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UNIVERSITI PUTRA MALAYSIA EFFECTS OF LAND APPLICATION OF RAW AND COMPOSTED RECYCLED PAPER MILL SLUDGE ON Khaya senegalensis AND Orthosiphon stamineus ROSAZLIN BINTI ABDULLAH FP 2013 29
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Page 1: UNIVERSITI PUTRA MALAYSIA EFFECTS OF LAND …kertas kitar semula, pepejal takorganik dan bahan kimia tambahan yang digunakan dalam pemprosesan kertas kitar semula. Enap cemar ini adalah

UNIVERSITI PUTRA MALAYSIA

EFFECTS OF LAND APPLICATION OF RAW AND COMPOSTED RECYCLED PAPER MILL SLUDGE ON Khaya senegalensis AND Orthosiphon stamineus

ROSAZLIN BINTI ABDULLAH

FP 2013 29

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EFFECTS OF LAND APPLICATION OF RAW

AND COMPOSTED RECYCLED PAPER MILL

SLUDGE ON Khaya senegalensis AND

Orthosiphon stamineus

ROSAZLIN BINTI ABDULLAH

DOCTOR OF PHILOSOPHY

UNIVERSITI PUTRA MALAYSIA

2013

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EFFECTS OF LAND APPLICATION OF RAW AND COMPOSTED

RECYCLED PAPER MILL SLUDGE ON Khaya senegalensis AND

Orthosiphon stamineus

By

ROSAZLIN BINTI ABDULLAH

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

in Fulfilment of the Requirements for the Degree of Doctor of Philosophy

June 2013

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COPYRIGHT

All materials 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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DEDICATION

Dedicated to my parents, En. Abdullah Mohd Noh and Pn. Junidah Hamid, brothers

and sisters who has been the pillars and inspirations of my life.

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Abstract of thesis presented to the Senate of Universiti Putra

Malaysia in fulfilment of the requirement for the degree of Doctor of Philosophy

EFFECTS OF LAND APPLICATION OF RAW AND COMPOSTED

RECYCLED PAPER MILL SLUDGE ON Khaya senegalensis

AND Orthosiphon stamineus

By

ROSAZLIN BINTI ABDULLAH

June 2013

Chairman : Assoc. Prof. Che Fauziah Ishak, PhD

Faculty : Agriculture

Recycled Paper Mill Sludges (RPMS) are complex mixtures of chemically recycled

paper pulp, inorganic solid and chemical additives used in the paper manufacturing.

These sludges are the final processed wastes from pulp and paper industries which

are generated from different stages of papermaking. All paper industries produce

sludge where disposal quantity is increasing every year which if not handled

appropriately, led to environmental problem in the country. Since the usage of RPMS

is restricted in Malaysia, studies on utilization of RPMS from Malaysian industries

should be carried out to investigate the effect of RPMS on soil fertility, plant

productivity and quality. The general objective of this study was to evaluate the

effects of land application of raw and composted RPMS for agriculture and forestry

applications in agroforestry system. Paper mill sludges have alkaline pHs ranging

from 6.33 - 7.84 and thus can be important when utilized for acidic soil. Paper mill

sludges contain total organic carbon ranging from 18.92 – 33.67% and organic

matter content of 32.62 – 58.05% which can influence the biological, chemical and

physical properties of soils. Paper mill sludges contain several essential plant

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elements including N (0.31 – 4.05%), P (0.02 - 0.08%), K (0.02 - 0.42%), Ca (0.36 -

1.28%) and Mg (0.41- 1.06%). In general, the concentrations of heavy metals (Cd, Cu,

Ni, Mn, Pb and Zn) in the paper mill sludges did not exceed Class 2 of the categories

proposed by British Columbia Pulp and Paper Association (2000). The spectrum of

13C NMR obtained in this study suggested that the RPMS exhibited peaks of

cellulose and contains little lignin or hemicellulose like material. The FTIR

spectrum complemented the structural information obtained in the 13

C NMR

spectrum. Similarly, environmental contaminants of harmful chemicals such as

dioxins/furans and PAHs should not be of concern in RPMS as the levels were

negligible. Therefore, RPMS can be safely used as a fertilizer or soil amendment for

land application. Recycled paper mill sludge mixed with EFB fibres at 1:1 ratio was

recommended to be suitable for land application in agriculture and forestry. From

this study, the compost can be used as potting media and as soil conditioner enriched

with plant nutrients or as a soil amendment to improve the biological, chemical or

physical properties of a soil. Based on the potentially mineralizable N contents,

double the rates of recommended inorganic fertilizer (300 and 200 kg N-1 of raw

and RPM compost, respectively) were suggested for land application of Khaya

senegalensis and Orthosiphon stamineus. Application of raw and RPMS compost

produced higher dry matter yield and growth performance than the control

treatments for Khaya senegalensis and Orthosiphon stamineus for glasshouse and

field condition and were comparable to the inorganic fertilizer treatments. Based on

carbon fractionation study, results after 1 year duration indicated that utilization of

RPMS as organic amendment onto soil produced higher C and N contents in free

and occluded light fraction (F-LF and O-LF) and particulate organic matter (POM).

Meanwhile, the paper mill sludge application has significantly reduced the soil bulk

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density in the top soil which significantly affects the soil structure. However, the

resonance peaks of any type of C structure in the soil remained completely

unobservable even after removal of the magnetic materials followed by HF

extraction. The FTIR spectra in soil at various time of sampling exhibited the same

absorbance which indicates that no qualitative changes occurred during 6 months

and 1 year of raw and RPMS compost application compared with the control

treatments under glasshouse and field conditions. Total concentrations of Cu, Ni, Pb

and Zn in soils were below the Investigation Level for Malaysian soils which the

levels are taken at the 95th

percentile of the heavy metals data for agricultural soils.

Meanwhile, the concentrations of Cd are below the Australian Ecological

Investigation Level (EILs) of 3 mg kg-1

. Concentrations of heavy metals in leaves

were below the MPC value of the Malaysian Food Act 1983 and Food Regulation

1985. In the fractionation study, cadmium was dominant in the exchangeable

fractions. Meanwhile, Cu, Ni, Mn, Pb and Zn occurred in the residual fraction.

Application of raw and composted RPMS to soil showed an increase of

concentration of Cu, Mn, Zn, Ni, Pb and As in the leachates at 15, 30, 60 and 120

cm soil depths compared to the control in the following order, NO3- > Zn > Mn >

Cu > Ni > Pb > Cd. The concentration of NO3-, Cd, Cu, and Zn were below the

established threshold value for drinking water by World Health Organization (WHO,

2008) guideline, which is the international guideline adopted by Malaysia.

However, concentrations of Mn, Ni and Pb values were found to exceed the

threshold value of WHO (2008) regulations. Therefore, heavy metals in the

leachates need to be monitored until no more of these metals are released from the

treated soil. This study indicated that using raw RPMS with addition of EFB (1:1)

was able to improve the structure of raw RPMS as a compost product and potential

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as organic fertilizer to substitute for the inorganic N fertilizer. Hopefully, this

research can be used as preliminary information and reference on utilization of raw

and RPMS compost as soil amendment for land application especially in Malaysia.

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Abstrak tesis yang dikemukakan kepada Senat Universiti Putra Malaysia sebagai

memenuhi keperluan untuk Ijazah Doktor Falfasah

KESAN APLIKASI BAHAN MENTAH DAN KOMPOS ENAPCEMAR

KILANG KERTAS KITAR SEMULA KE ATAS TANAH,

Khaya senegalensis DAN Orthosiphon staminues

Oleh

ROSAZLIN BINTI ABDULLAH

Jun 2013

Pengerusi : Prof. Madya Che Fauziah Ishak, PhD

Fakulti : Pertanian

Enap cemar kilang kertas kitar semula (RPMS) adalah campuran komplek kimia

kertas kitar semula, pepejal takorganik dan bahan kimia tambahan yang digunakan

dalam pemprosesan kertas kitar semula. Enap cemar ini adalah bahan buangan

daripada proses akhir daripada industri pulpa dan kertas yang dihasilkan dari

pelbagai peringkat pembuatan kertas. Semua industri kilang kertas menghasilkan

enapcemar di mana kuantiti pelupusan semakin meningkat setiap tahun yang boleh

membawa kepada masalah alam sekitar di negara ini jika tidak ditangani dengan

baik. Oleh kerana penggunaan RPMS dikawal di Malaysia, maka kajian mengenai

penggunaan RPMS daripada industri Malaysia perlu dijalankan untuk menyiasat

kesan RPMS kepada kesuburan tanah, produktiviti dan kualiti tumbuhan. Objektif

am kajian ini dijalankan untuk menilai kesan aplikasi bahan mentah dan kompos

RPMS ke atas tanah untuk pertanian dan perhutanan di dalam system hutan tani.

Enap cemar kilang kertas mempunyai pH alkali antara 6.33 - 7.84, di mana ianya

penting jika digunakan pada tanah asid. Enap cemar kilang kertas mengandungi

jumlah karbon organik antara 18.92 – 33.67 % dan kandungan bahan organik antara

32.62 -58. 05% yang mungkin menyebabkan perubahan kepada sifat biologi, kimia

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dan fizikal tanah. Enap cemar kilang kertas mengandungi unsur-unsur yang

diperlukan untuk tumbuhan termasuk N (0.31 - 4.05%), P (0.02 - 0.08%), K (0.02 -

0.42%), Ca (0.36 -1.28%) dan Mg (0.41 – 1.06%). Secara umum, kepekatan logam

berat (Cd, Cu, Ni, Mn, Pb dan Zn) dalam enap cemar kilang kertas tidak melebihi

Kelas 2 dalam pengelasan yang dicadangkan oleh Persatuan Pulpa dan Kertas

British Columbia (2000). Spektrum 13

C NMR yang diperolehi dalam kajian ini

mempamirkan bahawa RPMS terdiri daripada selulosa dan mengandungi sedikit

lignin atau hemiselulosa. Spektrum FTIR melengkapi maklumat struktur yang

diperolehi dalam spektrum NMR 13

C. Begitu juga, pencemaran alam sekitar bahan

kimia berbahaya seperti dioksin / furan dan PAHs tidak harus menjadi kebimbangan

dalam penggunaan RPMS kerana arasnya dalam RPMS adalah rendah. Daripada

kajian ini, RPMS selamat diaplikasikan sebagai baja atau pemulih tanah untuk

diaplikasikan ke atas tanah. Enap cemar kilang kertas yang dicampur dengan gentian

tandan kosong kelapa sawit pada nisbah 1:1 (v/v) disyorkan sesuai untuk

diaplikasikan ke atas tanah untuk pertanian dan perhutanan. Daripada kajian ini,

kompos boleh digunakan sebagai media tanaman berpasu dan sebagai bahan

penyubur tanah atau pemulih tanah untuk meningkatkan sifat biologi, kimia atau

fizikal tanah. Berdasarkan potensi mineralisasi kandungan N, pada tahap dua kali

ganda kadar baja takorganik (300 and 200 kg N-1

bahan mentah dan kompos RPMS)

disyorkan untuk diaplikasikan ke atas tanah untuk Khaya senegalensis dan

Orthosiphon stamineus. Aplikasi bahan mentah dan kompos RPMS memberikan

hasil yang lebih tinggi dan meningkatkan pertumbuhan tanaman Khaya senegalensis

dan Orthosiphon staminues untuk keadaan di rumah kaca dan di lapangan

berbanding dengan kawalan dan setanding dengan baja takorganik. Berdasarkan

pemeringkatan karbon selepas 1 tahun kajian, penggunaan RPMS sebagai pemulih

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tanah menunjukkan peningkatan kandungan C dan N pada pemeringkatan pecahan

bebas dan terperangkap (F-LF dan O-LF) dan zarah bahan organic (POM).

Sementara itu, aplikasi bahan mentah dan kompos RPMS kilang kertas

mengurangkan ketumpatan tanah yang memberi kesan ke atas struktur tanah.

Walaubagaimanapun, tiada kehadiran resonan C dalam tanah walaupun selepas

penyingkiran bahan magnet diikuti oleh pengekstrakan HF. Spektrum FTIR dalam

tanah pada pelbagai peringkat persampelan menunjukkan bahawa tiada perubahan

kualitatif berlaku selama 6 bulan dan 1 tahun oleh bahan mentah dan RPMS kompos

berbanding kawalan pada pengeraman, rumah kaca dan kajian lapangan. Jumlah

kepekatan Cu, Ni, Mn Pb dan Zn dalam tanah adalah di bawah paras penyiasatan

untuk tanah di Malaysia yang merupakan tahap persentil ke-95 data logam berat

untuk tanah pertanian. Sementara itu, kepekatan Cd adalah di bawah paras siasatan

ekologi Australia (EILs). Kepekatan logam berat dalam daun Misai Kucing

(O.stamineus) adalah di bawah tahap yang dibenarkan (MPC) oleh akta Makanan

Malaysia 1983 dan Peraturan 1985. Dalam kajian pemeringkatan, kadmium adalah

dominan dalam dalam bentuk tukarganti. Sementara itu, Cu, Ni, Mn, Pb dan Zn

adalah dominan dalam bentuk sisa baki. Aplikasi bahan mentah dan kompos RPMS

ke atas tanah menunjukkan peningkatan kepekatan NO3-, Cd, Cu, Mn, Ni, Pb dan Zn

dalam air larutlesap pada kedalaman 15, 30, 60 dan 120 cm berbanding dengan

kawalan dengan turutan berikut, NO3-, > Zn> Mn> Cu> Ni> Pb> Cd. Kepekatan

NO3-, Cd, Cu, dan Zn adalah di bawah paras nilai garispaduan untuk air minuman

oleh Pertubuhan Kesihatan Sedunia (WHO, 2008), di mana ia adalah garispanduan

antarabangsa yang digunapakai oleh Malaysia. Walaubagaimanapun, kepekatan Mn,

Ni, dan Pb di dapati melebihi daripada nilai garispanduan WHO (2008). Oleh itu,

larutlesap logam berat hendaklah di beri perhatian sehingga tiada lagi logam yang

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dilarutlesap dari tanah yang diberi rawatan. Kajian ini menunjukkan penggunaan

bahan mentah RPMS dengan tambahan EFB (1:1) mampu memperbaiki struktur

bahan mentah sebagai produk kompos dan berpotensi sebagai baja kimia untuk

menggantikan baja N takorganik N. Adalah diharapkan agar kajian ini boleh

membekalkan maklumat dan digunakan sebagai rujukan awal mengenai penggunaan

bahan mentah dan kompos RPMS sebagai bahan pemulih untuk diaplikasikan ke

atas tanah, terutamanya, di Malaysia.

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ACKNOWLEDGEMENTS

In the name of Allah, the Most Gracious and the Most Merciful

Alhamdulillah, all praises to almighty Allah for the strength and His blessing in

completing this thesis. Special appreciation goes to my supervisor, Assoc. Prof. Dr.

Che Fauziah Ishak for her invaluable guidance, constructive comment and constant

support throughout the experimental and thesis works. My appreciations also go to

my supervisory committee members; Prof. Datin Dr. Rosenani Abu Bakar and Dr.

Wan Rasidah Abdul Kadir.

I would like to express my gratitude to all the laboratory technicians and staffs at the

Faculty of Agriculture, UPM and staff at the Soil Chemistry Laboratory (MKT),

FRIM for their co-operations during my laboratory and field studies.

As for Cik Noor Hazlyna Din, Tai Kin Leong, Supian Manan, Aini Azura, Jariani

Jani, Haley, Rozita Osman and Neni Kartini, heartiest thanks for their

encouragements and support. Those who either directly or indirectly contributed in

this study, your kindness are very much appreciated.

Last but not least, I would also like to thank the Ministry of Higher Education

(MOHE), University of Malaya and Universiti Putra Malaysia, for the financial

support given which makes my study possible.

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APPROVAL

I certify that a Thesis Examination Committee has met on 28 June 2013 to conduct

the final examination of Rosazlin Binti Abdullah on her thesis entitled “Effects of

Land Application of Raw and Composted Recycled Paper Mill Sludge on Khaya

Senegalensis and Orthosiphon Stamineus” in accordance with the Universities and

University College 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 Doctor of Philosophy.

Members of the Thesis Examination Committee were as follows:

Shamshuddin Jusop, PhD

Professor

Faculty of Agriculture

Universiti Putra Malaysia

(Chairman)

Aminuddin Husin, PhD

Associate Professor

Faculty of Agriculture

Universiti Putra Malaysia

(Internal Examiner)

Ahmad Husni Mohd. Hanif, PhD

Associate Professor

Faculty of Agriculture

Universiti Putra Malaysia

(Internal Examiner)

Dar-Yuan Lee, PhD

Professor

National Taiwan University

(External Examiner)

_____________________

NORITAH OMAR, PhD

Assoc. Professor and Deputy Dean

School of Graduate Studies

Universiti Putra Malaysia

Date: 16 August 2013

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

accepted as fulfillment of the requirement for the Degree of Doctor of Philosophy.

The members of the Supervisory Committee were as follows:

Che Fauziah Ishak, PhD

Associate Professor

Faculty of Agriculture

Universiti Putra Malaysia

(Chairman)

Rosenani Abu Bakar, PhD

Professor

Faculty of Agriculture

Universiti Putra Malaysia

(Member)

Wan Rasidah Abdul Kadir, PhD

Researcher

Forest Research Institute of Malaysia

(Member)

_____________________________

BUJANG BIN KIM HUAT, PhD

Professor and Dean

School of Graduate Studies

Universiti Putra Malaysia

Date:

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DECLARATION

Declaration by graduate student

I hereby confirm that:

this thesis is my original work;

quotations, illustrations and citations have been duly referenced;

this thesis has not been submitted previously or concurrently for any other degree

at any other institutions;

intellectual property from the thesis and copyright of thesis are fully-owned by

Universiti Putra Malaysia, as according to the Universiti Putra Malaysia

(Research) Rules 2012;

written permission must be obtained from supervisor and the office of Deputy

Vice-Chancellor (Research and Innovation) before thesis is published (in the form

of written, printed or in electronic form) including books, journals, modules,

proceedings, popular writings, seminar papers, manuscripts, posters, reports,

lecture notes, learning modules or any other materials as stated in the Universiti

Putra Malaysia (Research) Rules 2012;

there is no plagiarism or data falsification/fabrication in the thesis, and scholarly

integrity is upheld as according to the Universiti Putra Malaysia (Graduate

Studies) Rules 2003 (Revision 2012-2013) and the Universiti Putra Malaysia

(Research) Rules 2012. The thesis has undergone plagiarism detection software.

Signature: __________________ Date: 28 June 2013

Name and Matric No.: ROSAZLIN BINTI ABDULLAH (GS20977)

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TABLE OF CONTENTS

Page

ABSTRACT ii

ABSTRAK vi

ACKNOWLEDGEMENTS x

APPROVAL xi

DECLARATION xiii

LIST OF TABLES xx

LIST OF TABLES xxiii

LIST OF PLATES xxvi

LIST OF ABBREVIATIONS xxvii

CHAPTER

1 INTRODUCTION 1

1.1 Background 1

1.2 Objectives 6

1.3 Hypothesis 6

2 LITERATURE REVIEW 7

2.1 Paper Mill Industry 7

2.2 Recycled Paper Mill Sludge Generation 7

2.2.1 Recycled Paper Mill Sludge Properties 9

2.2.2 Recycled Paper Mill Sludge Management 10

2.2.3 Land Application of Recycled Paper Mill Sludge 10

2.2.4 Benefit of Recycled Paper Mill Sludge Utilization in

Agriculture

12

2.2.5 Composted Recycled Paper Mill Sludge 13

2.3 Nitrogen Mineralization in Soil 15

2.3.1 Soil N Mineralization Potential 16

2.3.2 Factors Affecting Soil N mineralization 17

2.3.3 Nitrogen Losses During Decomposition 18

2.4 Soil Organic Matter 19

2.4.1 Methods of Soil Organic Matter Characterization 22

2.4.1.1 Soil Organic Matter Fractions 22

2.4.1.2 Nuclear Magnetic Resonance (NMR)

Spectroscopy

23

2.4.1.3 Fourier Transform-Infrared (FTIR) Spectroscopy 27

2.5 Potential Contamination of Paper Mill Sludge 29

2.5.1 Heavy Metals 29

2.5.1.1 Factors Affecting Accumulation of Heavy Metals

in Soil

30

2.5.1.2 Heavy Metals in Recycled Paper Mill Sludge 31

2.5.1.3 Heavy Metals Fractionation 33

2.5.1.4 Leaching of Heavy Metals 36

2.5.2 Organic Contaminants 37

2.6 Agroforestry 38

2.6.1 Khaya senegalensis 39

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2.6.2 Orthosiphon stamineus 40

3 GENERAL MATERIALS AND METHODS 42

3.1 Introduction 42

3.2 Materials 42

3.2.1 Recycled Paper Mill Sludge 42

3.2.2 Oil Palm Empty Fruit Bunches 42

3.2.3 Recycled Paper Mill Sludge Compost 43

3.2.4 Soil 43

3.3 Methods 43

3.3.1 Determination of Moisture Content 43

3.3.2 Determination of pH 44

3.3.3 Determination of Electrical Conductivity (EC) 44

3.3.4 Determination of Total Nitrogen (Kjedahl Method) 44

3.3.5 Determination of Total Organic Carbon 45

3.3.6 Determination of Available Phosphorous 45

3.3.7 Determination of Exchangable Bases and Cation Exchange

Capacity (CEC)

45

3.3.8 Determination of Particle Size Distribution (Texture) 46

3.3.9 Bulk Density Analysis 46

3.3.10 13

C NMR Analysis 46

3.3.11 FTIR Spectroscopy Analysis 47

3.3.12 Determination of Total Heavy Metals in RPMS and Soil 48

3.3.13 Determination of Available Heavy Metals in Soil 49

3.3.14 Physical Fractionation for C (Density and Particle Size

Fractionation)

49

3.3.15 Sequential Extraction Methods 52

3.3.15.1 Water Soluble Fraction 52

3.3.15.2 Exchangeable Fraction 52

3.3.15.3 Carbonate Fraction 53

3.3.15.4 Fe-Mn Fraction 53

3.3.15.5 Organic Fraction 53

3.3.15.6 Residual Fraction 54

3.4 Preparations and Analyses of Plant Samples 56

3.4.1 Determination of Total Heavy Metals (Dry Ashing Method) 56

3.4.2 Determination Total Nitrogen (Kjedahl Method) 57

4 STUDY 1: CHARACTERIZATION OF RECYCLED PAPER MILL

SLUDGES FROM VARIOUS PAPER MILLS

58

4.1 Introduction 58

4.2 Materials 59

4.2.1 Recycled Paper Mill Sludge Sampling 59

4.3 Methods 60

4.3.1 Physical and Chemical Characteristics of Paper Mill Sludges 61

4.3.2 Analytical Procedure for PAHs 61

4.3.3 Analytical Procedure for Dioxin/Furan 63

4.4 Results and Discussion 64

4.4.1 Physico-chemical Characteristics of Paper Mill Sludges 64

4.4.2 13

C NMR spectra of Paper Mill Sludges 69

4.4.3 FTIR Spectra of Paper Mill Sludges 71

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4.4.4 Heavy Metals Concentrations of Paper Mill Sludges 72

4.4.5 Organic Contaminants 76

4.4.5.1 Polycyclic Aromatic Hydrocarbon (PAHs) 76

4.4.5.2 Dioxins and Furans 78

4.5 Conclusion 78

5 STUDY 2: COMPOSTING OF RECYCELD PAPER MILL SLUDGE

MIXED WITH OIL PALM EMPTY FRUIT BUNCHES

80

5.1 Introduction 80

5.2 Materials and Methods 81

5.2.1 Recycled Paper Mill Sludge, Shredded Empty Fruit Bunches ,

Beneficial Effective Microorganism and Molasses

81

5.2.2 Experimental Design and Treatment 82

5.2.3 Compost Analysis 83

5.2.4 Test for Phytotoxicity of Composts 84

5.2.4.1 Germination Test 84

5.2.4.2 Potting Media Test 85

5.2.5 Statistical Analysis 85

5.3 Results and Discussion 85

5.3.1 Characteristics of Raw Recycled Paper Mill Sludge and

Shredded Empty Fruit Bunches

85

5.3.2 Characteristics of Compost Pile during Composting 87

5.3.3 Characteristics of RPMS Compost 91

5.3.4 Phytotoxicity Test 93

5.3.5 13

C NMR Spectra of Composted Paper Mill Sludge 96

5.3.6 FTIR Spectrum of Composted Paper Mill Sludge 97

5.4 Conclusion 98

6 STUDY 3: NITROGEN MINERALIZATION IN SOILS INCUBATED

WITH COMPOSTED AND RAW PAPER MILL SLUDGE

100

6.1 Introduction 100

6.2 Materials and Methods 101

6.2.1 Laboratory Experiment 101

6.2.2 Field Experiment 102

6.2.3 Chemical Analyses 102

6.2.4 Statistical Analyses 103

6.3 Results and Discussion 103

6.3.1 Nitrogen Mineralization (Incubation Experiment) 103

6.4 Conclusion 109

7 STUDY 4: EFFECTS OF LAND APPLICATION OF RAW AND

COMPOSTED RECYCLED PAPER MILL SLUDGE

APPLICATION ON Khaya senegalensis AND Orthosiphon

Stamineus UNDER GLASSHOUSE CONDITION

111

7.1 Introduction 111

7.2 Materials and Methods 113

7.2.1 Location, Soil and Treatment 113

7.2.2 Application of Raw and RPMS compost and Fertilizer 115

7.2.3 Crop Maintenance 116

7.2.4 Measurement of Growth Parameters At Harvest 116

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7.2.4.1 Khaya senegalensis 116

7.2.4.2 Orthosiphon. stamineus 117

7.2.5 Soil sampling 117

7.2.6 Physical Fractionation for C (Density and Particle Size

Fractionation)

117

7.2.7 Sequential Extraction Methods 118

7.2.8 Statistical Analyses 118

7.3 Results and Discussion 118

7.3.1 Growth Performance 118

7.3.2 Soil Properties in the Soil 123

7.3.3 Concentration of Macronutrient in the Soil 125

7.3.4 Physical Fractionation for C 127

7.3.4.1 Free and Occluded Light Fractions of Carbon and

Nitrogen Concentration

127

7.3.4.2 Particulate Organic Matter (POM) of Carbon and

Nitrogen Concentration

129

7.3.4.3 Soil Dry Matter Present in the Different Size

Obtained by the Physical Fractionations

129

7.3.5 Changes of soil organic matter content by 13

C NMR 132

7.3.6 Changes of soil organic matter content by FTIR 133

7.3.7 Heavy Metals in Soil 133

7.3.8 Available Heavy Metals in Soil 135

7.3.9 Effect on Nitrogen Concentration and Content in Plant Parts 136

7.3.10 Concentration of Heavy Metals in Plant Parts 138

7.3.11 Concentrations of Heavy Metals in Leaves (Based on Fresh

Weight)

140

7.3.12 Effect on Uptake Heavy Metals in Plant Parts 141

7.3.13 Correlation between Total and Available Heavy Metals in Soil

with Soil Chemical Properties and Plants Parts

144

7.3.14 Fractionation Study 148

7.3.14.1 Fractionation of Heavy Metals in Raw and RPMS

Compost

148

7.3.14.2 Fractionation of Heavy Metals in Soil after One

Year Application of Raw and RPMS Compost

150

7.3.14.3 Correlation between Heavy Metals Fractions in

Soil with Plant Parts

154

7.4 Conclusion 156

8 STUDY 5: EFFECTS OF LAND APPLICATION OF RAW AND

COMPOSTED RECYCLED PAPER MILL SLUDGE

APPLICATION ON Khaya senegalensis AND Orthosiphon

Stamineus UNDER FIELD CONDITION

157

8.1 Introduction 157

8.2 Materials and Methods 158

8.2.1 Location, Soil and Treatment and Climate (Agroforestry

System)

158

8.2.2 Application of Raw and RPMS compost and Fertilizer 161

8.2.3 Crop Maintenance 162

8.2.4 Measurement of Growth Parameters At Harvest 162

8.2.4.1 Khaya senegalensis 162

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8.2.4.2 Orthosiphon. stamineus 163

8.2.5 Soil sampling 164

8.2.6 Nitrogen Mineralization/Immobilization 164

8.2.7 Physical Fractionation for C (Density and Particle Size

Fractionation)

165

8.2.8 Sequential Extraction Methods 165

8.2.9 Leaching Experiment 165

8.2.9.1 Treatment and Sampling 165

8.2.9.2 Laboratory Analysis 166

8.2.10 Statistical Analyses 166

8.3 Results and Discussion 167

8.3.1 Growth Performance 167

8.3.2 Soil Properties in the Soil 173

8.3.3 Macronutrient in the Soil 176

8.3.4 Nitrogen Mineralization/Immobilization 178

8.3.5 Physical Fractionation for C 182

8.3.5.1 Free and Occluded Light Fractions of Carbon and

Nitrogen Concentration

182

8.3.5.2 Particulate Organic Matter (POM) of Carbon and

Nitrogen Concentration

183

8.3.5.3 Soil Dry Matter Present in the Different Size

Obtained by the Physical Fractionations

184

8.3.6 Changes of soil organic matter content by 13

C NMR 189

8.3.7 Changes of soil organic matter content by FTIR 190

8.3.8 Heavy Metals in Soil 190

8.3.9 Available Heavy Metals in Soil 193

8.3.10 Nitrogen Concentration and Content in Plant Parts 195

8.3.11 Concentration of Heavy Metals in Plant Parts 196

8.3.12 Concentrations of Heavy Metals in Leaves (Based on Fresh

Weight)

199

8.3.13 Effect on Uptake Heavy Metals in Plant Parts 199

8.3.14 Correlation between Total and Available Heavy Metals in Soil

with Soil Chemical Properties and Plants Parts

201

8.3.15 Fractionation Study

8.3.15.1 Fractionation of Heavy Metals in Soil After

Application of Raw and RPMS Compost

204

8.3.15.2 Correlation between Heavy Metals Fractions in

Soil with Plant Parts

208

8.3.16 Leaching of Nitrate-N and Heavy Metals after One Year

Application of Raw and Composted Recycled Paper Mill

Sludge

210

8.3.16.1 Concentrations of Nitrate in the Leachates 210

8.3.16.2 Concentrations of Cadmium in the Leachates 211

8.3.16.3 Concentrations of Copper in the Leachates 212

8.3.16.4 Concentrations of Nickel in the Leachates 213

8.3.16.5 Concentrations of Manganese in the Leachates 214

8.3.16.6 Concentrations of Lead in the Leachates 215

8.3.16.7 Concentrations Zinc in the Leachates 216

8.4 Conclusion 217

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9 GENERAL DISCUSSION ON GLASSHOUSE AND FIELD STUDY 219

9.1 Growth Performance of Khaya senegalensis and Orthosiphon

Stamineus after Land Application of Raw And Composted RPMS

219

9.2 Soil Accumulation and Plant Uptake after Land Application of Raw

And Composted RPMS

221

9.3 Physical Fractionation for C, NMR and FTIR in Soil after Land

Application of Raw And Composted RPMS

222

9.4 Heavy metals Uptake after Land Application of Raw And Composted

RPMS

224

10 CONCLUSION AND RECOMMENDATIONS 231

REFERENCES 238

BIODATA OF STUDENT 256

LIST OF PUBLICTIONS, AWARD AND PATENT 257


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