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

Engineering Lab IV Vision

DKK3761

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: PEO 2: Our graduates will demonstrate effective communications, leadership and teaming skills 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: PEO 4: Our graduates will demonstrate the foundation and depth for successful chemical engineering careers in industry, academia, or government 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 PO2 PO3 PO4 Ability to acquire and apply knowledge of science and engineering fundamentals. Acquired sufficient technical competence in chemical engineering and related disciplines. Ability to assist and solve chemical engineering and related problems under supervision. 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.

Engineering Lab IV CONTENTS

DKK3761

PAGE A. B. Teaching Plan Laboratory Report Format & Evaluation B1. Laboratory Report Format B2. Report Evaluation B3. Laboratory Front page C. Occupational Safety & Health (OSH) 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 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 23 11 4 5

Engineering Lab IV A. TEACHING PLAN

DKK3761

Engineering Lab IV 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%

DKK3761

(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)

Engineering Lab IV

DKK3761 Report Evaluation For Part A

Instruction: Please assess each item using the given scales. Fractional marks will be given for each category. Item Assessed Organization and Format Unacceptable (1) Not follow FKKSA laboratory report format. Not well organized. Contents show lack of knowledge. Acceptable (2) Partially follow FKKSA laboratory report format. Contents show enough of knowledge but still a few concept and ideas are loosely connected. Good (3) Follow FKKSA laboratory report format of writing; all needed sections present. Well organized. Contents show enough knowledge of subject. Very Good (4) Follow FKKSA laboratory format of writing; all needed sections present. Well organized and easily followed. Contents show full knowledge of subject. Excellent (5) 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. 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. Score

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.

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

Engineering Lab IV
Item Assessed Unacceptable (1) Very little background information or information is incorrect OR, does not give any information about what to expect in the laboratory report Acceptable (2) Some introductory information, but still missing some major points. OR, gives little information Good (3) Introduction is nearly complete, missing some minor points.

DKK3761
Very Good (4) Introduction is complete and well written but theory may not be backed up to concise lead-in to the laboratory experiment. Excellent (5) 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. Score

Introduction

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

Engineering Lab IV
Item Assessed Methodology Unacceptable (1) 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. Acceptable (2) 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. Good (3) 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.

DKK3761
Very Good (4) Materials and methodology are complete. Mostly easy to follow. Description of procedure can be replicated. Excellent (5) Materials and methodology are complete and adequately detailed. Logical and easily followed. Description of procedure is complete, ensuring that it can be replicated. Score

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 experiments 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 experiments 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 experiments improvement.

Keywords: Experiment Summary, Recommendation

Engineering Lab IV
Item Assessed Unacceptable (1) Acceptable (2) Good (3)

DKK3761
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. Appendices available in laboratory report but poorly constructed

All citations in text are available in list of reference and list of reference is more than 3. Appendices available in laboratory report in structured manners

All citations in text are available in list of reference. List of reference is more than 3 and variety source. Appendices available in laboratory report in structured manners, clearly and precise Minimal to no spelling mistakes. Spell checked and proofed throughout. Good sentence and paragraph structure and transitions.

Keywords: Book Reference, Journal Reference, Website Reference Appendices Appendices not available in laboratory report. Only a few appendices available in laboratory report.

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.

Keywords: Language Timeliness Laboratory report handed in more than one week late Keywords: Punctuality Total Assessment Marks (55%) Up to one week late Up to three days late Handed in one day late Laboratory report handed in on time

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 : Instructors Name Group of Member Name 1. 2. 3. 4. 5. Group No. Section Marks Part A Part B TOTAL : : : 55 45 100 : : ID

FACULTY OF CHEMICAL AND NATURAL RESOURCES ENGINEERING 10

Engineering Laboratory IV DKK3761 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

Engineering Laboratory IV DKK3761

______________________________
Assoc. Prof. Zulkafli Hassan Dean of FKKSA Dated: Nov 2009

C2.

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.

DONT
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.

12

Engineering Laboratory IV DKK3761 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. 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

Engineering Laboratory IV DKK3761 C3. Chemical Safety Data Sheet (CSDS) for Ethylene Glycol

ETHYLENE GLYCOL ICSC: 0270

March 1999

1,2-Ethanediol 1,2-Dihydroxyethane CAS No: 107-21-1 RTECS No: KW2975000 EC No: 603-027-00-1 TYPES OF HAZARD / EXPOSURE FIRE EXPLOSION EXPOSURE Cough. Dizziness. Headache. Inhalation Dry skin. Skin Redness. Pain. Eyes Safety goggles. Protective gloves. PREVENT GENERATION OF MISTS! Ventilation. Fresh air, rest. Artificial respiration may be needed. Refer for medical attention. Remove contaminated clothes. Rinse skin with plenty of water or shower. First rinse with plenty of water for several minutes (remove contact lenses if easily possible), then take to a doctor. 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. PACKAGING & LABELLING HOCH2CH2OH Molecular mass: 62.1

ACUTE HAZARDS / SYMPTOMS Combustible.

PREVENTION NO open flames.

FIRST AID / FIRE FIGHTING Powder, alcohol-resistant foam, water spray, carbon dioxide.

Abdominal pain. Dullness. Nausea. Unconsciousness. Vomiting. Ingestion

Do not eat, drink, or smoke during work.

SPILLAGE DISPOSAL Collect leaking and spilled liquid in sealable containers as far as Xn Symbol possible. Wash away remainder with plenty of water. Personal R: 22 protection: filter respirator for organic gases and vapours. S: ()2 EMERGENCY RESPONSE NFPA Code: H1; F1; R0

SAFE STORAGE Separated from strong oxidants, strong bases. Dry. Ventilation along the floor. IMPORTANT DATA

Physical State; Appearance ODOURLESS, COLOURLESS VISCOUS HYGROSCOPIC LIQUID Chemical dangers On combustion, forms toxic gases. Reacts with strong

Routes of exposure The substance can be absorbed into the body by inhalation and through the skin. Inhalation risk A harmful contamination of the air will be reached rather

14

Engineering Laboratory IV DKK3761

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

slowly on evaporation of this substance at 20C. Effects of short-term exposure The 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 exposure The substance may have effects on the central nervous system, resulting in abnormal eye movements (nystagmus).

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

ENVIRONMENTAL DATA

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

Engineering Laboratory IV DKK3761 C4. Chemical Safety Data Sheet (CSDS) for Ethanol

ETHANOL ICSC: 0044

Ethyl alcohol CAS No: 64-17-5 RTECS No: KQ6300000 UN No: 1170 EC No: 603-002-00-5 TYPES OF HAZARD / EXPOSURE CH3CH2OH / C2H6O Molecular mass: 46.1

ACUTE HAZARDS / SYMPTOMS Highly flammable.

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

FIRST AID / FIRE FIGHTING Powder, alcohol-resistant foam, water in large amounts, carbon dioxide.

FIRE

Vapour/air mixtures are explosive. EXPLOSION

Closed system, In case of fire: keep drums, etc., cool by ventilation, explosionspraying with water. proof electrical equipment and lighting. Do NOT use compressed air for filling, discharging, or handling.

EXPOSURE Inhalation Cough. Headache. Fatigue. Drowsiness. Dry skin. Redness. Pain. Burning. Eyes Burning sensation. Headache. Confusion. Dizziness. Unconsciousness. SPILLAGE DISPOSAL Ventilation. Remove all ignition sources. Collect leaking and spilled liquid in sealable containers as far as possible. Wash away remainder with plenty of water. Do not eat, drink, or smoke during work. Ventilation, local exhaust, or breathing protection. Protective gloves. Safety goggles. Fresh air, rest.

Skin

Remove contaminated clothes. Rinse and then wash skin with water and soap. First rinse with plenty of water for several minutes (remove contact lenses if easily possible), then take to a doctor. Rinse mouth. Refer for medical attention.

Ingestion

PACKAGING & LABELLING F Symbol R: 11 S: (2-)7-16 UN Hazard Class: 3 UN Pack Group: II

SAFE STORAGE Fireproof. Separated from strong oxidants. IMPORTANT DATA Physical State; Appearance COLOURLESS LIQUID, WITH CHARACTERISTIC ODOUR. Physical dangers The vapour mixes well with air, explosive mixtures are easily Routes of exposure The substance can be absorbed into the body by inhalation of its vapour and by ingestion. Inhalation risk

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Engineering Laboratory IV DKK3761

formed. Chemical dangers Reacts 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 limits TLV: 1000 ppm as TWA; A4 (not classifiable as a human carcinogen); (ACGIH 2004). MAK: 500 ppm, 960 mg/m; Peak limitation category: II(2); Carcinogen category: 5; Pregnancy risk group: C; Germ cell mutagen group: 5; (DFG 2004).

A harmful contamination of the air will be reached rather slowly on evaporation of this substance at 20C. Effects of short-term exposure The 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 exposure The 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: 79C Melting point: -117C Relative density (water = 1): 0.8 Solubility in water: miscible Vapour pressure, kPa at 20C: 5.8 Relative vapour density (air = 1): 1.6 Relative density of the vapour/air-mixture at 20C (air = 1): 1.03 Flash point: 13C c.c. Auto-ignition temperature: 363C Explosive limits, vol% in air: 3.3-19 Octanol/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 24C. Card has been partly updated in April 2005. See section Occupational Exposure Limits.

17

Engineering Laboratory IV DKK3761 C5. Emergency Notification & Response

UNI V E R SI T I M A L AY SI A P AH AN G
F A C U L T Y O F C H E M IC A L N A T U R A L R E S O U R C E S & E N G IN E E R IN G C H E M I C A L S P I L L A G E N O T I F I C A T I O& R E S P O N S E N
BY WHOM PROCESS FLOW INFORMATION

START

W IT NESS

FOU N D C H EM IC AL SPILLAGE

W IT NESS

ALER T PER SONN EL IN ADJ AC EN T AR EA & EVACU AT E N ON ESSEN T IAL PERSON FR OM SPILL AR EA Poin t T o R emember : 1. Pleas e do not handle spillage unless you w ear a com plete Personal Protective Equipm ent (PPE). 2. If flam m able vapors are involved , do not operate electrical s witc hes unless to turn off elec tric equipment . 3. If spilled m aterial is flam m able , ex tinguish flam es and all other sources of ignition .

W IT NESS

NO

TR AIN ED FOR H AN DLE SPILLAGE

YES F IND SAFE LOCATION ENVIRONM EN T

W IT NESS

SPILL ON

PEOPLE W IT NESS REFER T O C SD S F OR ACT ION (AC C ID EN TAL R ELEASE M EASU R ES PART ) R EFER T O C SD S F OR AC TION (FIRST AID M EASUR ES PAR T ) SHE Co ntact N:o 09-549 2430 / 2387 / 2419 / 2640 IN FORM SH E U NIT / FIR ST AID ER F irst Aid er Co ntact N o : En. Anuar : 013- 6986946 En. H isham : 012- 3058524 Pn. H afiz ah : 012- 9848565 IF EM ERGENC Y OC CU R A FT ER OFF ICE HOURC ON TA C T U M P ; SEC U R ITY A T 549 1121 09 FIR ST AID T R EAT MEN T

W IT NESS

IN FORM SHE UN IT

SITE C OM M AND ER / EM ER GENC Y C OOR D INATOR

AC T IVATE EM ER GEN C Y R ESPONSE T EAM (ER T)

EM ER GENC Y R ESPONSE T EAM (ER T)

C LEAN TH E SPILL

EM ER GENC Y R ESPONSE T EAM (ERT) / W IT NESS NO

SEN D VIC TIM T O C LIN IC T OGET HER W IT H C SD S

U MP Stud ent Health U n it Co ntact: N o 09- 549 2539

EM ER GENC Y R ESPONSE T EAM (ER T)

SPILL SECUR ED

YES SITE C OM M AND EREM ER GEN CY / COOR D INATOR CALL F IRE& RESC U E D EPT U PON T HE AR RIVAL FIR E & R ESCU E D EPT , H AN DOVER ALL DU TIES TO TH EM F IR E & RESCU E D EPT C ONT A C T N O . GEN ER AL 999 : T AM AN TAS09-538 3704 : KUAN T AN 09-513 5544 :

EM ER GEN CY RESPON SE T EAM (ERT) AND FIR E& R ESCUE D EPT

F IR E& RESC U E D EPT

SPILL SEC URE AND FIR E & R ESC U E D EPT C ON FIR M CON D ITION IS SAF E DEC LARE EM ERGENC Y OVER

SITE C OM M AND EREM ER GEN CY / COOR D INATOR

END

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Engineering Laboratory IV DKK3761

UN I V E R SI T I M A L A Y SI A P A H A N G
F A C U L T Y O F C H E M IC A& N A T U R A L R E S O U R C E S L E N G IN E E R IN G FIRE NOTIFICATION RESPONSE &
BY WHOM PROCESS FLOW INFORMATION

ST AR T

W IT N ESS

F OU N D F IR E

BIG F IR E / U N C ON T R OLLABLE W IT N ESS ASSESS SIT U AT ION

SM ALL F IR E C ON T R OLLABLE /

W IT N ESS

NO

KN OW H OW T O F IGH T F IR E ?

YES W IT N ESS LOOKIN G F OR F IR E F IGH T IN G EQU IPM EN T H A N D L IN G OF F IR E EXT IN GU ISH ER P Pull the s afety pin A Aim disc harge noz z le to fire bas e S Squeeze the lev er S Sw eep bac k and forth as y ou m ove c los er to the fire

W IT N ESS

PU T OU T F IR E

YES

NO W IT N ESS SH OUT F IR!EF IR E BR EAK !, EM ER GEN C Y GLASS F IN D SAF E LOC AT ION IN F OR M SH E & U N IT AC T IVAT E EM ER GEN C Y R ESPON SE T EAM (ER T) IN F OR M SH E U N IT

W IT N ESS

SIT E C OM M AN D EREM ER GEN C Y / C OOR D IN AT OR

SH E C ON T A C T N.O 09-549 2801 / 2803 / 2847 IF EM ER GEN C Y OC C U R A F T ER OF F IC E H OU ; C ON T A C T U M P R SEC U R IT Y A T 549 1121 09

EM ER GEN C Y R ESPON SE T EAM (ER T)

YES

PU T OU T F IR E

NO SIT E C OM M AN D EREM ER GEN C Y / C OOR D IN AT OR C ALL F IR E R ESC U E D EPT & F IR E & R ESC U E D EPT C ON T A C T . O N GEN ER AL 999 : T AM AN T AS09-538 3704 : KU AN T AN 09-513 5544 :

EM ER GEN C Y R ESPON SE T EAM T) (ER AN D F IR E& R ESC U E D EPT

U PON T H E AR R IVAL F IR ER ESC U E & D EPT, H AN D OVER ALL D U T IES T O T H EM

F IR E& R ESC U E D EPT

F IR E PU LL OU T AN D F IR E ESC U E &R D EPT C ON F IR M BU ILD ING IS SAF E

SIT E C OM M AN D EREM ER GEN C Y / C OOR D IN AT OR

D EC LAR E EM ER GEN C Y OVER

END

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Engineering Laboratory IV DKK3761

UNI V E R SI T I M A L A Y SI A P AH A NG
F A C U L T Y O F C H E M IC A & N A T U R A L R E S O U R C E S L E N G IN E E R IN G HUMAN INJURY NOTIFICATIONRESPONSE &
BY WHOM PROCESS FLOW INFORMATION

ST AR T

W IT N ESS

H U M AN IN JU R Y

W IT N ESS

NO

T R AIN ED IN F IR ST AID TR EAT M EN T

Po in t T o R emember : 1. D o not m ove victim unless to prev ent further injury . 2. D o not rem ove any evidence

YES W IT N ESS F IR ST AID T R EAT M EN T

SH E C o n tact N:o 09-549 2801 / 2803 / 2847 Fir st A id er C o n tact : o N En. Anuar : 013-6986946 En. H isham : 012-3058524 Pn. H afiz ah : 012-9848565 IF EM ER GEN C Y OC C U R A F T ER OF FIC E H OU; C ON T A C T U M P R SEC U R IT Y A T 549 1121 09

W IT N ESS

IN F OR M SH E U N IT IR ST AID ER /F

EM ER GEN C Y R ESPON SE TEAM (ER T)

NO

N EED F U R TH ER TR EAT M EN T

YES EM ER GEN C Y R ESPON SE TEAM (ER T) / W ITN ESS SEN D VIC TIM T O C LIN/IC OSPITAL H

U M P Stu dent H ealth U nit C o n tact N o : 09- 549 2539 H T A A C on tact N o : 09-557 2222

SIT E C OM M AN D EREM ER GEN C Y / C OOR D IN AT OR

EM ER GEN C Y OVER

END

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Engineering Laboratory IV DKK3761

UNI VE R SI T I M AL AY SI A P AH ANG
F A C U L T Y O F C H E M IC A L N A T U R A L R E S O U R C E S & E N G IN E E R IN G GAS LEAKAGE NOTIFICATION RESPONSE &
BY WHOM PROCESS FLOW INFORMATION

STAR T

W I TN ESS

D ET EC T GAS LEAKAGE

W IT N ESS

ALER T PER SON N EL IN AD JAC EN T AR EA C U T OF F GAS SU PPLY F R OM SOU R C E Po int T o R emember : 1 . Please do not handle gas leakage unless y ou w ear a com plete Personal Prot ectiv e Equipm ent (PPE). 2 . If flam m able gas involv e not , do operate electrical s w itc hes unles s to turn off electric equipm ent . 3 . If gas leak ge is flam m able , extinguis h flam es and all other s ourc es of ignition .

W IT N ESS

W IT N ESS

NO

T R AIN ED T O H AN D LE GAS LEAKAGE YES R EFER T O C SD S F OR AC TION (AC C ID EN T AL R ELEASE M EASU R ES PAR ) T

NO

IN VOLVE IN J U R Y

YES R EF ER T O C SD S FOR AC T ION (FIR ST AID M EASU R ES PAR T )

W IT N ESS

SH E C on tact N o : 09-549 2801 / 2803 / 2847 W IT N ESS IN F OR M SH E U N IT IN FOR M SH E U N ITF IR ST AID ER / F ir st A id er C o n tact N o : En. Anuar : 013-6986946 En. H is ham : 012-3058524 Pn. H afizah : 012-9848565 IF EM ER GEN C Y OC C U R A F TER OF F IC E H OU R C ON T A C T U M P ; SEC U R ITY A T 549 1121 09

SIT E C OM M AN D ER / EM ER GEN C Y C OOR D IN AT OR

AC T IVAT E EM ER GEN C Y R ESPON SE T EAM(ER T)

EM ER GEN C Y R ESPON SE T EAM (ER T)

FIR ST AID T R EAT M EN T

EM ER GEN C Y R ESPON SE T EAM (ER T) / W IT N ESS

SEN D VIC TIM T O C LIN IC T OGET H ER W IT H C SD S

U M P Stud ent H ealth U nit C o n tact :N o 09- 549 2539

EM ER GEN C Y R ESPON SE T EAM (ER T)

YES

GAS LEAKAGE SEC U R ED

NO SIT E C OM M AN D ER EM ER GEN C Y / C OOR D IN AT OR C ALL F IR E& R ESC U E D EPT U PON T H E AR R IVAL F IR E & R ESC U E D EPT , H AN D OVER ALL D U T IES T O T H EM F IR E & R ESC U E D EPT C ON T A C T N O . GEN ER AL: 999 T AM AN T AS 09-538 3704 : KU AN T AN 09- 513 5544 :

EM ER GEN C Y R ESPON SE T EAM T) (ER AN D F IR E& R ESC U E D EPT

FI R E& R ESC U E D EPT

GAS LEAKAGE SEC U R E AN D F IR E& R ESC U E D EPT C ON F IR M C ON D IT ION IS SAF E D EC LAR E EM ER GEN C Y OVER

SIT E C OM M AN D ER EM ER GEN C Y / C OOR D IN AT OR

END

21

Engineering Laboratory IV DKK3761

UN I VE R SI T I M AL A Y SI A P AH ANG
F A C U L T Y O F C H E M IC A L N A T U R A L R E S O U R C E S & E N G IN E E R IN G EXPLOSION NOTIFICATION RESPONSE &
BY WHOM PROCESS FLOW INFORMATION

ST AR T

W ITN ESS

F OU N D EXPLOSION

W ITN ESS

SH OUT EXPLOSION EXPLOSION !, !, BR EAK EM ER GEN CY GLASS F IN D SAF E LOC ATION IN FOR M SHE & U NIT AC T IVAT E EM ERGEN C Y R ESPON SE T EAM (ER T) SH E C ON TA C T N.O 09-549 2801 / 2803 / 2847 IF EM ER GEN C Y OCC U R AF T ER OFF IC E H OU R C ON T A C T U M P SEC U R IT Y A T 549 1121 09

W IT N ESS

SIT E COM M AN D EREM ER GEN C Y / C OOR D INAT OR

EM ER GEN CY R ESPON SE T EAM (ER T)

UN D ER CONT R OL ASSESS SITU ATION

EM ER GEN CY R ESPON SE T EAM (ER T)

PU T OU T EXPLOSION

NO

BEYON D C ON T ROL

YES SIT E COM M AN D EREM ER GEN C Y / C OOR D INAT OR C ALL F IRE R ESC U E D EPT &

F IRE & R ESC U E D EPT CONT A C T N O . GEN ER AL 999 : T AM AN T AS09-538 3704 : KU AN TAN 09-513 5544 :

EM ER GEN C Y R ESPON SE T EAM T) (ER AND FIR E& R ESC U E D EPT

U PON T H E ARR IVAL F IR ER ESC U E & D EPT, H AN DOVER ALL DU T IES TO T H EM

F IRE & R ESC U E D EPT

EXPLOSION OVER AN D F IR E & R ESC UE DEPT C ON F IRM BU ILD ING IS SAFE

SIT E COM M AN D EREM ER GEN C Y / C OOR D INAT OR

D EC LAR E EM ERGEN C Y OVER

END

22

Engineering Laboratory IV DKK3761 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. 2. Tray Drier Unit Rice 4. 3. Air velocity measurement device 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

Engineering Laboratory IV DKK3761 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. states RESULTS Table Experimental Data 1 Heating Level : Air Speed Time,t min 0 5 10 : Air Temp., T1 Air Humidity, F1 Air Temp., T2 Air Humidity, F1 Mass, m 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

Table Experimental Data 2 Heating Level : Air Speed Time,t min 0 5 10 : Air Temp., T1 Air Humidity, F1 Air Temp., T2 Air Humidity, F1 Mass, m

24

Engineering Laboratory IV DKK3761 GUIDE FOR DISCUSSION 1. 2. Plot the mass of material to be dried versus drying time. Explain the plotted graph. Find the X value and complete the table. Table Experimental Data 1 Time,t min 0 5 10 Air Temp., T1 Air Humidity, F1 X Air Temp., T2 Air Humidity, F1 X Mass, m

Table Experimental Data 2 Time,t min 0 5 10 Air Temp., T1 Air Humidity, F1 X Air Temp., T2 Air Humidity, F1 X Mass, m

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

25

Engineering Laboratory IV DKK3761 Psychrometric Chart and Air Characteristics

Figure 1: Psychrometric Chart

Engineering Laboratory IV DKK3761 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. EQUIPMENT/APPARATUS/MATERIAL 1. CTS4 Climbing Film Evaporator 2. Steam supply 3. Vacuum pump 4. Stop watch 5. Digital balance EXPERIMENTAL PROCEDURES 1. 2. 3. 4. 5. 6. 7. 8. Prepare standard salt solution and get its conductivity by using conductivity meter. Prepare 20L salt solution with concentration 25g/L and feed in the feed vessel. Start the vacuum operation so that the liquid from the feed vessel can be sucked into the vessel column. Flow the cooling water to cool down the steam in the condenser. Set the feed flow rate FI 1 at 0.3 L/min and vacuum pressure at 0.4 bar. Set the steam pressure at 0.5 bar. 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. Repeat steps 6 to 7 for steam pressure 1 bar(g). RESULT 6. Beakers 7. Glass rod 8. Portable conductivity meter 9. Water supply

Engineering Laboratory IV DKK3761 Experimental Data Steam Pressure (Bar) 0 5 10 0.5 15 20 25 30 0 5 10 1.0 15 20 25 30 GUIDE FOR DISCUSSION 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. Time (s) T1 (0C) T2 (0C) Volume (mL) V3 V5 V3 Conductivity (mS) V5

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 Absorptioncolumnisoneoftheseparationtechniquesthatinvolveliquidandvapor.Oneor morecomponentofagasmixturecanbeseparatedwhenacertainliquidflowthroughitcounter currently. The liquid absorbs the component(s) and mass transfer process which separates the component(s)fromgasmixtureoccurs.Packedmaterialisusedtoincreasethecontactsurfacearea inabsorptionprocesswhichenhancestheefficiencyandshortensthedurationoftheprocess. EQUIPMENT/APPARATUS/MATERIAL 1. Packed Absorption Column 2. Air Compressor EXPERIMENTAL PROCEDURES 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. 3. Water and Air 4. Stop watch

Chemical Engineering Laboratory II BKF3751 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 Water flow rate, W (L/min) 2.5 Table 1 Air flow rate, G Pressure Drop, P (L/min) (cm H2O) Time (every 5 minutes)

3.0 Table 2 Water flow rate, W Pressure Drop , P (L/min) 2.0 2.5 3.0 3.5 (cm H2O)

Air flow rate, G (L/min) 50

Time (every 2 minutes)

GUIDE FOR DISCUSSION 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. 4. 5. 6. industries? 7. Explain roughly one of the applications that are listed above? Describe the following terms: Flooding point, flooding velocity, and loading point. Discuss your data and results obtained from the experiment. List down 5 application of this process that is used in petrochemical

Engineering Laboratory IV DKK3761 EXPERIMENT 4: THIN FILM EVAPORATOR UNIT OBJECTIVE 1. 2. To demonstrate the separation of ethanol from water using the thin film To determine effect of heating temperature and vacuum pressure on the separation evaporative process 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. EQUIPMENT/APPARATUS/MATERIAL 1. BP215 Thin Film Evaporator 2. Stop watch 3. Beakers 4. Refractometer EXPERIMENTAL PROCEDURES 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: 100C vacuum controller PIC-1 : 400 mbar 5. Cooling Water Supply 6. Ethanol 7. Measuring Cylinder 8. Water

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

Engineering Laboratory IV DKK3761 when the distillate temperature doesnt 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 N o. Heating Temp.
o

: Distillate Flowrate RI mL/min Bottom Product Flowrate RI Composi mL/min tion

P1 : 60% stroke, 60 stroke/min Vacuum Pressure mbar 400 400 400 400 Temp
o

Composit ion

1 2 3 4 5 6

100 100 100

GUIDE FOR DISCUSSION 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
Efficiency = distillate flow rate x distillate compositio n x100 % feed flow rate x feedcompos ition

5. Compare the separation efficiencies between different operating conditions to determine the effect of temperature and pressure.

Engineering Laboratory IV DKK3761

Engineering Laboratory IV DKK3761

FEED RATE SETTING DIAGRAM FOR FEED PUMP

Chemical Engineering Laboratory II BKF3751 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. EQUIPMENT/APPARATUS/MATERIAL 1. Rotadest R50 Rotary Evaporator 2. Stop watch 3. Beakers 4. Refractometer EXPERIMENTAL PROCEDURES 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: 5. Cooling Water Supply 6. Ethanol 7. Measuring Cylinder 8. Water

Chemical Engineering Laboratory II BKF3751 a. Bath temperature T1C-1 : 80C 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 Time Minute 5 10 Distillate Temperature o C : Distillate Volume mL RI Distillate Composition Vol % Distillate Flow Rate mL/min Volume of Ethanol in Distillate mL

Volume and Composition of Concentrate: GUIDE FOR DISCUSSION 1. Plot the calibration curve of RI Vs ethanol composition 2. Plot a graph of distillate temperature, composition, flowrate vs. time. Discuss the findings

Chemical Engineering Laboratory II BKF3751 3. Calculate the overall separation efficiency of rotary evaporator. Efficiency = Total amount of ethanol in distillate Initial amount of ethanol in rotary flask X 100%

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

Chemical Engineering Laboratory III BKF3781 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.

EQUIPMENT/APPARATUS/MATERIAL 1. Sieve Tray Distillation Unit 2. Refractometer 3. 5L of binary mixture (ethanolwater). 4. Beakers. EXPERIMENTAL PROCEDURES 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.

Chemical Engineering Laboratory III BKF3781 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) 1.00 1.50 2.00 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) 1.00 1.50 2.00 Temp (oC) Distillation RI Mole Fraction Bottom Product Temp (oC) RI Mole Fraction HETP (mm)

Chemical Engineering Laboratory III BKF3781 GUIDE FOR DISCUSSION 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

Engineering Laboratory IV DKK3761 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

EXPERIMENTAL PROCEDURES 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. 4. 5. 6. Remove valve HV-01 and fill the feeding funnel V-100 with the homogeneous mixture. Switch ON the main power supply at the control panel. ON computer or the software program. Set the thermostat at 70C, Chiller at 12C 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. 9. Once the chiller temperature and thermostat temperature have reach the set points, the equipment is ready for experiment 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. 4.

The collected distillate and condensate can then be used for futher testing. The feed flowrate is calculated by dividing the total volume of sample collected to the total time taken.

GENERAL SHUT-DOWN PROCEDURES 1. 2. 3. 4. 5. 6. Switch off vacuum pump. Close valve HV03 to stop feeding. Switch off stirrer motor. Turn off thermostat. Close HV13. Open valve HV 01, HV 06 and HV 07. 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 Effect of stirrer speed Vacuum pressure, PT-200 Evaporator Temperature, TT-100 Feed Flow rate Contact time EG-water ratio 100mbar 70C ml/min 10 min 7:3

Time Start

Stirrer Speed(rpm) 50 100 200 220

Distillate Volume (ml)

Concentrate Volume (ml)

Separation Efficiency (%)

1. Effect of evaporator temperature Feed flow rate Stirrer speed, M-500 Vacuum pressure Contact time EG-water ratio ml/min 220rpm 100mbar 10min 7:3

Time Start

Temp (C) 70 72 74 76

Distillate Volume (ml)

Concentrate Volume (ml)

Separation Efficiency (%)

GUIDE FOR DISCUSSION 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.

V-1 0 0

Fe d g Fu n l e in ne

V 0 -1 1

M aterial: Boro. glass Capacity: ap prox. 200 m 0 l c/w tem perin jacket; p g ressure eq ualizing tu , need valve be le In GL4 Outlet: NS2 2 let: 5; 9/3

Co Tra ld p

V-1 2, V 0 0 -1 3

M aterial: Boro. glass For dry ice usage c/w drain valve DN6 Vacuum: 2 KF15/3 x Outlet: NS29/32

Gra uae Cy e d t d lind rs

V 0 to V 0 -1 4 -1 7
M aterial: Boro. glass Capacity: 2 m 50 l Round bottom

Material: Boro. glass Capacity: 25 m 0 l c/w/ DN valves for inlet 3 outlet & ventin g Inlet: NS29 2; Outlet: NS29/32 /3

Prod Ve ls uct sse

V 0 -1 8

Ve ls sse

T-2 0 0

M aterial: Boro. glass Capacity: 2 m 0 l Round Bottom

Sh Pah Ev p t ort t a oraor

Material: Boro. glass c/w roller wiper cage(Rulon rolls); m agnetic 2 stirrer sealin , heating jacket (0.03 m); g 2 coolingcoil (0.05 m ); Feed: NS29/32 ; Outlet: NS2 9/32; Vacu um: NS 9/32 2

E-3 0 0
H ain Ja e e t g ck t
M aterial: Boro. glass 2 Su rface: 0.03 m

E-3 1 0
Coolin Coil g
Material: Boro. glass Surface: 0.05m2

B-4 0 0
Th rm l Oil Bah e a t
Rang 28 to 28 C ( 1 K) e: 0 0.0 Heater: 3000 watt Bathcapacity: approx. 12-L Pum m 24 LPM p: ax.

B-4 1 0
Ch r ille
Range: 5 to 25 C ( C) 2 Cooling cap acity: 1 00 BTU/hr 8,0 Bath capacity: 50-L Pu p: 50 LPM m

M0 -5 0
St r D e irre riv
Power: 100 W Torque: 250 Ncm Sp eed: 8 to 20 rpm 00 Ou tput: 0 1 0V

P-1 0 0
Va u Pu p cu m m
2-stage Rotary Vane Type Ultim Vacuum: 6 x 10-3 m ate bar Pum ingSpeed: 2.9m3 p /hr

HV 01

V 0 -1 0
HV 13

HV 02

TIC TT 100 100

SIC 500 ST 500

M0 -5 0
El.

M
HV 03

B 0 -4 0

TT 102

T-2 0 0
PT 200

( 0 E-3 1) E-3 0, 0
V 14

Vent

P 0 -1 0

V-1 1 0

HV 04

TT 103

HV 05

HV 06 HV 10

HV 07

V 0 -1 2 V 0 -1 8

V 0 -1 3

TIC TT 101 101

HV 12 HV11 HV 08 HV 09

El.

B 0 -4 1 V-1 4 0 V 0 V 0 V 0 -1 5 -1 6 -1 7

Sh Pah D illa ionU it ort t ist t n

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