vapor - liquid equilibrium (kuc) · 4.1 diagram alir percobaan ... open feed cover, insert the...

EXPERIMENT MODULE

CHEMICAL ENGINEERING EDUCATION LABORATORY

VAPOR - LIQUID EQUILIBRIUM

(KUC)

CHEMICAL ENGINEERING

FACULTY OF INDUSTRIAL TECHNOLOGY

INSTITUT TEKNOLOGI BANDUNG

2018

INSTRUCTIONAL LABORATORY

CHEMICAL ENGINEERING FTI - ITB

MODUL KESETIMBANGAN UAP CAIR (KUC)

KUC – 2018 2

Contributors:

Dr. Antonius Indarto, Dr. Ardiyan Harimawan, Gisela Swastika, Mirna Jatiningrum, Darien Theodric




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TABLE OF CONTENTS

TABLE OF CONTENTS ................................................................................................................................ i

LIST OF FIGURES ...................................................................................................................................... ii

LIST OF TABLES ....................................................................................................................................... iii

CHAPTER I................................................................................................................................................ 1

PREFACE .................................................................................................................................................. 1

CHAPTER II .............................................................................................................................................. 2

GOALS AND OBJECTIVES ......................................................................................................................... 2

2.1 Goals ............................................................................................................................................. 2

2.2 Objectives...................................................................................................................................... 2

CHAPTER III ............................................................................................................................................. 3

EXPERIMENTAL DESIGN .......................................................................................................................... 3

3.1. Equipments and Measurement Tools .......................................................................................... 3

3.2. Materials ...................................................................................................................................... 3

3.3 Ebuliometer Equipment Layout .................................................................................................... 3

BAB IV ...................................................................................................................................................... 5

WORKING PROCEDURE ........................................................................................................................... 5

4.1 Diagram Alir Percobaan ................................................................................................................ 5

4.2 Working Procedure on the Usage of Ebuliometer ........................................................................ 5

BIBLIOGRAPHY ........................................................................................................................................ 8

APPENDIX A ............................................................................................................................................. 9

RAW DATA TABLE .................................................................................................................................... 9

APPENDIX B ........................................................................................................................................... 12

CALCULATION PROCEDURE ................................................................................................................... 12

JOB SAFETY ANALYSIS ........................................................................................................................... 13




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LIST OF FIGURES

Figure 1. Ebuliometer equipment layout. ................................................................................................ 4

Figure 2. Experimental flow diagram. .................................................................................................... 5

Figure 3. Curve example of refratometer calibration. ........................................................................... 10




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LIST OF TABLES

Table 1. Calibration of Refractormeter. .................................................................................................. 9

Table 2. Experiment table. ...................................................................................................................... 9

Table 3. Example of refractometer calibration. .................................................................................... 10

Table 4. Example of Experiment Data. ................................................................................................. 11




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CHAPTER I

PREFACE

The liquid vapor equilibrium data is the thermodynamic data subjected to the design and

operation of distillation columns. Examples of actual thermodynamic data of liquid vapor

equilibrium in various design methods of packed column and tray column distribution can be

seen in Treyball 1982 and King 1980. The equilibrium of liquid vapor can be obtained

through experiments and measurements. However, a comprehensive experiment can be

obtained from a series of measurement methods. Comprehensive real experiments take a long

time and cost a great deal, so a more common way is to measure the data in some conditions

and then summarize it in the form of mathematical models that are relatively easy to

implement in computations. The development of the mathematical model must also have an

appropriate theoretical foundation so that it can be accounted for application beyond the limit.

This experiment aims to obtain the liquid vapor equilibrium data of binary systems. The data

obtained are correlated in the form of thermodynamic models. Assessment of model

parameters is performed by non-linear regression based on the least squares number criteria.

To achieve the objectives of this experiment, adequate understanding of the topic is important

before meeting:

1. Vapor-liquid equilibrium (Daubert 1985, Smith dan Van Ness 1987, Sandler

1989,Prausnitz et al 1986, etc)

2. Vapor-Liquid Equilibrium measurement techniques (phase equilibrium Walas

1985,Black 1987)

3. Data consistency trial of Vapor-liquid equilibrium (Lu 1960)

4. Multivariable minimization techniques using Simplex (Reklaitis1982, Edgar and

Himmelblau 1988, optimization course module Soerawidjaja, 1990)

5. Gas chromatography analysis and refractive index




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CHAPTER II

GOALS AND OBJECTIVES

2.1 Goals

By doing the vapor-liquid equilibrium practicume module, students can learn principles of

binary system of vapor-liquid equilibrium.

2.2 Objectives

By the end of this practicum, students are expected to:

1. Have experience in conducting experiments about vapor-liquid equilibrium

2. Able to do calculations concerning vapor-liquid equilibrium based on one of the

thermodynamic module in literature.

3. Able to determine parameters in thermodynamic model above.




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CHAPTER III

EXPERIMENTAL DESIGN

3.1. Equipments and Measurement Tools

Equipments used in the experiments are:

1. SOLTEQ Vapor Liquid Equilibrium consisting of: condenser, evaporator, bottom

hold up, pressure relief valve, control panel, top sampel collector, rotameter, and

heater.

2. Glass thermometer

3. Measuring Cup

4. Beaker Glass

5. Refractometer

6. Water hose

3.2. Materials

Mixture of binary ethanol/methanol/acetone/water. 5L of mixture is needed for each

experiment.

3.3 Ebuliometer Equipment Layout

In this experiment, the measured data is isobaric data under atmospheric conditions.

Equilibrium data retrieval is done by using ebuliometer as shown in Figure 3.1.




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Figure 1. Ebuliometer equipment layout.




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BAB IV

WORKING PROCEDURE

4.1 Diagram Alir Percobaan

Generally, the experiment is done by following procedure shown by Figure 4.1.

Start

Calibration of refractometer

Start up of SOLTEQ/VLE

End

Insert feed, turn on heater

Data processing

Match data with literature

Sample retrieval, check with

refractometer until three similar

consecutive data

Data

Feed preparation

VLE data from literature

Figure 2. Experimental flow diagram.

4.2 Working Procedure on the Usage of Ebuliometer

The main equipment in the experiment, ebuliometer, is operated by following few steps as

follows:

Start-up :

1. Check all valve condition, valves must be in closed condition

2. Check heater condition, heater must be in off condition.




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3. Turn on equipment by connecting it’s electrical connection.

4. Main switch is turned on.

Procedure:

1. Open feed cover, insert the feed, and close the lid.

2. Open valve 13 and valve 14, check feed level, make sure level is on ¾ of maximum

level, then close valve 13 and valve 14.

3. Check the condition of valve 8, make sure valve 8 is in open condition to make it in

atmospheric pressure.

4. Cooling water valve is turned on, condensor is turned on.

5. Open valve 10, check if cooling water is flowing between 5-10 LVM and wait until

constant. Wait until flow becomes constant.

6. Set starting temperature to 100⁰C on TT01

7. Turn on heater

8. Wait for 5 minutes, record temperature shown on TT02, get sample out.

9. To retrieve sample containing condensate from gas:

a. Open valve 5 and 6. Make sure valve 5 is opened until all condensates have gotten

in, then close the valve.

b. Open valve 7 to retrieve the sample.

10. To retrieve the liquid sample:

a. Open valve 12

b. Open valve 4 and 2

c. Wait for a moment, then close valve 2

d. Open valve 3 to retrieve sample.

Shut Down :

1. Turn off heater

2. Open valve 11

3. Wait until value shown on TT02 ≤ 50⁰C.

4. open valve 2 and valve 3, store all liquid on provided containtment.

5. Open valve 6 and valve 7, store all liquid and put into provided containtment.

6. Wash ebuliometer by inserting cooling water hose to valve 3 and wait until water

level increases to ¾ maximum level. Then turn off cooling water valve and close




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valve 3 at the same time. Hose is returned away. Open valve 3 until all water in the

equipment is drained off.




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BIBLIOGRAPHY

Smith, V., Van Ness, Introduction to Chemical Engineering Thermodynamics, 4th

Edition,

McGraw-Hill, Singapore, 1987, Chapter 10, 11, 12

Larrinaga, L., Graphically Determining the Wilson Parameters, Chemical Engineering,April

1981, pp. 87-91

Silverman, N., and Tassios, D., The NUmber of Roots in thr Wilson Equation and ItsEffect

on Vapor Liquid Equilibrium Calculations, Ind. Eng. Chem. Proc. Des. Dev.,16(1), 1977




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APPENDIX A

RAW DATA TABLE

Component A = __________ Component B = ___________

Density A = __________ Density B = ___________

Mr A = __________ Mr B = ___________

Table 1. Calibration of Refractormeter.

Volume

A

Volume

B

Mole

Fraction wt%

Refractive

Index

Table 2. Experiment table.

P VA (L) VB (L) Temperature (oC) Refractive Index Composition

(wt%)

Liquid Vapor Liquid Vapor Liquid Vapor




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Example:

Component A = Metanol 99.9% Component B = Air

Density A = 0.79 g/mL Density B = 1 g/mL

Mr A = 32.04 g/mol Mr B = 18 g/mol

Table 3. Example of refractometer calibration.

Volume

A

Volume

B

Mole

Fraction wt%

Refractive

Index

0 10 0.0000 0.00 1.3334

1 9 0.0470 8.07 1.3354

2 8 0.0999 16.49 1.3369

3 7 0.1598 25.29 1.3404

4 6 0.2283 34.50 1.3414

5 5 0.3074 44.13 1.3425

6 4 0.3997 54.23 1.3417

7 3 0.5087 64.83 1.3406

8 2 0.6397 75.96 1.3387

9 1 0.7998 87.67 1.3342

10 0 1.0000 100.00 1.33

Figure 3. Curve example of refratometer calibration.

1.326

1.328

1.33

1.332

1.334

1.336

1.338

1.34

1.342

1.344

0.0000 0.2000 0.4000 0.6000 0.8000 1.0000 1.2000

Re

frac

tive

Ind

ex

Refractive Index




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Table 4. Example of Experiment Data.

P

(atm)

VA

(L)

VB

(L)

Temperatur

e (oC)

Refractive

Index

Compositio

n (wt%)

Composition

from Literature

(wt%)

Error (%)

Liq Vap Liq Vap Liq Vap Liq Vap Liq Vap

1 1 3 86.2 83.

3

1.3

379

1.341

0

0.10

5

0.49

8

0.12 0.53 12.5 6.04

1 2 3 82.8 79.

9

1.3

394

1.338

7

0.15

0

0.61

5

0.17 0.61 11.7

6

-

0.82

1 3 3 78.1 77.

8

1.3

410

1.336

4

0.21

0

0.71

5

0.3 0.67 30.0 -

6.72

1 2 1 73.7 72.

7

1.3

415

1.334

8

0.47

0

0.78

2

0.480 0.79 2.08 1.01

1 3 1 72.0 71.

0

1.3

407

1.333

3

0.52

0

0.85

0

0.560 0.83 7.14 -

2.41

1 5 1 70.1 69.

3

1.3

371

1.332

6

0.68

5

0.88

0

0.650 0.88 -5.38 0.00




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APPENDIX B

CALCULATION PROCEDURE

Data processing needed in the experiment can be done by following below procedure:

1. perpar Txy graph according to the literature

2. Density calculation:

( )

( )

3. Mole fraction calculation

((

)

( )

)




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JOB SAFETY ANALYSIS

No. Material Properties Countermeasures

1. Water

Colorless

Odorless

Not-Toxic

Boiling point of 100 oC

Melting point of 100 oC

Stable

Electrically conductive

No specific countermeasures

needed.

2. Ethanol

Liquid

Colorless

Volatile

Flammable in liquid or gas phase

Light odor

Boiling point : 78oC

Melting point : -114oC

Soluble in water

make sure containtment is closed

when not being used

Keep in cool place with good

ventilation

Put away from fire

Avoid contact with eye and

mouth.

Accidents that may happen Countermeasures

Inhaled ethanol vapor Get victim to room with frash air. If not conscious and

breathing, give resuscitation. Seek medical aid.

Solution splashed or spilled from test tube In case of contact with eye or skin, wash with water for

at least 15 minutes. If swallowed, seek medical aid.

Short circuit connection due to equipment

contact with water

Disconnect electrical connection to the equipment

Broken equipment Don’t panic and immediately clean shards. If shards got

contacted with skin, clean the wound with antiseptic. In

case of urgent condition, seek medical aid.

Safety Gears

Lab coat Goggle Gloves Shoes




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Asisten Pembimbing Koordinator Lab TK

Preparation of the equipment

Make sure hose from condensor is connected

well.

Make sure all valves are closed in the starting

of the experiment, expect for pressure

controlling valve.

Make sure elecrical cables are connected well

and don’t interfere with experiment.

Calibration with refractometer

Make sure electrical connection on

refractometer is connected well.

Be careful in applying acetone and

sample into refractometer

Percobaan

Pastikan semua valve dibuka dan ditutup

pada waktu yang tepat

Pastikan heater menyala setelah umpan

masuk ke dalam ebuliometer

Pastikan kondensor mengalir selama

percobaan

Pasca Percobaan

Umpan dikuras dari ebuliometer setelah

temperatur heater turun hingga di bawah 50˚C

Alat diperbolehkan dimatikan setelah

temperatur kesetimbangan di bawah 50˚C

Putus hubungan listrik setelah alat telah di

switch off

Bilas tempat umpan dengan air bersih

Matikan aliran dan rapikan selang kondensor

Pastikan semua valve tertutup setelah semua

aktivitas selesai dilakukan, kecuali valve

pengatur tekanan

Experiment

Make sure all valves are opened and

closed at the right time

Make sure the heater is turned on after

feed is introduced into ebuliometer

Make sure condensor in on during

experiment

After experiment

Feed is flushed from ebuliometer after heater

temperature drops below 50˚C

The equipment can be turned off after the

equilibrium temperature reaches below 50˚C

Unplug electrical connection after the

equipment is switched off.

Wash feed containtment with clean water

Turn of fluid flow and tidy condensor hose

Make sure all valves are closed after all

activities are done, except for pressure

controlling valve.

vapor - liquid equilibrium (kuc) · 4.1 diagram alir percobaan ... open feed cover, insert the...

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