-01 and fill the feeding funnel V-100 with the homogeneous mixture.

4. Switch ON the main power supply at the control panel.

5. ON computer or the software program.

6. Set the thermostat at 70°C, Chiller at 12°C and vacuum pump pressure at 100mbar. Manually

maintain the pressure throughout the experiment. [To adjust vacuum pump pressure, manually

adjust valve, V14. To adjust the desired flow rate, adjust the opening valve HV03. To adjust the

desired stirrer speed, adjust it from the software].

7. Open valve HV-13 to allow for some of the hot bath to circulate through the heating jacket of

the feeding funnel to pre-heat the feed in the funnel.

NOTE: Valve HV13 must be close before switching off the thermostat, B-400.

8. Once the chiller temperature and thermostat temperature have reach the set points, the

equipment is ready for experiment

9. For every set of experiment, run for 10 minutes. After 10 mins, records down the volume of

distillate from V-104 and volume of concentrate from V-105-107.

10. Repeat the experiment with different operating parameters as shown in the table in result and

discussion.

11. Follow the operating procedure to shut down the equipment. DO NOT let the wiper roller to

run without the flow of feed.

SAMPLING PROCEDURE

1. For every batch of experiment, to ensure the feed flowrates are the same, HV03 should not be

close at each sampling. To do this, switch off the vacuum pump, open HV07, HV08 and HV09

to let the condensate and distillate to flow into V-104 to V-107 respectively.

2. After all the liquid are flows into each vessel. Close back HV07, HV08 and HV09. Continue to

run the next experiment by switching on the vacuum pump again.

3. The collected distillate and condensate can then be used for futher testing.

4. The feed flowrate is calculated by dividing the total volume of sample collected to the total

time taken.

GENERAL SHUT-DOWN PROCEDURES

1. Switch off vacuum pump.

2. Close valve HV03 to stop feeding.

3. Switch off stirrer motor.

4. Turn off thermostat. Close HV13.

5. Open valve HV 01, HV 06 and HV 07.

6. After 15 minutes, switch off chiller and turn off the main power.

NOTE: DO NOT attempt to remove any vessel while the vacuum pump is running.

RESULT

1. Effect of stirrer speed

Vacuum pressure, PT-200 100mbarEvaporator Temperature, TT-100 70°C

Feed Flow rate ml/minContact time 10 min

EG-water ratio 7:3

Time Start Stirrer Speed(rpm)Distillate

Volume (ml)ConcentrateVolume (ml)

Separation Efficiency (%)

50

100

200

220

2. Effect of evaporator temperature

Feed flow rate ml/min

Stirrer speed, M-500 220rpm

Vacuum pressure 100mbar

Contact time 10min

EG-water ratio 7:3

Time Start Temp (°C)Distillate

Volume (ml)ConcentrateVolume (ml)

Separation Efficiency (%)

70

72

74

76


1. Based on the experimental results, comment on the effects of the parameters on the thermal

separation efficiency.

2. For every set of experiment:

a) Plot a graph of stirrer speed vs. separation efficiency.

b) Plot a graph of evaporator temperature vs. separation efficiency.

Discuss about each of plotted graph.

FORMULAS

1. Molarity = Mole / Liter

= (Specific Gravity x Purity x 1000mg/L) / Molecular Weight

2. Mole = Mass / Molecular Weight

3. M1V1 = M2V2 M1,M2 = Molarity; V1,V2 = Volume

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DKK3761