universiti putra malaysia muhammad hazwan bin hamzah fk 2013

UNIVERSITI PUTRA MALAYSIA

MUHAMMAD HAZWAN BIN HAMZAH

FK 2013 74

OPTIMIZATION AND KINETICS OF CITRONELLA OIL EXTRACTION BY OHMIC HEATED HYDRO DISTILLATION

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OPTIMIZATION AND KINETICS OF CITRONELLA OIL EXTRACTION

BY OHMIC HEATED HYDRO DISTILLATION

By


Thesis Submitted to the School of Graduate Studies, Universiti Putra Malaysia,

in Fulfilment of the Requirements for the Degree of Master of Science

June 2013

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All material contained within the thesis, including without limitation text, logos,

icons, photographs and all other artwork, is copyright material of Universiti Putra

Malaysia unless otherwise stated. Use may be made of any material contained within

the thesis for non-commercial purposes from the copyright holder. Commercial use of

material may only be made with the express, prior, written permission of Universiti

Putra Malaysia.

Copyright © Universiti Putra Malaysia

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Abstract of thesis presented to the Senate of Universiti Putra Malaysia in fulfilment of

the requirement for the degree of Master of Science

OPTIMIZATION AND KINETICS OF CITRONELLA OIL EXTRACTION

BY OHMIC HEATED HYDRO DISTILLATION

By


June 2013

Chair: Associate Professor Hasfalina Che Man, PhD

Faculty: Engineering

Citronella grass is an aromatic plant with a variety of applications and tremendous

economic potentials. The essential oil from the citronella grass has a variety of uses

such as in traditional medication, perfume industry and soap manufacturing. A

proposed method for citronella oil extractionwas developed with the application of

ohmic heated hydrodistillation. The main objective of this research was to determine

the parameters of the citronella oil extraction to achieve maximum oil yield by ohmic

heated hydro distillation. The parameters affecting citronella oilextraction by ohmic

heated hydro distillation such as powerinput, extraction time, solvent to solid ratio

and crushing frequency were investigated.The optimum parameters were found at a

power input of 77 V up to the boiling point of water and followed by 50 V until the

end of extraction, 2 hours extraction time, a solvent to solid ratio of 3:1 and a

crushing frequency of once. The optimized parameters were then applied to hydro

distillation and steam distillation. Thekinetics of extraction was proposed and

validated based on asecond-order model.The maximum amount of yield of optimized

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parameters in kinetic study by ohmic heated hydro distillation was 7.64 mL/kWh in

comparison with hydro distillation and steam distillation methods that resulted oil

yield 3.87 mL/kWh and 1.69 mL/kWh, respectively. The proposed model fitted well

with the experimental data showed that the coefficient of determination, R2 more than

0.97. The chemical, physical and biological properties of citronella oil and leaves

extracted using three different extraction methods were also determined. Gas

chromatography-mass spectrometry analysis found that the major constituents of

citronella oil for the different extraction methods were citronellal, citronellol and

geraniol. The results for specific gravity and refractive index at 20 °C were ranged

from 0.8879 to 0.8916 and 1.4671 to 1.4743, respectively. The citronella oil colour

intensity in terms of red and yellow units was 2.0 Y to 0.7R 4Y. Scanning electron

micrographs of citronella grass showed some microfractures and cell wall became less

rigidity for ohmic heated hydro distillation. Results of this research revealed that

ohmic heated hydro distillation could be introduced as an alternative technology to

conventional methods.

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Abstrak tesis yang dikemukakan kepada Senat Universiti Putra Malaysia sebagai

memenuhi keperluan untuk ijazah Master Sains

PENGOPTIMUMAN DAN KINETIK PENGEKSTRAKAN MINYAK SERAI

WANGI OLEH PENYULINGAN HIDRO PEMANASAN OHMIK

Oleh


Jun 2013

Pengerusi: Profesor Madya Hasfalina Che Man, PhD

Fakulti: Kejuruteraan

Serai wangi adalah tumbuhan beraroma yang mempunyai pelbagai aplikasi dan

potensi ekonomi yang besar.Minyak serai wangi mempunyai pelbagai kegunaan

seperti digunakan dalam ubat tradisional, industri minyak wangi dan pembuatan

sabun.Satu cadangan kaedah pengekstrakan minyak serai wangi telah dibangunkan

dengan menggunakan penyulingan hidro pemanasan ohmik.Objektif utama

penyelidikan ini adalah bertujuan menentukan parameter pengekstrakan minyak serai

wangi untuk mendapatkan hasil minyak yang maksimum melalui penyulingan hidro

pemanasan ohmik. Parameter yang mempengaruhi pengekstrakan minyak serai wangi

oleh penyulingan hidro pemanasan ohmik adalah seperti input kuasa, masa

pengekstrakan, nisbah pelarut kepada pepejal dan frekeunsi menghancur telah dikaji.

Parameter optimum ditemui pada input kuasa 77 V sehingga takat didih air dan diikuti

dengan 50 V sehingga akhir pengekstrakan, masa pengekstrakan selama 2 jam, nisbah

pelarut kepada pepejal sebanyak 3:1 dan sekali frekuensi menghancur. Parameter

optimum kemudiannya diaplikasikan dalam penyulingan hidro dan penyulingan wap.

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Kinetik pengekstrakan telah dicadangkan dan disahkan berdasarkan model tertib

kedua. Jumlah hasil maksimum pada parameter optimum bagi kajian kinetik oleh

penyulingan hidro pemanasan ohmik ialah 7.64 mL/kWj berbanding dengan kaedah

penyulingan hidro dan penyulingan stim yang menghasilkan masing-masing 3.87

mL/kWj dan 1.69 mL/kWj. Model yang dicadangkan disesuaikan baik dengan data

eksperimen menunjukkan pekali penentuan, R2 lebih daripada 0.97.Sifat kimia, fizikal

dan biologi minyak dan daun serai wangi dengan menggunakan tiga kaedah

pengekstrakan berbeza juga ditentukan. Analisis gas kromatografi-jisim spektrometri

menunjukkan juzuk utama kandungan minyak serai wangi untuk kaedah

pengekstrakan berbeza iaitu citronellal, citronellol dan geraniol. Keputusan bagi

graviti spesifik (20 °C) dan indeks biasan (nD 20 °C) masing-masing antara 0.8879

hingga 0.8916 g/mL dan 1.4671 hingga 1.4743. Keamatan warna minyak serai wangi

daripada segi unit merah dan kuning adalah 2.0 K hingga 0.7M 4K.Imbasan

mikrograf elektron serai wangi menunjukkan sedikit pecahan mikro dan menjadikan

dinding sel kurang kukuh untuk penyulingan hidro pemanasan ohmik.Keputusan

penyelidikan ini membuktikan bahawa penyulingan hidro pemanasan ohmik boleh

diperkenal sebagai teknologi alternatif kepada kaedah konvensional.

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ACKNOWLEDGEMENTS

In the name of Allah, most Gracious, most Compassionate. Thanks to Allah for giving

me the courage, patience and confidence in order to complete this report.

First and foremost, a very special thanks and appreciation to my supervisory

committee Assoc. Prof. Dr. Hasfalina Che Man, Assoc. Prof. Dr. Zurina Zainal

Abidin and Mr. Hishamuddin Jamaludin for giving me the opportunity to work under

their supervision, their valuable time, guidance and consultation throughout this

project.

I would also like to thank Ministry of Higher Education Malaysia for providing the

Research University Grant Scheme (RUGS) grant and supporting this project number

(RUGS/05-01-12-1633RU).

Not forgetting respective colleagues for their kind help and moral supports in doing

this project. I also would like to kindly thank all those who helped me including

laboratory technician with their valuable support during my research to accomplish

my master’s thesis. Last but not least, to my beloved family, thank you for your

support and concern, and giving me the strength to complete this challenging project.

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I certify that a Thesis Examination Committee has met on 4 June 2013 to conduct the

final examination of Muhammad Hazwan bin Hamzah on his thesis entitled

“Optimization and Kinetics of Citronella Oil Extraction by Ohmic Heated Hydro

Distillation” in accordance with the Universities and University Colleges Act 1971

and the Constitution of the Universiti Putra Malaysia [P.U.(A) 106] 15 March 1998.

The Committee recommends that the student be awarded the Master of Science.

Members of the Thesis Examination Committee were as follows:

Desa bin Ahmad, PhD

Professor Ir.

Faculty of Engineering

Universiti Putra Malaysia

(Chairman)

Jamarei bin Othman, PhD

Senior Lecturer



(Internal Examiner)

Shafreeza binti Sobri, PhD

Senior Lecturer



(Internal Examiner)

Mashitah Mat Don, PhD

Associate Professor

Universiti Sains Malaysia

(External Examiner)

_______________________________

NORITAH OMAR, PhD

Professor and Deputy Dean

School of Graduate Studies


Date: 2 August 2013

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This thesis was submitted to the Senate of Universiti Putra Malaysia and has been

accepted as fulfilment of the requirement for the degree of Master of Science. The

members of the Supervisory Committee were as follows:

Hasfalina Che Man, PhD

Associate Professor



(Chairman)

Zurina Zainal Abidin, PhD

Associate Professor



(Member)

Hishamuddin Jamaludin

Senior Lecturer

Food Technology Section

Universiti Kuala Lumpur

Malaysian Institute of Chemical and Bioengineering Technology

(Member)

_______________________________

BUJANG BIN KIM HUAT, PhD

Professor and Dean

School of Graduate Studies


Date:

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DECLARATION

I declare that the thesis is my original work except for quotations and citations which

have been duly acknowledged. I also declare that it has not been previously, and is not

concurrently, submitted for any other degree at Universiti Putra Malaysia or at any

other institution.

_______________________________________


Date: 4 June 2013

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TABLE OF CONTENTS

Page

ABSTRACT iii

ABSTRAK v

ACKNOWLEDGEMENTS vii

APPROVAL viii

DECLARATION x

LIST OF TABLES xiii

LIST OF FIGURES xiv

CHAPTER

1 INTRODUCTION 1

1.1 Background 1

1.2 Problem Statements 2

1.3 Objectives 4

1.4 Scope of the Study 4

1.5 Overview of the Thesis 5

2 LITERATURE REVIEW 6

2.1 Introduction 6

2.1.1 Citronella 6

2.2 Citronella Oil Extraction 9

2.2.1 Hydro Distillation 12

2.2.2 Ohmic Heated Hydro Distillation 14

2.2.3 Steam Distillation 17

2.3 Kinetic Study 19

2.4 Summary of the Literature Review 20

3 MATERIALS AND METHOD 22

3.1 Flow Diagram of Citronella Oil Extraction Steps 22

3.2 Raw Material Preparation 23

3.3 Set Up of Ohmic Heated Hydro Distillation 23

3.3.1 Optimization of Ohmic Heated Hydro Distillation of

Citronella Grass

25


3.4.1 Hydro Distillation 27

3.4.2 Steam Distillation 27

3.5 Citronella Oil and Citronella Grass Analysis 28

3.5.1 Oil Yield Determination 28

3.5.2 Chemical Analysis 29

3.5.3 Physical Analysis 30

3.5.4 Biological Analysis 30

4 RESULTS AND DISCUSSION 31

4.1 Optimization of Ohmic Heated Hydro Distillation of

Citronella Grass

31

4.1.1 Effect of Power Input 31

4.1.2 Effect of Extraction Time 33

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4.1.3 Effect of Solvent to Solid Ratio 34

4.1.4 Effect of Crushing Frequency 36


4.2.1 Proposed Model 38

4.2.2 Model Analysis 41

4.2.3 Model Validation 46

4.3 Chemical Analysis 46

4.4 Physical Analysis 51

4.5 Biological Analysis 53

5 CONCLUSION AND RECOMMENDATIONS 57

5.1 Conclusion 57

5.2 Recommendations 58

REFERENCES 60

APPENDICES 71

BIODATA OF STUDENT 79

LIST OF PUBLICATIONS 80

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universiti putra malaysia muhammad hazwan bin hamzah fk 2013