KINETIC OF LIQUID PHASE REACTION (KIN) · MODUL KINETIKA REAKSI FASA CAIR (KIN) KIN – 2018 i...

EXPERIMENT MODULE

CHEMICAL ENGINEERING EDUCATION LABORATORY

KINETIC OF LIQUID PHASE REACTION

(KIN)

CHEMICAL ENGINEERING

FACULTY OF INDUSTRIAL TECHNOLOGY

INSTITUT TEKNOLOGI BANDUNG

2018

INSTRUCTIONAL LABORATORY

CHEMICAL ENGINEERING FTI - ITB

MODUL KINETIKA REAKSI FASA CAIR (KIN)

KIN – 2018 ii

Contributors:

Dr. Subagjo, Dr. I.G.B.N. Makertihartha, Dr. Ardiyan Harimawan, Hilman Prasetya Edi,

Muhammad Afif Naufal, Darien Theodric




KIN – 2018 i

TABLE OF CONTENTS

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

LIST OF FIGURES ......................................................................................................................... iii

LIST OF TABLES .......................................................................................................................... iv

CHAPTER I ..................................................................................................................................... 5

PREFACE ........................................................................................................................................ 5

CHAPTER II EXPERIMENT GOALS AND OBJECTIVES ......................................................... 6

2.1 Goals ...................................................................................................................................... 6

2.2 Objectives .............................................................................................................................. 6

BAB III ............................................................................................................................................. 7

EXPERIMENTAL DESIGN ............................................................................................................ 7

3.1 Experimental Scheme ............................................................................................................ 7

3.2 Supporting Equipment ........................................................................................................... 7

CHAPTER IV ................................................................................................................................... 8

WORKING PROCEDURE .............................................................................................................. 8

4.1 Working Procedure ............................................................................................................ 8

4.1.1 Calibratio of Equipment Scale ................................................................................... 8

4.1.2 Determining H2O2 Concentration and Solution Preparation ...................................... 9

4.1.3 Determining Heat Capacity of Reactor .................................................................... 10

4.1.4 Determining β Value ................................................................................................ 11

4.1.5 Determination of Reaction Heat ............................................................................... 12

4.1.6 Determination of Ea and A....................................................................................... 13

4.1.7 Determination of Mixture Density ........................................................................... 14

4.2 Measuring Methods ............................................................................................................. 14




KIN – 2018 ii

BIBLIOGRAPHY .......................................................................................................................... 15

APPENDIX A ................................................................................................................................ 16

RAW DATA TABLE ..................................................................................................................... 16

A.1 Temperature Calibration of Thermometer to Real Temperature ......................................... 16

A.2 Temperature Calibration of Thermocouple to Thermometer Temperature ......................... 16

A.3 Determining Heat Capacity of Reactor ............................................................................... 16

A.4 Determining β Value ........................................................................................................... 17

A.5 Determining Heat Capacity of Solution .............................................................................. 17

A.6 Determining ΔHr, Ea, and A Value ..................................................................................... 17

APPENDIX B ................................................................................................................................. 18

CALCULATION PROCEDURE ................................................................................................... 18

B.1 Determination of Real Temperature from Thermometer Calibration .................................. 18

B.2 Determination of Real Temperature from Thermocouple Calibration ................................ 18

B.3. Determination of (m.Cp)reactor ............................................................................................. 18

B.4. Determination of (m.Cp)solution ............................................................................................ 18

B.5 Determination of (m.Cp)system .............................................................................................. 19

B.6 Determination of H2O2 concentration by standardization with KMnO4 .............................. 19

B.7 Determination of Value. ................................................................................................... 19

B.8 Determination of β Value ................................................................................................... 19

B.9 Determination of ΔHr .......................................................................................................... 20

B.10 Determination of Solution Density .................................................................................... 20

B.11 Determination of Degree of Reaction , Ea, dan A ............................................................. 20

APPENDIX C ................................................................................................................................. 21

SPECIFICATION AND LITERATURE DATA ........................................................................... 21

C.1 Literature Data ..................................................................................................................... 21




KIN – 2018 iii

LIST OF FIGURES

Figure 1. Equipment scheme of the experiment. .............................................................................. 7

Figure 2. Experimental flow diagram of thermometer calibration. .................................................. 8

Figure 3. Experimental flow diagram of thermocouple calibration. ................................................ 9

Figure 4. Experimental flow diagram of determining H2O2 concentration. ..................................... 9

Figure 5. Experimental flow diagram of H2O2 preparation. ........................................................... 10

Figure 6. Experimental flow chart of Na2S2O3 solution preparation. ............................................. 10

Figure 7. Experimental flow diagram of determining heat capacity of reactor.............................. 10

Figure 8. Experimental flow diagram of determining β value. ...................................................... 11

Figure 9. Experimental flow diagram of determination of reaction heat. ...................................... 12

Figure 10. Experimental flow diagram of Ea and A. ..................................................................... 13

Figure 11. Experimental flow diagram of determination of mixture density. ................................ 14




KIN – 2018 iv

LIST OF TABLES

Table 1. Equipments and materials used in experiment. .................................................................. 7

Table 2. Data of temperature calibration of thermometer to real temperature. .............................. 16

Table 3. Calibration data of calibration of thermocouple temperature to thermometer temperature.16

Table 4. Data needed in determining heat capacity of reactor. ...................................................... 16

Table 5. Data needed in determining β value. ................................................................................ 17

Table 6. Data needed in determining heat capacity of solution. .................................................... 17

Table 7. Experiment data of determining ΔHr, Ea, and A. ............................................................ 17

Table 8. Density of water at various temperature. ......................................................................... 21

Table 9. Specific heat of water at various temperature .................................................................. 21

Table 10. ΔHr and β data for various reaction paths. ..................................................................... 21

CHAPTER I

PREFACE

Chemical engineering is the technical science of processes and processing that alters the state,

energy content, and/or composition of a material group to produce products with higher value and

benefit. Individuals who get official recognition as those who already mastered and practiced the

science of engineering is called a chemical engineer or a graduate of chemical engineering.

The duties of a chemical engineer concerning the application of chemical reactions in

practice/industry are:

1. To determine the size and operating conditions of the chemical reactor required to

produce a certain amount of product

2. To control, evaluate, and optimize the performance of operating reactors in the plant.

Implementation of such tasks requires the reaction kinetics data, that is quantitative information

about the rate/speed of the reaction and the influence of process variables such as temperature and

concentration on reaction rate. If the reaction kinetics data is completely unavailable, a chemical

engineer must be able to independently collect the data and then summarize them into ready-

made quantitative formulas.

The effort of collecting and summarizing the reaction kinetics data is called the determination of

reaction kinetics. This activity is generally in the form of experimental review in the laboratory,

because the development of kinetics science of chemical reactions has not reached the level that

allows for precise theoretical forecasting about the rate of reaction.

Students first have to understand about:

1. basic principles of mass & energy conservation and their application in the analysis

exothermic reaction beaviour in closed system.

2. basic principles of homogeneous reaction kinetics




KIN – 2018 6

CHAPTER II

EXPERIMENT GOALS AND OBJECTIVES

2.1 Goals

This practicum has goals to:

1. Learn about one experimental method in determining liquid phase homogen reaction

kinetics, especially between H2O2 ahnd Na2S2O3 in batch reactor.

2. Introduce one interpretation of reaction kinetic data.

2.2 Objectives

The objective of this practicum is that the student can find the correlation of equation of the

liquid phase reaction kinetic and determine the parameters of the homogeneous reaction.




KIN – 2018 7

BAB III

EXPERIMENTAL DESIGN

3.1 Experimental Scheme

The scheme of liquid phase reaction kinetics experiment is shown in Figure 1 below.

Figure 1. Equipment scheme of the experiment.

3.2 Supporting Equipment

Equipments and materials that are used in this experiment are shown in Table 1 below.

Table 1. Equipments and materials used in experiment.

Equipments and Measurement Tools Materials/Chemical Substances

1. Cup glass 100 ml (adiabatic batch reactor)

2. Magnetic stirrer

3. Titration equipment

4. Measuring pipette

5. Measuring cup

6. Volumetric flask

7. Thermocouple

8. Signal converter

9. Recorder (computer)

10. Thermometer

1. H2O2 Solution

2. Na2S2O3 Solution

3. KMnO4 Solution

4. H2SO4 Solution




KIN – 2018 8

CHAPTER IV

WORKING PROCEDURE

4.1 Working Procedure

4.1.1 Calibratio of Equipment Scale

a. Temperature calibration of thermometer

Figure 2. Experimental flow diagram of thermometer calibration.

b. Thermocouple calibration to thermometer




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Start

Water, T (30-100°C)

The temperature is measured

using thermometer and

thermocouple at the same time

and place

End

Calibration data of thermocouple

to thermometer are obtained

Figure 3. Experimental flow diagram of thermocouple calibration.

4.1.2 Determining H2O2 Concentration and Solution Preparation

a. Determining H2O2 concentration

Start

Concentrated H2O2 solution

End

Titration data are obtained, H2O2

concentration known

Dillute H2O2 solution

Titration with KMnO4 solution

(certain coencentration)

Figure 4. Experimental flow diagram of determining H2O2 concentration.




KIN – 2018 10

b. Preparation of H2O2 solution

Concentrated H2O2 solution Aqua DM

H2O2 solution with desired

concentration

Figure 5. Experimental flow diagram of H2O2 preparation.

c. Preparation of Na2S2O3 solution

Solid Na2S2O3 Aqua DM

Na2S2O3 solution with desired

concentration

Figure 6. Experimental flow chart of Na2S2O3 solution preparation.

4.1.3 Determining Heat Capacity of Reactor

Cold water (Td, md) Hot water (Tp, mp)

Water mixture

Mixture temperature obtained

Measure temperature with thermocouple

Heat capacity is obtained (Cp)

Mass balance analysis

Heat accumulation = heat in – heat out

Figure 7. Experimental flow diagram of determining heat capacity of reactor.




KIN – 2018 11

4.1.4 Determining β Value

H2O2 solution (a M, x mL, To) Na2S2O3 solution (b M, y mL)

Solution mixture

Mixture temperature obtained


Ratio of Ca/Cb

Figure 8. Experimental flow diagram of determining β value.




KIN – 2018 12

4.1.5 Determination of Reaction Heat


Solution mixture of H2O2 and

Na2S2O3 with stoichiometric ratio

T mixture is obtained


Calculate T difference

Mix with ratio of Ca/Cb


Accumulated heat = heat in – heat out

Reaction heat is obtained

Figure 9. Experimental flow diagram of determination of reaction heat.




KIN – 2018 13

4.1.6 Determination of Ea and A




Recorded data


and record the temperature

Reaction heat obtained



Accumulated heat = heat in – heat out

Ea and A are obtained

Arrhenius and rate equation

Figure 10. Experimental flow diagram of Ea and A.




KIN – 2018 14

4.1.7 Determination of Mixture Density




Cold mixture solution

Let cool and measure temperature with

thermocouple

Solution mass is obtained


Insert

Density of mixture is obtained

Pycnometer

Solution in pycnometer

Weigh

Aqua DM, Ta

Water mass is obtained

Insert

Pycnometer

Aqua DM in pycnometer

Weigh

Figure 11. Experimental flow diagram of determination of mixture density.

4.2 Measuring Methods

The experimental parameters obtained in the Liquid Phase Reaction Kinetics experiment are

temperature at a certain time by using thermocouple connected with the converter (signal

modifier) to be forwarded into the computer to obtain experimental data.




KIN – 2018 15

BIBLIOGRAPHY

Root, R.B., and Schmitz, R.A., AIChEJ, 15(5), 1969, pp.670-679

Coohen, W.C., and Spencer, J.L., Chem. Eng. Sci., 58 (12), 1962,pp.40-41 3.

Glasser, D., and Williams, D.F., Ind. Eng. Chem. Fundamental., 10(3), 1971, pp. 516-519.




KIN – 2018 16

APPENDIX A

RAW DATA TABLE

A.1 Temperature Calibration of Thermometer to Real Temperature

Table 2. Data of temperature calibration of thermometer to real temperature.

Material Real temperature (oC) Thermometer Temperature (

oC)

Melting Ice

Boiling

Water

A.2 Temperature Calibration of Thermocouple to Thermometer Temperature

Table 3. Calibration data of calibration of thermocouple temperature to thermometer

temperature.

Thermometer Temperature (oC) Thermocouple Temperature (

oC)

A.3 Determining Heat Capacity of Reactor

Table 4. Data needed in determining heat capacity of reactor.

Data Cold water reactor Hot water

Cp (J/g.0C)

ρ (g/mL)

Volume (mL)




KIN – 2018 17

T start (oC)

T end (oC)

A.4 Determining β Value

Table 5. Data needed in determining β value.

Run V H2O2 (ml) V Na2S2O3 (ml) α T min T max ΔT

1

2

3

A.5 Determining Heat Capacity of Solution

Table 6. Data needed in determining heat capacity of solution.

Data Cold solution Reactor Hot Solution

ρ (g/mL)

Volume (mL)

T start (oC)

T end (oC)

Cp (J/g.0C)

A.6 Determining ΔHr, Ea, and A Value

Table 7. Experiment data of determining ΔHr, Ea, and A.

Time, t (s) Temperature, T (oC)




KIN – 2018 18

APPENDIX B

CALCULATION PROCEDURE

B.1 Determination of Real Temperature from Thermometer Calibration

Determination of real temperature from thermometer temperature can be done by using

regression from calibration result

(1)

B.2 Determination of Real Temperature from Thermocouple Calibration

Determination of real temperature from thermocouple temperature can be done using

regression from calibration result of thermocouple temperature to thermometer temperature.

Then, the equation is substituted to equation (1).

(2)

(3)

B.3. Determination of (m.Cp)reactor

The heat capacity value of reactor can be determined by black principle, that heat

introduced or accepted to the system will equal to heat released by system. By following

equation, the reactor receives heat from hot water.

(4)

B.4. Determination of (m.Cp)solution

The heat capacity value of reactor can be determined by black principle, that heat

introduced or accepted to the system will equal to heat released by system. By following

equation, the reactor receives heat from hot water.

(5)




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B.5 Determination of (m.Cp)system

The heat capacity value of system can be determined using following equation:

(6)

B.6 Determination of H2O2 concentration by standardization with KMnO4

The concentration of concentrated H2O2 can be determined by titration with KMnO4 with

the addition of H2SO4 as an acidic atmosphere. The concentrated H2O2 should be diluted first

so that the required volume of KMnO4 to minimize H2O2 can be minimized. Here is the

equation used to determine the concentration of H2O2

[ ]

[ ]

(7)

Before titration is done with KMnO4, the standardization of KMnO4 solution is needed by

using H2C2O4.

B.7 Determination of Value.

The value of α equals to the ratio of H2O2 and Na2S2O3 mole.

(8)

B.8 Determination of β Value

The value of β can be determined by substituting two linear equation from ascending or

descending regression for max (y) to (x) so the value (x) can be obtained, which is the

experimental β value. Following are equations used.

Ascending linear

(9)

Descending linear

(10)

Subtitute equation y1 and y2 to obtain the value of x (β)

(11)




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B.9 Determination of ΔHr

The value of heat of reaction can be determined using the following formula:

(12)

B.10 Determination of Solution Density

The density of the solution can be determined using following procedure:

Determination of pycnometer volume

(13)

Determination of solution density

(14)

B.11 Determination of Degree of Reaction , Ea, dan A

Equation from linear regression that can be used to determine parameters from reaction

kinetics is

( ) . 1

ln . ln . .( )

.

s

ra b

bso o

r

dTmCp Eadt H V AR TmCp

Ca T TH V

(15)




KIN – 2018 21

APPENDIX C

SPECIFICATION AND LITERATURE DATA

C.1 Literature Data

Literature data that are needed in this experiment are:

1. Water density at various temperature

Table 8. Density of water at various temperature.

Temperature (0C) Ρwater (kg/m

3)

2. Water specific heat at various temperature

Table 9. Specific heat of water at various temperature

Temperature (0C) Cpwater

(kg/m3)

3. Reaction path of H2O2 dan Na2S2O3 which is defined by β value.

Table 10. ΔHr and β data for various reaction paths.

No Reaction β ∆H

1 2Na2S2O3 + H2O2 → Na2S4O6 + 2NaOH 0.5 -163300

2 Na2S2O3 + H2O2 → Na2S2O4 + 2 H2O 1.0 -173300

3 3Na2S2O3 + 4H2O2 → 2Na2S3O6 + 2NaOH +3H2O 1.33 -512800

4 Na2S2O3 + 4H2O2 +2NaOH→ Na2SO4 + 5H2O 4.00 -879000

5 3Na2S2O3 + 5H2O2 → 2Na2S4O6 + 2 Na2SO4 +5H2O 1.67 -432400

6 2Na2S2O3 + 4H2O2 → Na2S3O6 + 2Na2SO4 +4H2O 2.00 -596500

7 4NaOH + Na2S3O6 + 4H2O2 → 3Na2SO4 +6H2O

4. Reaction between H2O2 and KMnO4

MnO4- + 8H

+ + 5e → Mn

2+ + 4H2O

H2O2 → O2 + 2H+ + 2e

2 MnO4- + 6H

+ + 5 H2O2 → 2Mn

2+ + 8H2O + 5O2




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5. Reaction between KMnO4 and H2C2O4

MnO4- + 8H

+ + 5e → Mn

2+ + 4H2O

C2O42-

→ 2CO2 + 2e

2 MnO4- + 16H

+ + 5C2O4

2- → 2Mn

2+ + 8H2O + 10CO2

6. Rate equation between H2O2 and Na2S2O3




KIN – 2018 23

JOB SAFETY ANALYSIS

No Material Properties Countermeasures

1 Hydrogen

peroxide

(H2O2)

Odorless

Colorless

Liquid phase

in room

temperature

Strong

oxidator

Boiling point =

103 0C

Freezing point =

-15 0C

pH = 5.0 – 6.0 Density = 1,45

gr/cm3

Mr = 34.0147

gr/mol

Always wear Personal Protective

Equipment such as goggle, self-

contained breathing apparatus (if

the concentration of H2O2 exceeds

10 ppm), gloves, closed clothing

(don’t use wool, leather, or cotton),

and closed shoes.

In case of eye contact, wash with

water for 15 minutes while

blinking. Immediately seek medical

treatment because of its corrosive

properties and potency to cause

blindness.

In case of skin contact, wash skin

with water and soap. Seek aid in

case of irritation.

If swallowed, wash mouth with 1-2

glass of water. Avoid vomitting and

seek aid immediately.

If inhaled, immediately get out of

the room and get fresh air. Seek aid

in case of breathing trouble.

2 Sodium

Tiosulphate

(Na2S2O3)

crystalline

powder

White

odorless

Stable in

normal

pressure and

temperature.

Boiling point =

100 0C

Freezing point =

48 0C

pH = 6.0-8.5

Mr = 158,1

gr/mol







and closed shoes.

Keep in close containtment that is

dry and cool.



blinking. Immediately seek

medical treatment because of its

corrosive properties and potency to

cause blindness.

If swallowed, wash mouth with 1-2

glass of water. Avoid vomitting

and seek aid immediately.




3 Potassium

Permanganate

(KMnO4)

Dark Purple

Solid

Strong

Melting point =

240 0C

Density = 2,70







KIN – 2018 24

No Material Properties Countermeasures

Oxidator

Flammable

Odorless

gr/cm3

Mr = 158,0339

gr/mol




and closed shoes.

Keep in close containtment that is

dry and cool.



blinking. Immediately seek

medical treatment because of its

corrosive properties and potency to

cause blindness.

If swallowed, don’t vomit. If

conscious, immediately drink 2-4

glass of milk or mineral water. If

unconscious, don’t put anything

into the mouth, seek immediate

medical aid.




4 Water (H2O) Inflammable

Odorless

Colorless

Boiling point =

100 0C

Freezing point =

0 0C

Density = 1

gr/cm3

No specific countermeasure.

Accidents that may happen Countermeasures

Peroxide explosion due to substance being

exposed to light or heat

Keep peroxide in cool containtment, far from

light exposure, in closed containtment. Peroxide

is only taken out of the containtment if will be

directly used and immediately returned to the

containtment after use.

Accidents due to water spill Always clean working environment periodically

to prevent water puddle and check all pipe

connections and valves kept closed perfectly.

Short circuit due to electricity contact with

water

Put electric cable away from water and clean

working environtment from water that comes out

of the containtment to prevent water spill which

causes water puddle.

Equipments falling down and broken Take big shards by hand carefully, then gather in

one place. Wipe small shards to the dustbin.

Working Safety Equipment




KIN – 2018 25

Goggle Gloves Lab coat Closed shoes

Asisten Pembimbing Koordinator Lab TK

KINETIC OF LIQUID PHASE REACTION (KIN) · MODUL KINETIKA REAKSI FASA CAIR (KIN) KIN – 2018 i...

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