PHYSICO-CHEMICAL AND MICROSTRUCTURE OF ARTIFICIAL … · Kebolehkesanan campuran kapur zeolit telah...

PHYSICO-CHEMICAL AND MICROSTRUCTURE OF ARTIFICIAL SOILS

STABILISED WITH LIME-ZEOLITE

FELIX LING NGEE LEH

A thesis submitted in fulfilment of the

requirements for the award of the degree of

Doctor of Philosophy (Civil Engineering)

Faculty of Civil Engineering

Universiti Teknologi Malaysia

FEBRUARY 2016

iii

To my beloved father, mother, wife, daughters and siblings

iv

ACKNOWLEDGEMENT

This project will not be successful without the support from those who have

directly and indirectly helped me along the path. I am very grateful and would like to

convey my gratitude to every single one who has made this thesis possible.

Firstly, I would like to express my gratitude to Prof. Dr. Khairul Anuar bin

Kassim as my supervisor to this study. I would like to thank him for his inspire

guidance throughout the whole process of this project.

Secondly, specially thank to my co-supervisor Prof. Dr. Ahmad Tarmizi bin

Abdul Karim for his advices and guidance. Very appreciate to him for sharing his

experiences and knowledge in this project.

Thirdly, I would like to thank my superior Prof. Dato’ Dr. Ismail bin Bakar,

Head of Research Centre for Soft Soil (RECESS), UTHM for his support and help.

I would also like to thank all the technical staffs in the Geotechnical

Laboratory of FKA, UTM; Research Centre for Soft Soil (RECESS), UTHM; Ibnu

Sina, UTM, Materials Science Lab, FKM, UTM; Materials Science Lab, FKMP,

UTHM; Polymer Lab, FKKSA, UTM; Polymer Lab, FKMP, UTHM; Analytical Lab,

FKAAS, UTHM; Wastewater Lab, FKAAS, UTHM and others who had helped me a

lot during my experimental work.

Lastly, I would like to thank my parents, wife and two daughters who have

given me strong moral support throughout the study. Without them, I doubt that I

would have the chance to complete my research.

v

ABSTRACT

The chemical stabilisation by admixing soil with lime is widely used in soft soil stabilization but its effectiveness in organic soil is low. Studies have shown that besides the organic content, the type of organic matter also influences the effectiveness of lime stabilisation. Artificial soils were utilized in this study to minimize potential influential factors that may be affected by the geochemistry variability of natural organic soils. Two types of organic matter, namely organic acid (contains humic acid and fulvic acid) and coco peat were utilized to simulate humified and non-humified organic matters that are normally found in natural organic soils. Commercially processed kaolin with different fineness and nSi/nAl were chosen as the base soil. The base soil and organic matter were manually mixed in different ratios based on their dry unit weight. Lime was partially replaced with zeolite with the aim to produce additive with self cementing matrix. The effectiveness of blended lime zeolite was investigated in this study. The total amounts of additives ranged from 7.5% to 15% were utilized based on the results of the Initial Consumption of Lime (ICL). Half of the remoulded test specimens were cured with a constant temperature of 50°C in an oven while the other part of the samples was cured at room temperature. The curing periods were set as 7, 28 and 56 days before being tested for unconfined compressive strength. Strength is utilized to determine the effectiveness of additives in stabilising artificial soils. The morphology of the stabilised and unstabilised materials was examined using a Field Emission Scanning Electron Microscope (FESEM), while the mineralogy of the materials was determined using X-Ray Diffraction (XRD) in order to unveil the hardening mechanisms of stabilised soils. General Linear Model (GLM) was utilized to determine the significant main factors, and interactions factors on the strength of artificial soil. The significant factors were used as the input parameters for multiple regression analysis to develop the strength prediction model. The models were utilised to predict the strength of stabilised materials within the inference space defined by the experiment. Overall, the mixture of coco peat and organic acid showed a deleterious effect on the strength of lime-zeolite stabilised artificial soils by lowering the soil’s pH and increasing its porosity. However, the results of the organic acid samples with different pH and cured in different curing temperature were inconsistent. The availability of needle-like structures or Calcium Silicate Hydrate (C-S-H) phase was used as an indicator of successful in the cementation process without being inhibited by organic matter. The 20% replacement of lime with zeolite was found to achieve the highest strength when used to stabilise artificial soils with 30% of organic acid under a laboratory environment. A 20% replacement of lime with zeolite was found to experience only a slight decrease in pH and was able to enrich the elemental properties of lime with silica and alumina, which are important for producing a cementing matrix in an alkaline environment.

vi

ABSTRAK

Penstabilan kimia dengan kapur telah digunakan secara meluas dalam penstabilan tanah lembut tetapi keberkesanannya adalah rendah untuk tanah organik. Keberkesanan penstabilan kapur dipengaruhi oleh kandungan organik dan jenis bahan organik. Tanah tiruan yang digunakan dalam kajian ini bertujuan mengurangkan faktor pengaruh yang berpunca daripada sifat kepelbagaian geokimia tanah organik semulajadi. Dua jenis bahan organik, iaitu asid organik (asid humic dan asid fulvic) dan gambut kelapa digunakan sebagai pengganti bahan organik terurai dan tidak terurai yang lazim ditemui dalam tanah organik semulajadi. Kaolin komersial yang mempunyai kehalusan dan nilai nSi/nAl yang berbeza telah dipilih sebagai tanah asas. Tanah asas dan bahan organik telah dicampur secara manual pada nisbah yang berlainan berdasarkan kepada unit berat kering. Sebahagian kapur adalah digantikan dengan zeolit untuk menghasilkan bahan campuran yang mempunyai matriks pensimenan sendiri. Kebolehkesanan campuran kapur zeolit telah dikaji dalam kajian ini. Jumlah bahan campuran yang digunakan adalah dalam lingkungan 7.5% kepada 15% bergantung kepada Kadar Penggunaan Kapur (ICL). Separuh daripada spesimen yang dibentuk semula akan dirawat dalam ketuhar pada suhu 50°C. Manakala sebahagian lagi dirawatkan pada suhu bilik. Tempoh rawatan sampel adalah ditetapkan pada 7, 28 dan 56 hari sebelum diuji untuk menentukan kekuatan tak terkurung. Kekuatan digunakan sebagai penentu keberkesanan bahan pencampur dalam menstabilkan tanah tiruan. Morfologi bahan distabil atau tidak distabil telah diuji menggunakan alat Pelepasan Imbasan Mikroskop Elektron (FESEM), manakala mineralogi bahan telah dikaji menggunakan kaedah Pembelauan Sinar-X (XRD) untuk mengenali mekanisma pengerasan tanah. Model Linear Umum (GLM) telah digunakan bagi menentukan kesesuaian faktor-faktor utama, dan interaksinya sebagai parameter masukan untuk analisis regresi berganda bagi membangunkan model ramalan kekuatan yang boleh digunakan untuk meramal kekuatan bahan stabil dalam ruang inferens yang ditakrifkan oleh ujikaji. Secara amnya, campuran gambut kelapa dan asid organik telah menunjukkan kesan negatif ke atas kekuatan tanah tiruan dengan menurunkan pH dan meningkatkan keliangan. Namun demikian, kesan asid organik ke atas kekuatan tanah tiruan adalah tidak konsisten untuk nilai pH campuran dan suhu rawat yang berbeza. Penemuan struktur berbentuk jarum atau fasa Kalsium Silika Hidrat (C-S-H) digunakan sebagai penanda kejayaan proses pensimenan tanpa diberhentikan oleh bahan organik. Penukaran 20% kapur dengan zeolit didapati mencapai kekuatan paling tinggi apabila digunakan untuk merawat tanah tiruan yang mengandungi 30% asid organik dalam suasana makmal. Sebanyak 20% penukaran kapur dengan zeolit hanya mengalami penurunan nilai pH yang rendah dan dapat memperkayakan ciri-ciri asas kapur dengan silika dan alumina. Elemen silika dan alumina adalah penting dalam menghasilkan matriks simen dalam suasana alkali.

vii

TABLE OF CONTENTS

CHAPTER TITLE PAGE

DECLARATION ii

DEDICATION iii

ACKNOWLEDGEMENTS iv

ABSTRACT v

ABSTRAK vi

TABLE OF CONTENTS vii

LIST OF TABLES xii

LIST OF FIGURES xv

LIST OF ABBREVIATIONS & SYMBOLS xxvi

LIST OF APPENDICES xxviii

1 INTRODUCTION 1

1.1 Background of Study 1

1.2 Problem Statement 2

1.3 Objectives of Study 3

1.4 Significance of Study 4

1.5 Scope of Study 5

1.6 Organisation of Thesis 7

2 LITERATURE REVIEW 9

2.1 Introduction 9

2.2 Soil – Lime Reactions 10

2.2.1 Reactions Process of Lime with Soil 11

viii

2.2.1.1 Hydration 11

2.2.1.2 Flocculation 11

2.2.1.3 Cementation 12

2.2.1.4 Carbonation 12

2.2.2 Reaction Products of Pozzolanic Reaction 13

2.2.3 Factors that Affect Soil-Lime Reactions 17

2.2.3.1 Effect of Curing Periods 18

2.2.3.2 Effect of Curing Temperature 19

2.2.3.3 Types of Soil 22

2.2.3.4 Dosage of Lime 23

2.2.3.5 Types of Lime 28

2.3 Reactions of Soil Organic Matter in Chemical Stabilisation 29

2.3.1 Types of Soil Organic Matter 29

2.3.2 Effects of Soil Organic Matter on Chemical Stabilisation 33

2.3.3 Use of Coco Peat in Laboratory Study 41

2.4 Natural Zeolite 43

2.4.1 Characterisation of Natural Zeolite 44

2.4.2 Use of Natural Zeolite as Pozzolan in 47 Cement Industry

2.5 Chapter Summary 61

3 EXPERIMENTAL DESIGN AND

METHODOLOGY 62

3.1 Introduction 62

3.2 Characterisation of Natural Organic Soil 66

3.2.1 Field Explorations in Pontian, Johor 78

3.2.2 Field Explorations in Batu Pahat, Johor 83

3.3 Characterisation of Artificial Soil 84

3.4 Characterisation of Stabilisers 87

3.4.1 Lime-Hydrated Lime 89

3.4.2 Natural Zeolite 90

3.4.3 Lime-Zeolite 92

ix

3.5 Stabilisation of Artificial Soil 94

3.5.1 Design of Experiment 95

3.5.2 Mix Proportions of Artificial Soil and

Additive 103

3.5.3 Specimen Preparation 104

3.5.4 Specimen Curing and Testing 106


DATA ANALYSIS AND DISCUSSION OF SOILS

AND ADDITIVES 113

4

4.1 Introduction 113

4.2 Composition Properties of Natural Organic Soil 115

4.2.1 Mineralogical Composition 115

4.2.2 Chemical Composition 119

4.2.3 Composition of Soil Organic Matter 121

4.3 Artificial Soil 135

4.3.1 Physical Properties of Artificial Soil 135

4.3.2 Chemical Properties of Artificial Soil 148

4.3.3 Mineralogical of Artificial Soil 154

4.3.4 Microstructure of Artificial Soil 156

4.4 Properties of Additives 158

4.4.1 Hydrated Lime 158

4.4.2 Natural Zeolite 162

4.4.3 Blended Lime Zeolite 170


5 STRENGTH AND MICROSTRUCTURE

ANALYSIS OF ARTIFICIAL SOIL STABILISED

WITH LIME ZEOLITE 180


5.2 Unstabilised Artificial Soil 181

5.2.1 Unconfined Compressive Strength 181

x

5.2.1.1 Effect of Curing Temperature on Strength of Kaolin 188

5.2.1.2 Effect of Curing Temperature on Strength of Unstabilised Artificial Soil 192

5.2.1.3 Effect of pH on Strength of Unstabilised Artificial Soil 195

5.2.1.4 Effect of Organic Matter on Strength of Unstabilised Soil 197

5.2.2 Mineralogy, Microscopic and Elemental Analysis 200

5.3 Stabilised Artificial Soil 204

5.3.1 Unconfined Compressive Strength 204

5.3.1.1 Optimum Percentage of Lime for Artificial Soil 205

5.3.1.2 Effect of Organic Content on Strength of Lime Stabilised Artificial Soil 214

5.3.1.3 Effect of Lime replaced with Zeolite on Strength of Stabilised Kaolin 216

5.3.1.4 Effect of Lime replaced with Zeolite on Strength of Stabilised Artificial Soil 219

5.3.1.5 Effect of Curing Temperature on Strength of Stabilised Artificial Soil 222

5.3.1.6 Effect of pH on Strength of Stabilised Artificial Soil 226

5.3.1.7 Effect of Organic Matter on Strength of Stabilised Artificial Soil 230

5.3.1.8 Effect of Zeolite Increment on Strength of Lime Stabilised Artificial Soil 236

5.3.2 Mineralogy Analysis 238

5.3.2.1 Effect of Curing Condition 238

5.3.2.2 Effect of Curing Periods 240

xi

5.3.2.3 Effect of Organic Acid 251

5.3.2.4 Effect of Partial Replacement of Lime with Zeolite 252

5.3.3 Microscopic and Elemental Analysis 254


6 CONCLUSIONS & RECOMMENDATIONS 264


6.2 Conclusions 265

6.2.1 Composition of Natural Organic Soil 265

6.2.2 Physico-Chemical Properties and Microstructure of Artificial Soil 266

6.2.3 Physico-Chemical Properties and Microstructure of Blended Lime Zeolite 268

6.2.4 Strength and Microstructure of Unstabilised Artificial Soil 269

6.2.5 Strength and Microstructure of Stabilised Artificial Soil 271

6.3 Recommendations 273

REFERENCES 275

Appendices A-C 289-347

xii

LIST OF TABLES

TABLE NO. TITLE PAGE

2.1 Microstructural types observed for Calcium Silicate Hydrate 15

2.2 Summary of organic soil/peat soil stabilisation 24 2.3 Reactivity behavior of humic substances 31 2.4 Solubility behavior of humic substances 31 2.5 Summary of previous studies on the mechanism of soil

organic matter stabilisation 35

2.6 Guideline for selecting binders on the basis of soil classification shown in Figure 2.16 40

2.7 Chemical composition of natural zeolite and pozzolanic

materials (% w/w) 46 2.8 Compressive strength over curing periods of the zeolite

blended cement mortars 55 2.9 The clay-grout mixes 56 2.10 Mercury intrusion porosimeter (MIP) porosity over

curing periods of the zeolite blended cement pastes 57 2.11 Components and relative contents of the clinker-zeolite

blends 59 3.1 Reference standards for field explorations and

laboratory tests of natural organic soils 75 3.2 Detailing of field explorations in Pontian and Batu

Pahat, Johor 79

3.3 A variety of artificial soils 85

xiii

3.4 Reference standards for laboratory tests of physical, chemical, microstructure and mineralogical properties of artificial soil

88 3.5 Blended lime zeolite 93 3.6 List of reference standards for test of stabilisers 94 3.7 Contributing factors and variable type selected for the

experiment

98 3.8 Subcategories of experiment 99 4.1 Bulk chemical composition of organic soil in Batu

Pahat, Johor 120 4.2 Quantitative correlation with humic acid & fulvic acid

and possible structural units 131 4.3 Particle size distribution of kaolin mixed with organic

acid 138 4.4 Specific surface and particle size distribution of kaolin-

organic acid 139 4.5 Bulk chemical composition of kaolin and organic acid 152 4.6 Bulk chemical composition of artificial soil 152 4.7 Approximate chemical composition of kaolin, organic

and artificial soils 153 4.8 Phase contents and crystallinity percentage of materials 155 4.9 Phase contents and crystallinity percentage of artificial

soils 156 4.10 pH value of hydrated lime from Lime Treat (M) Sdn.

Bhd. 159 4.11 Chemical composition of hydrated lime from Lime

Treat (M) Sdn. Bhd. 159 4.12 Total organic carbon of hydrated lime marketed by

Lime Treat (M) Sdn. Bhd. 161 4.13 Types of natural zeolite tested in this study 162 4.14 Bulk chemical composition of natural zeolites 164

xiv

4.15 Total organic carbon of natural zeolites 165 4.16 Total alkaline and alkali earth elements and acid neutral

capacity of materials 165 4.17 Relative amorphous content and crystalline content 167 4.18 Possible structural units for natural zeolites 168 4.19 Particle size analysis of the blended lime zeolite 171 4.20 Specific gravity of blended lime zeolite 171 4.21 Bulk chemical composition of blended lime zeolite 173 4.22 Crystallinity of blended lime zeolite 174 4.23 Approximate chemical composition of additives 176 5.1 Unconfined compressive strength of unstabilised

artificial soil cured at 50°C 182 5.2 Unconfined compressive strength of unstabilised

artificial soil cured at room temperature 183 5.3 Details of artificial soils 198 5.4 Elemental composition of unstabilised artificial soil 204 5.5 Phase contents and crystallinity percentage of

10K0HA#, 7K3HA# and 5K5HA# using 10L0ZT 241 5.6 Phase contents and crystallinity percentage of 7K3HA*

and 5K5HA* using 10L0ZT 243 5.7 Phase contents and crystallinity percentage of 7K3HA*



and 5K5HA* using 0L10ZT 249 5.10 Approximate chemical composition of needle like/rod

like structure for soil type K7HA3* 261 5.11 Approximate chemical composition of needle like/rod

like structure for soil type K5HA5* 262

xv

LIST OF FIGURES

FIGURE NO. TITLE PAGE

2.1 SEM micrographs of different types of C-S-H phase formed in cement-Rice Husk Ash (RHA) paste after 120 days of hardening 14

2.2 SEM micrographs of cement paste at various curing

periods 14 2.3 Effect of drying technique on the formation of C-S-H

structure 16 2.4 Irreversible formation of C-S-H structure 16 2.5 Effect of partial pressures on C-S-H formation 17 2.6 Strength gains of Suddha’s soil over curing periods

with different lime content 19

2.7 Strength gains of soil over curing periods with

different lime-RHA contents 20 2.8 Strength gains of soil at different curing temperature

over increased curing periods 21 2.9 Changes in pH of lime stabilised soil over curing

periods at curing temperature of 20°C and 50°C 21 2.10 Strength gains in different types of soil stabilised with

a binder (25% lime and 75% cement) 23 2.11 Strength gains of soil in different humic acid contents

with different lime content 28 2.12 Electrons micrograph of moderately humified fibres

taken from an Irish Sphagnum peat 30 2.13 Electron micrograph of James Bay peat showing

networks of fibrous elements and perforated hollow particles 31

xvi

2.14 Classification and characteristics of the organic matter in soil 32

2.15 Soil organic matter fractionation procedure 33 2.16 Soil classification zones based on the natural water

content and humic acid content

41 2.17 Coconut fibres 42 2.18 Representative image of cross-sectional view of

coconut 42 2.19 XRD pattern of the zeolite-Heulandite type II 47 2.20 XRD pattern of the zeolite-clinoptilolite 47 2.21 Fineness and water demand of Kimolos zeolitic tuffs

vs. volcanic glass 49 2.22 The plots of water demand-Blaine values over addition

of Clinoptilolite 49 2.23 Plots of strength gain in OPC and Clinoptilolite

blended cement mortars over hydration periods 502.24 Plot of strength vs. percentage addition of zeolite and

volcanic glass at different curing periods 51 2.25 Results of Fratini’s test for evaluating the ability of the

zeolite A and X to act as pozzolan. Solid line: Solubility curve of Ca(OH)2 52

2.26 Results of Fratini’s test at shorter and variable reaction

times. Square: OPC; triangle: blend A-25; circle: blend X-25. Reaction times in hours are indicated within the open symbols 53

2.27 Plots of compressive strength over hydration days for

zeolite blended cement mortars 54 2.28 Plot of reactive silica content over changes in strength

of cement mortars 55 2.29 UCS values for ten mixes at 28 days 56 2.30 Plot of compressive strength over porosity of zeolite

blended cement pastes 57 2.31 Effects of percentage zeolite on the properties of the

clay stabilised with cement-zeolite grout 58

xvii

2.32 Plot of compressive strength of clinker-zeolite pastes over curing times 59

2.33 Unconfined compressive strength of the stabilised clay

mixed with cement-zeolite in the aggressive and control environments 60

3.1 Flow chart of experimental design and methodology 64 3.2 Sampling locations in Pontian, Johor 67 3.3 Peat boundary map of Pontian 68 3.4 Sampling locations in Batu Pahat, Johor 69 3.5 Geological map of Batu Pahat sampling locations 70 3.6 Sampling of peat and soft organic soils using

Eijkelkamp’s peat auger 71 3.7 Undisturbed tube sampler 71 3.8 Instrumental devices used for mineralogical and

molecular characteristics 73

3.9 GEONOR H60 Hand-held Vane tester 74 3.10 Unconfined compressive test on organic soil sample 75 3.11 Planetary micro mill – FRITSCH PULVERISETTE 7

premium line 77 3.12 Sampling location at MARDI Pontian, Pontian 79 3.13 Lithology map, Syit 133, Kukup 80 3.14 Location of cross-section 80 3.15 Detailing of cross-section A-A’ 81 3.16 Detailing of cross-section B-B’ 81 3.17 Peat/organic soil samples at Kg. Seri Kenangan,

Pontian 82

3.18 Peat/organic soil samples at Kg. China, Pontian 82 3.19 Organic soil samples at Parit Nipah, Batu Pahat, Johor 83 3.20 Organic soil sampling using 38mm cylindrical tube

sampler at Parit Nipah, Batu Pahat, Johor

83

xviii

3.21 Components of artificial soil (kaolin, organic acid and coco peat)

85

3.22 Artificial soil mixed manually in pocket sealed plastic

bag

86 3.23 Malvern zeta sizer 87 3.24 Hydrated lime 90 3.25 Natural zeolite before and after grinded into fine

powder

91 3.26 Natural zeolite 93 3.27 Contributing factors considered for strength

enhancement of materials 96 3.28 Phase diagram of wet method of deep mixing 103 3.29 Remoulding mould for specimens 104 3.30 Preparation of soil specimen using compressive device 105 3.31 Constant volume of specimen 107 3.32 Artificial soil specimens cured at elevated temperature 108 3.33 Room temperature curing of specimens 109 3.34 Specimens cured at elevated temperature 110 3.35 Geocomp Load Trac II for UCS tests 111 4.1 X-ray diffractogram of peat soil at depth of 0.5 m –

1.0 m (MARDI Pontian) 116 4.2 X-ray diffractogram of soil at depth of 3.8 m –

10 m (MARDI Pontian) 116 4.3 X-ray diffractogram of soil at depth of 2 m –

4 m (P4, Pontian) 117 4.4 X-ray diffractogram of soil at depth of 1.66 m –

2.5 m (Parit Nipah) 118 4.5 X-ray diffractogram of soil at depth of 24 in. – 48 in.

(Parit Sidek) 118

xix

4.6 X-ray diffractogram of soil at depth of 0.74 m – 1.5 m (Batu Puteh) 119

4.7 FTIR spectra of peat soil at 0 m - 3.5m (PS1, MARDI

Pontian) 122 4.8 FTIR spectra of peat soil at 0 m - 3.8m (PS1, MARDI

Pontian) 122 4.9 FTIR spectra of peaty clay at 3.8 m – 4m (PS1,

MARDI Pontian) 123 4.10 FTIR spectra of peaty clay at 3.8 m – 10.0 m (PS1,

MARDI Pontian) 123 4.11 FTIR spectra of Permas Kelapa (P4) 124 4.12 FTIR spectra of P33 124 4.13 FTIR spectra of P264 125 4.14 FTIR spectra of Parit Nipah PA1 (0 m-1.5m) 125 4.15 FTIR spectra of Parit Nipah PA1 (1.0 m -2.0m) 126 4.16 FTIR spectra of Parit Nipah PA2 (1.0 m -2.0m) 126 4.17 FTIR spectra of Parit Nipah PA3 (1.66 m -2.5m) 127 4.18 FTIR spectra of Parit Sidek PA1 (24 in. – 48 in.) 127 4.19 FTIR spectra of Parit Sidek PA3 (24 in. – 48 in.) 128 4.20 FTIR spectra of Batu Puteh-P1 (0 m -1.5m) 128 4.21 FTIR spectra of Batu Puteh-P2 (0.74 m -1.5m) 129 4.22 FTIR spectra of PS1 MARDI Pontian’s peat soil at 3.5

- 3.8m vs. analytical grade humic acid of Sigma Aldrich 134

4.23 Particle size distribution of kaolin S300 mixed with

organic acid 136 4.24 Particle size distribution of kaolin FM-C mixed with

organic acid 137 4.25 Compaction curve of artificial soils 140

xx

4.26 Effect of organic acid on maximum dry density and optimum moisture content of kaolin S300 141

4.27 Effect of organic acid on maximum dry density and

optimum moisture content of kaolin FM-C 141 4.28 Plot of maximum dry unit weight versus organic

content 142 4.29 Plot of optimum moisture content (%) versus organic

content 143 4.30 Variation of maximum dry unit weight versus organic

content 143 4.31 Variation of optimum moisture content versus organic

content 144 4.32 Variation of specific gravity over organic acid content,

and organic content of kaolin S300 145 4.33 Variation of specific gravity over organic acid content,

and organic content of kaolin FM-C 146 4.34 Scatterplot of organic acid versus liquid limit, plastic

limit and optimum moisture content after compaction of kaolin S300 147

4.35 Scatterplot of organic acid versus liquid limit, plastic

limit and optimum moisture content after compaction of kaolin FM-C 148

4.36 Relationship of LOI (%), pH and sulfate content of

artificial soils with organic acid (%) 149 4.37 Zeta potential of kaolin S300 over pH change 150 4.38 Zeta potential of kaolin S300 (70%) and organic acid

(30%) over range of pH 150 4.39 Zeta potential of kaolin S300 (50%) and organic acid

(50%) over range of pH 151 4.40 Zeta potential of kaolin S300 (70%), organic acid

(30%) and coco peat (5%) over range of pH 151 4.41 XRD diffractogram of unstabilised kaolin S300 vs.

kaolin FM-C 154 4.42 SEM micrograph of kaolin S300 and organic acid 157

xxi

4.43 SEM micrograph of artificial soils 157 4.44 Particle size distribution of hydrated lime 158 4.45 SEM micrograph of hydrated lime- mag. 10kX 160 4.46 SEM micrograph of hydrated lime- mag. 25kX 161 4.47 FTIR spectra of natural zeolite 167 4.48 SEM micrograph of zeolite- Mechastone - mag. 10kX 169 4.49 SEM micrograph of zeolite- Mechastone - mag. 15kX 169 4.50 Particle size distribution of blended lime zeolite 171 4.51 pH of blended lime zeolite 172 4.52 XRD diffractogram of blended lime zeolite 174 4.53 SEM micrograph of 8L2ZT - mag. 10kX 175 4.54 SEM micrograph of 5L5ZT - mag. 10kX 175 4.55 Scanning electron micrograph of the fractured surface

of limestone 176 4.56 Overlap of FTIR spectra of lime zeolite 177 5.1 Effect of organic acid and kaolin on unconfined

compressive strength of unstabilised artificial soil cured at 50°C over curing periods 184

5.2 Effect of organic acid and kaolin on unconfined

compressive strength of unstabilised artificial soil cured at room temperature over curing periods 185

5.3 Effect of curing temperature and contents of organic acid on unconfined compressive strength of unstabilised artificial soil (Kaolin S300 + organic acid) over curing periods 186

5.4 Effect of curing temperature and contents of organic

acid on unconfined compressive strength of unstabilised artificial soil (Kaolin FM-C + organic acid) over curing periods 186

xxii

5.5 Effect of curing temperature and mixture of organic acid and coco peat on unconfined compressive strength of unstabilised artificial soil (Kaolin S300) over curing periods 187

5.6 Effect of pH on unconfined compressive strength of

unstabilised artificial soil cured at 50°C over curing periods 187

5.7 Effect of coco peat on unconfined compressive

strength of unstabilised artificial soil cured at 50°C over curing periods 189

5.8 Main effect plots for strength of kaolin at different

curing temperatures 190 5.9 Interaction plot for strength of kaolin at different

curing temperatures 190 5.10 Individual value plot of moisture loss 191 5.11 Main effect plots for strength of artificial soils at

different curing temperatures 193 5.12 Interaction plot for strength of artificial soils at

different curing temperatures 194 5.13 Main effect plots for strength of artificial soil with

different contents of NaOH and cured for different periods 196

5.14 Interaction plot for strength of artificial soils with

different contents of NaOH and cured for different periods 196

5.15 pH of 7K3HA with different molarities of NaOH 197 5.16 Main effect plots for strength of kaolin mixed with

organic matter 199 5.17 Interaction plot for strength of kaolin partially

replaced with organic matter 199 5.18 Effect of organic acid and coco peat on itensity peaks

of unstabilised artificial soils cured at 50°C 201 5.19 SEM micrograph of unstabilised artificial soils with

organic acid and coco peat cured at 50°C 201

xxiii

5.20 SEM micrograph of unstabilised artificial soils (with only organic acid) 202

5.21 Identical cracks on particles of unstabilised artificial

soils (with only organic acid) 203 5.22 Scatterplot of strength versus initial density and final

density of stabilised artificial soils 206 5.23 Scatterplot of strength versus final moisture content of

cured artificial soils 207 5.24 Boxplot of strength versus main effects 207 5.25 Solubility of soil minerals at various pH 208 5.26 Boxplot of differences in density versus main effects 209 5.27 Main effects plot for strength of lime stabilised

artificial soils 210 5.28 Interaction plot for strength of lime stabilised artificial

soils 210 5.29 Initial consumption of lime for artificial soils 211 5.30 Dissolution curves of the studied humic acid particles 211 5.31 Individual value plot of pH 212 5.32 Main effect plots for strength of soil with different

organic acid contents 214 5.33 Interaction plot for strength of artificial soils stabilised

with lime 215 5.34 Initial consumption of lime for soil Kaolin S300 -

organic acid 216 5.35 Main effect plots for strength of kaolin cured with lime

zeolite 217 5.36 Interaction plot for strength of kaolin stabilised with

lime zeolite 218 5.37 Main effect plots for strength of artificial soils

stabilised with lime zeolite 220 5.38 Interaction plot for strength of artificial soils stabilised

with lime zeolite 220

xxiv

5.39 pH of lime stabilised artificial soils at various percentage of organic acid 221

5.40 Main effect plots for strength of artificial soils

stabilised using lime zeolite and cured at different curing temperature 223

5.41 Interaction plot for strength of artificial soils stabilised

using lime zeolite and cured at different curing temperature 223

5.42 Main effect plots for strength of artificial soils

stabilised with lime zeolite and cured at different curing temperature 225

5.43 Interaction plot for strength of artificial soils stabilised

with lime zeolite and cured at different curing temperature 225

5.44 Main effect plots for strength of artificial soils with

different contents of NaOH and cured with lime zeolite for different periods 227

5.45 Interaction plot for strength of artificial soils with

different contents of NaOH and cured with lime zeolite for different periods 228

5.46 pH of soil 7K3HA added with NaOH and lime-zeolite

at 0 day 229 5.47 Main effect plots for strength of stabilised kaolin

partially replaced with organic matter 231 5.48 Interaction plot for strength of stabilised kaolin

partially replaced with organic matter 231 5.49 Main effect plots for strength of stabilised Kaolin FM-

C partially replaced with organic acid 234 5.50 Interaction plot for strength of stabilised Kaolin FM-C

partially replaced with organic acid 235 5.51 Main effect plots for strength of lime stabilised

artificial soils with increased percentage of zeolite 237 5.52 Interaction plot for strength of lime stabilised artificial

soils with increased percentage of zeolite 237 5.53 X-ray diffractogram of stabilised 7K3HA* using

10L0ZT cured for 56 days 239

xxv

5.54 X-ray diffractogram of stabilised 5K5HA* using 10L0ZT cured for 56 days 240

5.55 X-ray diffractogram of stabilised 7K3HA using

10L0ZT cured at 50°C- reaction products (C-S-H) 251 5.56 X-ray diffractogram of stabilised 5K5HA using

10L0ZT cured at 50°C- reaction products (C-S-H) 252 5.57 X-ray diffractogram of reaction products for artificial

soil 7K3HA cured at room temperature 253 5.58 SEM micrograph of needle like structure for sample

7K3HA*-10L0Z 255 5.59 SEM micrograph of needle like structure for sample

5K5HA*-10L0ZT 255 5.60 SEM micrograph of needle like structure for sample



7K3HA*-5L5ZT 256 5.63 SEM micrograph of sample 5K5HA*-5L5ZT cured for

56 days 256 5.64 SEM micrograph of sample 5K5HA*-5L5ZT cured for

7 days 257 5.65 SEM micrograph of sample 7K3HA*-0L10Z cured for




7 days 259

xxvi

LIST OF ABBREVIATIONS AND SYMBOLS

Al - Aluminum

Al2O3 - Aliminium Oxide

ATR - Attenuated Total Reflectance

BS - British Standard

Ca2+ - Calcium Cation

CAH - Calcium Aluminum Hydrate

CaO - Calcium oxide

CaCO3 - Calcium Carbonate

Ca(OH)2 - Calcium hydroxide

CaSO4 - Calcium Sulphate

CSH - Calcium Silicate Hydrate

EDX - Energy Dispersive X-ray Analyzer

Fe2O3 - Ferric Oxide

FESEM - Field Emission Scanning Electron Microscope

FTIR - Fourier Transform Infrared

GPS - Global Position System

H2O - Water

HCI - Hydrochloric Acid

IC - Inorganic Carbon

ICDD - International Center for Diffraction Data

ICL - Initial Consumption of Lime

JMG - Minerals and Geoscience Department Malaysia

K+ - Potassium Cation

LL - Liquid Limit

LOI - Loss of Ignition

MARDI - Malaysia Agricultural Research & Development Institute

MC - Moisture Content

xxvii

Mg2+ - Ion Magnesium

MgO - Magnesium oxide

MP - Modified Peat

Na+ - Sodium Cation

NaOH - Sodium Hydroxide

(OH)- - Hydroxide ion

OPC - Ordinary Portland Cement

PI - Plasticity Index

PL - Plasticity Limit

ppm - Parts per million

RECESS - Research Centre for Soft Soil

RHA - Rice Hush Ash

SiO2 - Silica

SG - Specific Gravity

SOM - Soil Organic Matter

TC - Total Carbon

TEM - Transient Electromagnetic

TG - Thermal Gravimetric

TGA - Thermal Gravimetric Analyzer

TOC - Total Organic Carbon

UCT - Unconfined Compression Test

UTHM - Universiti Tun Hussein Onn Malaysia

UTM - Universiti Teknologi Malaysia

VP - Virgin Peat

WDXRF - Wavelength Dispersive X-ray Fluorescence

XRD - X-ray Diffraction

XRF - X-ray Fluorescence

ZrO2 - Zirconium Oxide

θ - Failure angle

xxviii

LIST OF APPENDICES

APPENDIX TITLE PAGE

A Summary of laboratory test results of MARDI

Pontian, Pontian; Parit Nipah, Parit Sidek & Batu Puteh, Batu Pahat; Particle size analysis of natural organic soil – CILAS test results; XRD diffractogram of peat/organic soil; FTIR spectra of peat/organic soil samples; Spreadsheet for mix design of specimens; Example of main effects plot and interaction plot

289 B Specification sheet of Kaolin S300 and FM-C;

Specification sheet of Organic Acid; XRD Diffractogram of organic acid (Humic acid and Fulvic acid); Physico-chemical properties of Kaolin and Artificial soil; Specific gravity test results of additives; XRD Diffractogram of Hydrated Lime; FTIR Spectra of Hydrated Lime; FESEM-EDX of Hydrated Lime; XRD Diffractogram of Zeolite; FTIR Spectra of Zeolite; FESEM-EDX of Zeolite 319

C Bulk chemical composition of stabilised artificial soils;

Strength prediction models 340

CHAPTER 1

INTRODUCTION

1.1 Background of Study

Malaysia, as a tropical country is reported to experience humid and wet

climates throughout the year. The organic materials in this region are found to be

well preserved over a long period of time because of their physico-chemical and bio-

chemical processes (Bujang and Faisal, 2007). Plants that were preserved and

disintegrated under anaerobic and high water content conditions have resulted in an

accumulation of organic soils in this region. Organic soil that is found to be low in

strength and high in compressibility is categorized as soft soils.

Soft soil stabilisation by admixing it with chemical stabilisers namely lime

and cement are able to improve its engineering properties. The improved engineering

properties of stabilised soil are found to be better in strength and variability control,

lower in compressibility and deformability, and increase in volume stability and

durability (Hausmann, 1990). However, Koslanant et al. (2006) found that lime or

cement stabilisation of soil are less effective when dealing with high organic content.

Soils with high organic content normally experience lower strength increase after

stabilisation, if compared with inorganic soils stabilised with the same types and

amounts of additive (Ruis and Hansson, 2001).

Organic soils which are formed by disintegration of organic matter exhibit

various engineering characteristics with the amount of organic contents and stages of

decomposition. Hence, the organic soil is categorized based on its contents (British

2

Standards Institution, 2015; Department of Standards Malaysia, 2005; IKRAM,

1995)and stages of decomposition (Von post classification system) in order to better

describe the soil behaviour. However, the engineering properties of organic soil with

organic matter higher than 20% are not suitable to be estimated using the mechanical

criteria of conventional mineral soil. (Bujang and Faisal, 2007). Indeed, the

properties of organic soil are not only governed by the organic contents but also vary

with types of organic matter (Huttunen and Kujala, 1996; Koslanant et al., 2006;

Kujala, et al., 1996; Kuno, et al., 1989).

1.2 Problem Statement

Lime has been found to be an effective stabiliser for soil as it is able to

increase its strength and stability under the action of water (National Lime

Association, 2004). However, lime is not very effective in stabilising organic soils

(Ruis and Hasson, 2001) even though the successfulness of organic soil stabilisation

is sometimes deduced from empirical test data. The major problem in the use of

calcium based stabiliser (including lime and cement) in the stabilisation of organic

soils is the effectiveness of stabiliser over time (Bujang, 2006; Chen et al., 2009;

Koslanant et al., 2006). Thompson (1966) explained that the pozzolanic reactions

were obstructed in organic soil because the soil particles (as the primary source of

silica and/or alumina) used in the stabilisation process, were “coated” by organic

cations, inhibiting the silica and/or alumina from dissolution, which results in an

absence of silica and/or alumina in pozzolanic reaction. As a result, the desired

improvement is hard to gain when dealing with high organic content. Sometimes, the

improvement might also disappear over time.

Chen et al. (2009) found that calcium-based stabilisers like lime and cement

are not suitable for soils with high organic content as the detailed mechanism

involved in organic soil stabilisation is still not fully understood. It was explained

that the organic molecules absorb calcium ions that are necessary for chemical

reactions between stabilisers and soils thus inhibiting the growth of reaction

products, such as Calcium Silicate Hydrate (C-S-H) and Calcium Aluminates

3

Hydrate (C-A-H). The reaction products of the chemical reaction (pozzolanic

reaction) are the main contributor for strength enhancement. Thus, a detail study of

its physico-chemical behavior is needed to understand the mechanisms involved in

stabilisation.

In addition, Chen et al. (2009) also urged that alternative methods other than

adding extra stabiliser must be used even with organic content as low as 1%. The

effectiveness of lime or cement stabilisation can be also affected by the types of

organic matter. Hence, it is practically difficult to determine the threshold of organic

content that will retard the lime or cement stabilisation.

1.3 Objectives of Study

This research study aims to investigate and evaluate the use of Zeolite as

pozzolan for lime stabilisation of artificial soils. Hence, the research study was

undertaken with the following objectives:-

(i) To analyse the molecular structure in terms of functional group and its

x-ray diffraction pattern in an attempt to identify the composition of

natural organic soil as reference guide to design artificial soil;

(ii) To establish the use of artificial soils with organic acid and coco peat,

and lime-zeolite as additives by determining its physico-chemical and

microstructural properties;

(iii) To assess the changes induced on the mineralogy and microstructure

of stabilised artificial soils with its unconfined compressive strength;

(iv) To evaluate the effect of various contributing factors, namely curing

periods, curing temperature, types and contents of inorganic soil,

types and contents of organic matter and percentage of additives

(lime-zeolite) on strength enhancement of artificial soils;

4

(v) To establish strength prediction models for stabilising artificial soils

with Lime- Zeolite

1.4 Significance of Study

The deleterious effect of organic matter on the strength of soil stabilised with

lime and cement is not yet fully understood yet even though many studies have been

completed. One of the main challenges is identifying the types and quantity of

organic matter of the soil because the types and content of organic matter are found

to change with the humification process and vary with time. Hence, there is a need

for a comprehensive study of using artificial soil with specific organic matter and

organic contents, especially the soil organic matter widely available in the peat/

organic soil of Malaysia.

In addition, even though natural zeolite (a kind of natural pozzolan that is

widely available in our neighboring region) has a successful application in the

cement industry as a pozzolan, there are no known studies on the use of it in soil

stabilisation with lime, or in particular with organic soil. In fact, the concept of

partially replacing lime with zeolite (rich in alumino-silicate) in order to produce a

self-cementing matrix in aqueous environment with organic matter is also novel.

Hence, there is a need to identify the possibilities of using zeolite to stabilise soil

with organic matter.

Therefore, there is a need to identify the composition of local natural organic

soils in order to design artificial soils that are able to address local problems. By

identifying the physico-chemical and microstructure of artificial soils stabilised with

lime-zeolite, this study will able to address the above mentioned gaps in knowledge

and may be useful for geotechnical engineers and/ or those who wish to develop

projects on local organic soil deposits.

5

1.5 Scope of Study

This study was carried out in four stages with the aim to investigate and

evaluate the use of zeolite as pozzolan for lime stabilising soil with organic matters.

The first stage focused on the composition properties of the natural organic soil in

Pontian, and Batu Pahat, Johor which served as an input for designing artificial soil.

Field exploration studies for peat and organic soils were carried out in Pontian, and

Batu Pahat, Johor. The tropical peat and organic soil samples were collected using a

peat auger or a tube sampler and tested for its mineralogy and organic composition.

All the specimens were dried at the low temperature of 50°C in order to avoid the

potential losses of volatile organic components in higher temperatures. The mineral

composition of natural organic soils was determined using X-Ray Diffraction (XRD)

and the elemental chemical composition was determined using X-Ray Fluorescence

(XRF). The functional group of soils was identified by using Fourier Transform

Infrared Spectroscopy (FTIR) which helped determine the organic composition of

the soils.

The second stage was focused on examining the material properties and

behaviour of artificial soils, natural zeolites and hydrated lime. The composition of

artificial soils was chosen by the composition details of natural organic soils.

However, the ratio of each component (organic matter vs. inorganic matter) was

purposely changed with the aim to study the effect of its content. Two different kinds

of processed soil (Kaolin S300 and Kaolin FM-C) with different ratios of silicate

over aluminates and size distributions were chosen as the base soil for this study. The

kaolin S300 and Kaolin FM-C are commercially processed inorganic soils from

Kaolin (M) Sdn. Bhd. Two different types of organic matter: organic acid and coco

peat were utilized in this study as substitute material of humified matter and non-

humified matter in the natural organic soils. The organic acid, which consists of

humic acid and fulvic acid, was originally imported by a local fertilizer shop from

China as soil conditioner for agriculture, while the coco peat (also known as coir

dust) was obtained by pre-drying and sieving the coir fiber/ coconut fiber through a

sieve aperture of 2 mm. The use of organic acid and coco peat as substitute material

of organic matter was also reported by other researches in horticulture studies (Abad,

et al., 2002; De Silva, and van Gestel, 2009; Sharma, et al., 2014) and chemical

6

stabilisation studies (Kujala, et al., 1996; Tremblay, et al., 2002; Modmoltin, et al.,

2004; Shao, et al., 2007; Xu, et al., 2007; Zhu, et al., 2009; M. Yunos, et al., 2013).

In addition, the hydrated lime was also directly obtained from Lime Treat (M) Sdn.

Bhd. in Pasir Gudang in order to insure freshness. The natural zeolite utilized in this

study was imported from Indonesia and marketed as MECHASTONE by Anugerah

Alam Sdn. Bhd.

The third stage included the parametric study which focused on the influence

of organic matter (organic acid and coco peat), the percentage of additive (lime-

zeolite), curing periods, and curing temperature on the mechanical properties of

stabilised and unstabilised soil. A variety of artificial soils with known types and

percentage of organic matter and inorganic matter was prepared and mixed with

various percentages of lime and zeolite as additive for stabilisation. A series of

parametric studies were planned and carried out in order to determine the effect of

inorganic material (two types of kaolin soil), and organic matter (humified matter-

organic acid; non-humified matter- coco peat) on the properties of soils. Besides that,

various ratios of lime zeolite were utilized to stabilise the artificial soils with the aim

to determine the suitability of zeolite as pozzolan in the lime stabilisation of soils.

The amount of additives utilized in this study was in the range of 7.5% to 15% by

referring to its initial consumption of lime (ICL). The remoulded specimens were

subjected to an unconfined compressive test after curing for 7, 28 or 56 days. The

specimens were either cured in a humid box (room temperature curing) or in an oven

with a constant temperature of 50°c. It was found that the elevated temperature of

50°c is ideal for enhancing the strength of specimen stabilised with lime (George, et

al., 1992). A total of 636 specimens were tested for its unconfined compressive

strength by counting in 3 replicates for each mixture. A selective small portion of

specimen obtained from tested specimen after a UCT test was further oven dried and

grinded into small particles for microstructure tests. The changes in mineralogy and

morphology were determined by using X-Ray Diffraction (XRD), and a Field

Emission Scanning Electron Microscope (FESEM), respectively with the aim to

identify its hardening mechanism. The findings of this study are served as a reference

on the use of zeolite as pozzolan for lime stabilisation of organic matter that

artificially added in.

7

Lastly, a group of strength prediction models were established by using a

statistical approach in which the correlation between the various contribution factors

namely organic content, curing periods, curing temperature and additive content

were taken into consideration. The other factors namely, moulding water content,

types of compaction and compactive effort are keep constant through controlled

experiments. The General Linear Model (GLM) was utilized to determine the

significance of the main factors, two-factor interactions, and three factor interactions.

The significance factors and interactions were utilized in multiple regression

analyses to develop a strength prediction model which can be utilized to predict the

strength of stabilised materials within the inference space defined by the experiment.

1.6 Organisation of Thesis

This thesis aims to investigate the physico-chemical and microstructure of

artificial soils stabilised with lime and zeolite. Overall, this thesis consists of six

chapters with each chapter focusing on a different subject matter as follows.

Chapter 1 is the introduction for the whole thesis which gives an overview of

the background of study, the problem statement, objectives of study, significance of

study and scope of study. It covers a brief overview on the current problems and

issues when stabilising soil with organic matter. In addition, this chapter also

explains the approach taken in order to understand the mechanisms of organic matter

stabilised with blended lime zeolite or in particular the role of zeolite as pozzolan.

Chapter 2 presents the review of literature related to this study, which

includes the materials chosen in this study namely organic soils, lime and zeolite.

This chapter also encompasses topic likes soil-lime reactions, the influence of

organic matter on pozzolanic reactions, the use of humic acid and coco peat as a

substitute in producing artificial soil, and the use of zeolite as pozzolan.

Chapter 3 focuses on the material characterisation and selection which

includes the exploration study of organic soil in Pontian, and Batu Pahat, Johor as

8

well as the methods and analysis of the physico-chemical, microstructure and

mineralogy of artificial soils. Furthermore, this chapter also includes details of the

characterization and selection of additive (hydrated lime and natural zeolite) that was

used in this study.

Chapter 4 presents the compositional properties of natural organic soils in

Pontian and Batu Pahat, Johor. The findings served as an input for designing

artificial soils. In addition, the physico-chemical and mineralogical properties of a

variety of artificial soils, and additives are also presented and discussed in this topic.

The material properties reported in this topic unveiled the characteristics and

behaviour of artificial soils and additives.

Chapter 5 presents the unconfined compressive strength of artificial soils with

and without stabilisation by additives. The effect of various contributing factors on

the strength of artificial soils such as the curing periods, curing temperatures, organic

contents, organic types and percentage of additives (hydrated lime and zeolite) are

analyzed using a statistical approach to determine the correlation. The findings from

the study are also compared with other researchers’ work. Besides that, the analysis

and discussion on the morphology of the materials under the Scanning Electron

Microscope, the bulk chemical composition and its phases determined via X-ray

techniques, the functional group of materials via Infrared Spectroscopy are also

presented in this chapter.

The last chapter in this thesis- Chapter 6 gives a summary of the whole result

as an integral part of the study. The recommendations for future works or further

works are also provided in this topic.

CHAPTER 2

LITERATURE REVIEW 2.1 Introduction

Stabilisation work of soil by lime and cement is a common improvement

method used for stabilizing soft clay and dredged sludge. Soft clay found near the

surface and the dredged sludge usually contains high organic content, which reduces

the effectiveness of lime or cement stabilisation.

In this study, lime was chosen as the main binder because lime was reported

by Onitsuka et al. (2003) to be more sensitive with organic matter compared to

cement. According to Koslanant et al. (2006), cement stabilisation was found to

cause water and soil pollution by leaching of hexavalent chromium.

Literatures on the reactions of soil with lime are reviewed and reported in the

first part of this chapter which covers an overview of short-term and long term

reactions of soil with lime. The second part of this chapter focuses on the effects of

organic materials in the chemical stabilisation of soil. The reactions of the organic

matter with lime and cement are reviewed in order to understand the problems

encountered by previous researchers when dealing with organic soils. Whereas, the

third part of this chapter reviews the case studies of using artificial soil in laboratory

studies with the aim to reduce the variability in soil properties. The last part of this

chapter is dedicated to the use of natural zeolites as pozzolan. Lime-pozzolan

mixtures are normally necessary if the soils are not sufficiently reactive. Additional

10

silica and alumina from the pozzolan potentially forms a stronger cementitious

matrix that forms a lime-stabilised layer.

Overall, this review aims to:

a) Outline the reactions of soil with chemical stabilizers – lime and also

types of reaction product;

b) Identify various factors that may influence the reactions of lime with soil;

c) Categorize types of organic matter in soil and explain how soil organic matter

can influence the reactions of lime with soil;

d) Outline the use of humic acid and coco peat as artificial soil in laboratory

studies with the aim to explain the interaction mechanism in between each

component;

e) Outline the characteristics of natural zeolite and explain its use as pozzolan in

cement industry and soil stabilization;

2.2 Soil – Lime Reactions Lime, a kind of calcium based stabilizer, has a long history in soil

stabilisation. It was first used in 1924 as a soil stabiliser to strengthen a short stretch

of highway in the United States of America (Bell, 1996). Since then, lime is used in

modern construction, primarily for stabilising clayey soils. It is found that lime is not

very effective for cohesionless soils unless other additives are used.

Generally, there are two types of lime which are commonly used in

stabilisation: hydrated lime [Ca(OH)2], and quicklime [CaO]. Lime modifies the soil

11

through cation exchange and stabilises it after the modification process has

completed.

2.2.1 Reaction Process of Lime with Soil

In the short term, soil will experience hydration (for quicklime) and

flocculation (ion exchange) when lime is added. Whereas, the longer reactions of

lime with soil will be a cementation and carbonation process that contributes to the

gain of strength.

2.2.1.1 Hydration

Quicklime is found to be able to react almost immediately with water in soil.

The reaction results in a drying process that is effective in improving the strength of

soil. Besides that, the heat generation and expansion of the lime when used in lime

columns and layers can further enhance the consolidation effect.

CaO + H2O → Ca(OH)2 + Heat (280 Cal/gm of CaO) (2.1)

2.2.1.2 Flocculation

The cations that absorbed to the surface of clay sized soil, such as Sodium

(Na2+) are ready to exchange with Calcium (Ca2+) when lime is mixed with soil. The

cation exchange process will change the structural components of the soil, causing

the soil to flocculate, aggregate or coagulate. From the perspective of its chemical

reaction, the flocculation, aggregation or coagulation of the soil particles are actually

caused by the replacement of univalent alkali ions that are normally attracted to the

negatively charged clay particles with the dissociated bivalent calcium ions in the

12

pore water. The reaction will reduce the plasticity of clay which is measured as

Atterberg limits. As a result of the reaction, the workability, strength and stiffness of

soil are increased.

2.2.1.3 Cementation

The cementation process is the second stage of the clay-lime reaction. The

process will only occur when the alumina-silicate of the soil mineral is disassociated

from its original lattice by the hydroxyl ions released from the lime forming new

compounds such as calcium silicate hydrate (C-S-H) and calcium aluminate hydrates

(C-A-H) gels. This process is also known as a pozzolanic reaction.

Ca2+ + 2(OH)- + SiO2 → C-S-H (2.2)

Ca2+ + 2(OH)- + Al2SiO3 → C-A-H (2.3)

The pozzolanic reaction is responsible for the strength enhancement of

stabilised soil. Lime is found to be an effective stabilizer in fine-grained soils in

which the effectiveness of stabilizer will be increased with the surface area of the soil.

Cementation, is, however, limited by the amount of available silica. Increasing the

quantity of lime will increase strength only up to the point where all the silica of the

clay is used up; adding too much lime can actually be counterproductive. This is in

contrast to stabilisation with cement, where strength continues to improve with the

amount of admixture.

13

2.2.1.4 Carbonation

Reaction of lime with carbon dioxide in the open air or in voids of the ground

forms a relatively weak cementing agent. This may be beneficial where lime is

plentiful; the CaCO3 formed will not react any further with the soil.

2.2.2 Reaction Products of Pozzolanic Reaction

The gain of strength in soil stabilised by calcium based stabilisers such as

lime and cement is mainly contributed by the cementation/ solidification process that

occurs through pozzolanic reaction. Reaction products of pozzolanic reaction,

namely Calcium Silicate Hydrate (C-S-H) or Calcium Aluminum Hydrate (C-A-H)

are able to reduce the porosity and increase the bonding of the materials through its

unique structure. There are different types of C-S-H structure observed under the

Scanning Electron Microscope namely needle like, reticular and flocs-like as shown

in Figure 2.1. Different forms of C-S-H are found when mortar cement is mixed with

Rice Husk Ash when compared to the C-S-H formed in plain mortar cement (Cizer

et al., 2006).

Apart from the materials involved in the pozzolanic reactions, the structure of

C-S-H is also found to be different throughout the curing periods as shown in Figure

2.2. The Calcium Silicate Hydrate (C-S-H) formed in cement paste at early stage is

shown in Figures 2.2(a) - (b). The C-S-H structures were progressively developed as

fabric structure as curing time increased. Besides that, some needle-like ettringite

(formed in the early stage) and rod-like ettringite were found in Figures 2.2(d) - (f) as

curing time increased. Ettringite (3CaO.Al2O3.3(CaSO4). 32H2O) is the hydration

products of calcium aluminate in cement with sulfate ions from dissolution of

gypsum and water (Prasanphan et al., 2010).

In fact, there are several types of C-S-H structure as observed using the

electron microscope and it can be described as needles, thin foils, hollow tubes and

14

amorphous gel (Jennings et al., 1981). A classification system is proposed and

summarized in Table 2.1 with the aim to explain the relationship between types of C-

S-H and its forming period.

(a) SEM micrographs of needle-like and reticular C-S-H phases formed inside the pore of the mortar cement after 120 days of hardening

(b) SEM micrographs of flocs-like C-S-H phases formed in the matrix of mortar cement mixed with RHA at ratio of 5-5 after 120 days of hardening

Figure 2.1 SEM micrographs of different types of C-S-H phase formed in cement-

Rice Husk Ash (RHA) paste after 120 days of hardening (Cizer et al., 2006)

(a) 1 day (b) 3 days (c) 7 days

(d) 14 days (e) 28 days (f) 28 days

Figure 2.2 SEM micrographs of cement paste at various curing periods

(Nontananandh et al., 2005)

15

Table 2.1 : Microstructural types observed for Calcium Silicate Hydrate*

(Jennings et al., 1981)

Classification Period formed Morphology and habits

Type E First few hours; Stage

I and II

Type O Between 4 and 24h;

stages III and IV

Type 1 Forms from type O

during first few days

Type 1' Can be formed from

type O during first

few days

Type 3 Froms from type O

after several days

Type 4 After first 24h

Early

- Thin flakes or foils which, when dried,

become cigar-shaped tubes 0.25 µm

long, radiating from C3S grains at all

angles.

Middle

- Amorphous gel ≈ 0.5 µm thick

surrounding C3S grains; behaved as

wet plastic material for first several

days; changed into other morphologies

depending on space available

- Slightly tapered needles 0.75-1.0 µm

long, radiating perpendicularly to C3S

grains, with aspect ratio of ≈ 10;

formed from type O in open areas

>1 µm; encouraged by drying and/ or

age

- Tapered fibers 0.25-0.5 µm long, often

branching; formed from type O by

pulling apart particles; seen only on

young fracture surfaces

Late

- Partly crumpled foils which are

interlocked; formed as type O ages

and/ or dries in regions where original

interparticle spacing is < 1 µm

- Dense gelatinous inner product *w/n = 0.5.

16

Fonseca and Jennings (2010) found that the morphology of the C-S-H

structure is more dependent on drying process rather than length of curing periods.

The findings suggested that the drying process contributed to the formation of fiber-

like or needle like structures as shown in Figure 2.3. A rapid drying process favors

the formation of thinner and longer needles when compared to a slow drying process.

Besides that, other factors such as pre-drying process and partial pressures will also

affect the formation of reaction products as shown in Figure 2.4 and Figure 2.5,

respectively.

(a) Rapid drying (b) Dry in 2 hours

Figure 2.3 Effect of drying technique on the formation of C-S-H structure

(Fonseca and Jennings, 2010)

(a) No pre-drying (b) Pre drying at 76% RH desiccator

Figure 2.4 Irreversible formation of C-S-H structure (Fonseca and Jennings, 2010)

17

(a) 100% RH (b) 88% RH

(c) 75% RH (d) 33% RH

Figure 2.5 Effect of partial pressures on C-S-H formation (Fonseca and Jennings,

2010)

2.2.3 Factors that Affect Soil-Lime Reactions Various factors that affect soil-lime reactions are the environment of the

reaction, the nature of soil, types and dosage of lime, and the mixing efficiency of the

soil-lime. The environment includes the temperature and time of curing. The nature

of soil refers to types of soil or other factors such as specific surface area, amount of

reactive silica, moisture content or organic content of soil, which directly contribute

to the efficiency of reactions. Practically, typical correlation factors of 0.25 to 0.5 are

always applied to the laboratory results (Keller Ground Engineering, 2014). One of

18

the reasons is because of the lower mixing efficiency in-situ when compared to the

remoulding works conducted in the laboratory. The mixing efficiency is not

reviewed in detail in this subtopic because this study is solely a laboratory study.

2.2.3.1 Effect of Curing Periods

Strength gains in soil stabilised with lime is found to be time dependent

because the main contributor for strength enhancement is the pozzolanic reaction.

This reaction will occur when the alumina-silicate of the soil mineral is disassociated

from its original lattice by the hydroxyl ions released from the lime forming new

compounds such as calcium silicate hydrate and calcium aluminate hydrates gels.

Hence, it is recommended in BS 1924: Part 2 (1990) that curing periods of 7, 28, 56

and 112 days are more appropriate for lime stabilised soil in order to make sure that

the strength is increased satisfactorily. A curing period of 28 days is recommended

for lime stabilised soil if a single fixed curing period was chosen.

Studies by Umesha et al. (2009), and Jha and Gill (2006) have shown that the

strength of lime and lime-RHA stabilised soil increased with curing periods. It is

found that the strength increment of soil was more significant at higher lime content

and also at the initial periods (as shown in Figure 2.6 and Figure 2.7). Hence, it is

shown that lime is required for pozzolanic reaction and the cementation process is

started even at the initial 7 days.

19

Figure 2.6 Strength gains of Suddha’s soil over curing periods with different lime

content (Umesha et al., 2009)

2.2.3.2 Effect of Curing Temperature

One of the factors that increased the strength gains in lime stabilised soil is

through increased curing temperature. Many studies, such as by Dzulkarnain (2007),

Jha and Gill (2006), Rao and Shivananda (2005), and George et al. (1992) have

found that increased temperature not only increased the strength gain and also the

rate of strength gain. Hence, it is shown in Figure 2.8 that the strength of lime

stabilised soil is higher at higher curing temperature. Besides that, the strength

increment rate will also increase at a higher temperature range when comparing a

temperature range of 30°C to 40°C with a temperature range of 20°C to 30°C.

It is believed that the gain of strength is resulted from the accelerated

pozzolanic reaction at higher temperature resulting from the increased kinetics of

soil-lime reactions. As a result, more lime is consumed during the pozzolanic

reaction and thus a significant drop of pH is expected at a higher temperature as

shown in Figure 2.9 (Al-Mukhtar et al., 2010).

20

Figure 2.7 Strength gains of soil over curing periods with different lime-RHA*

contents (Umesha et al., 2009) *RHA – Rice Husk Ash

21

Figure 2.8 Strength gains of soil at different curing temperature over increased

curing periods (Dzulkarnain, 2007)

Figure 2.9 Changes in pH of lime stabilised soil over curing periods at curing

temperature of 20°c and 50°c (Al-Mukhtar et al., 2010)

Curing (day)

Stre

ngth

(kPa

)

* Suhu = Temp.

22

2.2.3.3 Types of Soil

Soil is generally considered the material formed by the breakdown of rock

through physical and/or chemical weathering. Soil can be categorized into gravel,

sand, silt and clay depending on its particle size distribution. A smaller particle size

will exhibit higher surface area, speeding up the chemical stabilisation process using

lime.

However, some types of soil namely peat soil may not be formed by the

weathering of rock (Powrie, 1997). It is produced through the decomposition of

organic matters by the microbial that exist in the area. Hence, the content of organic

matter varies with the stages of decomposition and thus contains different types of

compounds including proteins, sugars, and polysaccharides (Dingus, 1999).

One of the main factors that govern the strength gain is the nature of the soil

(Keller Ground Eng., 2014). It is shown in Figure 2.10 that the strength gains in

different types of soil are varied even though the same type (lime/cement mixture at

a ratio of 25/75) and fixed contents of stabiliser (100kg/m3 and 150kg/m3) were used.

The plot shows that clayey Silt and clay gained the highest strength when compared

to other types of soil. In fact, the stabilisation effect very much depends on reactivity

of soil which may change with the content of clay minerals, its pozzolanicity, organic

and sulfur content (Ǻhnberg et al., 1995). However, the strength increment in lime

stabilized clayey soil will usually increase to a certain limit which depends on its

reactive silica and clay content (Umesha et al., 2009). The limit is always known as

optimum lime content.

Comparatively, the mud and peat soil have the lowest strength gain as shown

in Figure 2.10. Various works have been carried out by numerous researchers in this

region with the aim to increase the strength of organic soil/ peat soil as summarized

in Table 2.2. However, types of organic matter in the soil are not well described in

most of the reviewed studies. Thus, the influential effect of each organic matter on

the strength of organic soil is not well understood. Hence, deleterious effects of

23

organic matter on the strength gain of lime stabilised soil are further reviewed in

Subtopic 2.3 which focused on the reactions of organic matter in soil stabilisation.

Figure 2.10 Strength gains in different types of soil stabilised with a binder (25%

lime and 75% cement) (Ǻhnberg et al., 1995)

2.2.3.4 Dosage of Lime

In general, the dosage of lime required depends on the nature of soil. The

strength linearly increases with dosage until a certain limit, which is known as the

optimum lime content (Figure 2.11). The optimum lime content varies with the soil

and depending on its clay content and the reactive silica (Umesha et al., 2009). The

extra lime content over the optimum lime content will most likely remain unreacted

and act as a filler material which results in a negative effect on strength gains. Bell

(1996) explained that the negative effect could be due to the fact that lime itself has

neither appreciable friction nor cohesion and thus extra lime will not able to

contribute for strength enhancement.

24

Table 2.2 : Summary of organic soil/peat soil stabilisation

Researcher(s) Characteristics of

Soil

Additive(s) utilized Findings & Comments

Arman and

Munfakh (1972)

Lime Stabilization

of Organic Soils

- Organic content =

0%, 10% and 20%

-Calcium hydroxide

-Percentage of lime

utilized = 12%

- UCS of stabilized soil decreased with the increment of

organic content.

- UCS of stabilized inorganic soil (0% organic content) in the

range of 200 – 210 psi for a curing period of 7 days to 28

days.

- UCS of stabilized organic soil (10% organic content) in the

range of 110 – 160 psi for a curing period of 7 days to 28

days.

- UCS of stabilized organic soil (20% organic content) in the

range of 60 – 80 psi for a curing periods of 7 days to 28 days

- Some calcium ions from added lime are used to satisfy the

base-exchange capacity of the organic matter, and fewer

ions are available for the pozzolanic reaction. Hence, the

strength increment was low for soil with 20% organic

content comparative to soil with 10% organic content.

REFERENCES Abad, M., Noguera, P., Puchades, R., Maquieira, A. and Noguera, V. (2002).

Physico-chemical and chemical properties of some coconut coir dusts for use as

a peat substitute for containerized ornamental plants. Bioresource Technology.

82, 241-245.

Abd. Karim, A. T. (2009). Metals Release from Contaminated Soil Solidified/

Stabilized with Cement and Rubber Wood Bark Ash. Universiti Kebangsaan

Malaysia: phD Thesis.

Ahmadi, B. and Shekarchi, M. (2010). Use of Natural Zeolite as a Supplementary

Cementitious Material. Cement & Concrete Composites. 32, 134–141.

Ǻhnberg, H., Johansson, S-E., Retelius, A., Ljungcrantz, C., Holmquist, L., Holm, G.

(1995). Cement och kalk för djupstabilisering av jord, En kemisk - fysikalisk

studie av stabiliseringseffekter (in Swedish). SGI Rapport 48. Linköping. pp. 8-

13.

Alonso, M.C., Fernández Luco, L., García, J.L., Hidalgo, A., Huertas, F., 2007. Low-

pH Cementitious Materials Design and Characterization, Proceedings of the 12th

International Congress on the Chemistry of Cement, 8-13 July, Montreal.

Al-Mukhtar, Muzahim, Lasledj, Abdelmadjid, and Alcover, Jean-Francois. (2010)

Behaviour and Mineralogy changes in Lime-treated Expansive Soil at 50 °C.

Applied Clay Science. 50, 199-203.

Aminur, M. R., Kolay, P. K. and Taib S. N. L. (2009). Effect of Admixtures on the

Stabilization of Peat Soil from Sarawak. Indian Geotechnical Conf. (IGC),

Guntur, India. Dec 16-19, pp. 410-414.

Andersland, O. B., Khattak, A. S. and Al-Khafaji, A. W. N. (1981). Effect of organic

material on soil shear strength. Laboratory Shear Strength of Soil. ASTM STP

740. R. N. Yong and F. C. Townsend. Eds., American Society for Testing and

Materials, 226-242.

276

Andersson, R., Carlsson, T. and Leppanen, M. (2004). Soft Ground Technology

(GSP 112). Proceedings of the United Engineering Foundation / ASCE Geo-

Institute Soft Ground Technology Conference, pp. 158-169.

Arman, Ara and Munfakh, George A. (1972). Lime Stabilization of Organic Soils.

Highway Research Record. 381, pp. 37-45.

ASTM International (2005). C618-05. United States of America: ASTM

International.

ASTM International (2000). D2166-00. United States of America: ASTM

International.

ASTM International (1996). D5102-96. United States of America: ASTM

International.

Basiri, N. and Abdul Rahim, N. (2010). Kajian Pemetaan Gambut di Kawasan

Pontian, Johor. No. Laporan: JMG.JHR (GBN) 02/2010. Unpublished note,

Mineral & Geosciences Malaysia (JMG).

British Standards Institution (1990). BS 1377: Part 1- Part 9. London: British

Standards Institution.

Bell, F. G. (1996). Lime Stabilization of Clay Minerals and Soils. J. of Engineering

Geology, 42, 223-227.

Boardman, D. I., Glendinning, S. and Rogers, C. D. F. (2001). Development of

Stabilisation and Solidification in Lime-Clay Mixes. Geotechnique. 50(6), 533-

543.





British Standards Institution (2015). BS 5930. London: British Standards Institution.

British Standards Institution (2001). BS 6463-102. London: British Standards

Institution.

British Standards Institution (2010). BS EN 196-6. London: British Standards

Institution.


Institution.


Institution.

277

British Standards Institution (2009). BS ISO 10381-6. London: British Standards

Institution.

British Standards Institution (2009). BS ISO 13320. London: British Standards

Institution.

Brigante, M., Zanini, G. and Avena, M. (2009). Effect of pH, anions and cations on

the dissolution kinetics of humic acid particles. Colloids and Surfaces A:

Physicochemical and Engineering Aspects, 347, 180-186.

Bujang, B. K. Huat and Faisal Hj. Ali (2007). Ground Improvement Techniques.

Universiti Putra Malaysia Press: Serdang, Malaysia.

Bujang, B. K. Huat (2006). Effect of Cement Admixtures on the Engineering

Properties of Tropical Peat Soils. The Electronic Journal of Geotechnical

Engineering (EJGE). 11, Bundle B. EJGE.

Canpolat, F., Yilmaz, K., Kose, M. M., Sumer, M. and Yurdusev, M. A. (2004). Use

of zeolite, coal bottom ash and fly ash as replacement materials in cement

production. Cement and Concrete Research, 34, 731-735.

Caputo, D., Liguori, B. and Colella, C. (2008). Some Advances in Understanding the

Pozzolanic Activity of Zeolites: The Effect of Zeolite Structure. Cement &

Concrete Composites, 30, 455 – 462.

Casagrande, T., Misano, V., Cupo Pagano, M., and Sferra, F. (1999). Soil-binding

agent affinity in soil stabilisation with cement and/or lime. Geotechnical

Engineering for Transportation Infrastructure. Balkema: Rotterdam.

Chan, S. Y. N. and Ji, X. (1999). Comparative study of the initial surface absorption

and chloride diffusion of high performance zeolite, silica fume and PFA

concretes. Cement and Concrete Composites, 21 (4), 293-300.

Chen, D. H., Si, Z. M., and Mustafa Saribudak (2009). Roadway Heaving Caused by

High Organic Matter. Journal of Performance of Constructed Facilities, ASCE,

23(2), 100-108.

Chen, H. and Wang, Q. (2006). The Behaviour of Organic Matter in the Process of

Soft Soil Stabilization using Cement. Bull Eng Geol Env. 65, 445-448.

CILAS (1994). Particle Size Analyzer CILAS 920,930e,1064 & 1180 User Manual.

NT-1503192-31. Issue: September 2004. Orleans Cedex France: CILAS.

Cizer, O., Balen, K. Van, Elsen, J., and Gemert, D. Van (2006). Carbonation and

Hydration of Calcium Hydroxide and Calcium Silicate Binders with Rice Husk

278

Ash. Proceedings of the 2nd International Symposium on Advances in Concrete

through Science and Engineering. 11-13 September. Quebec City, Canada.

Clare, K. E. and Sherwood, P. T. (1956). Further studies on the effect of organic

matter on the setting of soil-cement mixtures. Journal of applied chemistry, 6,

317-324.

Cristelo, N., Glendinning, S., Fernandes, L., and Pinto, A. T. (2012). Effect of

calcium content on soil stabilisation with alkaline activation. Construction and

Building Materials, 29,167–174

Das, B. M. and Sobhan, K. (2014). Principles of Geotechnical Engineering

(8th ed.) Cencage Learning: USA.

Das, B. R. and Hati, S. (2010). Coir Fibre. Review. India, Aug 2010.

Department of Standards Malaysia (2005). MS 1056- Part 1. Putrajaya: Department

of Standards Malaysia.

De Silva, P. M. C. S. and van Gestel, C. A. M. (2009). Development of an alternative

artificial soil for earthworm toxicity testing in tropical countries. Applied Soil

Ecology. 43, pp. 170-174.

Dingus, Del D. (1999). Soil Science: Laboratory Manual. Upper Saddle River, N.J.:

Prentice Hall.

Drake, J. A. and Haliburton, T. A. (1972). Accelerated Curing of Salt-Treated and

Lime Treated Cohesive Soils. Highway Research Record. 381, 10 – 19.

Dzulkarnain bin M. Razak (2007). Effect of Temperature on Soil Stabilized with

Lime. Undergraduate thesis. Universiti Teknologi Malaysia, Skudai. In Malay

language.

Eades, J. L. and Grim, R. E. (1966). A Quick Test to Determine Lime Requirements

for Lime Stabilization. Highway Research Board, 139, 61-72.

Eijkelkamp (2005). 04.09-Peat Sampler Set [Operating Instructions]. Netherlands:

Eijkelkamp.

Elaiopoulos, K., Perraki, Th., and Grigoropoulou, E. (2008). Mineralogical study and

porosimetry measurements of zeolites from Scaloma area, Thrace, Greece.

Microporous and Mesoporous Materials: 112, 441–449

ELE International (2009). Construction Materials Testing Equipment [Product

Catalogue 12th Edition]. England: ELE International.

Evangelou, V. P. (1998). Environmental Soil and Water Chemistry: Principles and

Applications. Wiley-Interscience Publication: Canada.

279

Feng, Nai-Qian and Peng, Gai-Fei (2005). Applications of natural zeolite to

construction and building materials in China. Construction and Building

Materials. 19, 579–584

Filz, G. M., Hodges, D. K., Weatherby, D. E. and Marr, W. A. (2005). Standardized

Definitions and Laboratory Procedures for Soil-Cement Specimens Applicable

to the Wet Method of Deep Mixing. Innovations in Grouting and Soil

Improvement (GSP 136) in Proceedings of the Sessions of the Geo‐Frontiers

2005.

Fonseca, P. C. and Jennings, H. M. (2010). The effect of drying on early-age

morphology of C–S–H as observed in environmental SEM. Cement and

Concrete Research. 40, 1673–1680

Fornes, F., Belda, R. M., Abad, M., Noguera, P., Puchades, R., Maquieira, A. and

Noguera, V. (2003). The microstructure of coconut coir dusts for use as

alternatives to peat in soilless growing media. Australian Journal of

Experimental Agriculture, 43, 1171-1179.

Fragoulis, D., Chaniotakis, E. and Stamatakis, M. G. (1997). Zeolitic Tuffs of

Kimolos Island, Aegean Sea, Greece and Their Industrial Potential. Cement and

Concrete Res. 27( 6), 889-905.

FRIM (2015). Laboratory Test Report. Report No. BK 37/15. Kepong, Selangor:

Makmal Kimia Tanah, FRIM.

GEONOR A/S (1995). Inspection Vane Tester - H-60 [Instructions for use]. Oslo,

Norway: GEONOR A/S.

George, S. Z., Ponniah, D. A. and Little, J. A. (1992). Effect of temperature on lime-

soil stabilization. Construction & Building Materials. 6(4), 247-252.

Ghobadi, M. H., Abdilor, Y. and Babazadeh R. (2014). Stabilization of clay soils

using lime and effect of pH variations on shear strength parameters. Bull Eng

Geol Environ. 73, 611 – 619.

Gillman, G. P. and Sumpter, E. A . (1986). Modification to the compulsive exchange

method for measuring exchange characteristics of soils. Aust. J. Soil Res. 24, 61-

66.

Glasser, F. P. (1994). Cements in radioactive waste disposal. Materials Research

Society Bulletin, 12, 33-39.

Gretagmacbeth (2000). Munsell Soil Color Charts [Revised Washable Edition].

New York: Gretagmacbeth..

280

Haan, E. J. den (1998). Cement based stabilizers for Dutch organic soils.

Proceedings of the International Symposium on Problematic Soils, IS-

Tohoku'98, Sendai, Japan. October 28-30, pp. 53-56

Haberhauer, G., Rafferty, B., Strebl, F. And Gerzabek, M. H. (1998). Comparison of

the composition of forest soil litter derived from three different sites at various

decompositional stages using FTIR spectroscopy. Geoderma, 83, 331-342.

Hach Company (2005). DR5000 Spectrophotometer Procedures Manual [Second

Edition]. Germany: Hach Company.

Halim, A. Sanusi (2003). Potensi dan Pemanfaatan Endapan Zeolit di Daerah

Cipatujah, Kabupaten Tasikmalaya Provinsi Jawa Barat. Departemen Energi

dan Sumber Daya Mineral, Bandung. Unpublished note. (In Indonesia language).

Harris, P., Scullion, T. and Sebesta, S. (2004). Hydrated Lime Stabilization of

Sulfate-Bearing Soils in Texas. Technical Report: May 2002 - May 2004. Texas

Transportation Institute.

Harvey, O. R., Harris, J. P., Herbert, B. E., Stiffler, E. A. and Haney, S. P. (2010).

Natural organic matter and the formation of calcium-silicate-hydrates in lime-

stabilized smectites: A thermal analysis study. Thermochimica Acta, 505( 1-2),

106-113.

Hassink, J. (1997). The capacity of soils to preserve organic C and N by their

association with clay and silt particles. Plant and Soil, 191, 77–87. Hausmann, M. R. (1990). Engineering Principles of Ground Modification. McGraw-

Hill Publishing Company: Singapore.

Hebib, S. and Farrell, E. R. (2001). Some Experiences on the Stabilization of Irish

Peats. Can. Geotech. J. 40, 107-120.

Heinonen, R. 1955. Soil aggregation in relation to texture and organic matter.

Maatalouskoelaitoksen Maatutkimusosasto, Agrogeologisisa Julkaisuja, 64, 1–17.

Huttunen, E. and Kujala, K. (1996). On the Stabilization of Organic Soils.

Proceedings of the International Conference on Ground Improvement

Geosystems Vol. 1. 2 May. Tokyo, Japan, 411-414.

IKRAM (1995). GEOGUIDE 6 – Site Investigation for Organic Soils and Peats.

(JKR 20709-0341-95). Malaysia: IKRAM, JKR.

Islam, M. S., Saha, A., Rashid, Sk. H. & Salekin, S. (2005). Stabilization of Soft

Organic Soil using Carbide Lime. Proceedings of 6th International Conference on

281

Ground Improvement Techniques. 18- 19 July 2005. Coimbra, Portugal. Pp. 325

– 332.

Ismaiel, H.A.H. (2006). Treatment and Improvement of the Geotechnical Properties

of Different Soft Fine-grained Soils Using Chemical Stabilization. Shaker,

Aachen.

Janotka, I., Krajci, L. and Dzivak, M. (2003). Properties and utilisation of zeolite-

blended Portland cements. Clays and Clay Minerals. 51(6), 616-624.

Jegandan, S., Liska, M., Osman, A. A. M. and Al-Tabbaa, A. (2010). Sustainable

binders for soil stabilisation. Proceedings of the Institution of Civil Engineers.

Ground Improvement. 163 (G11), 53-61.

Jennings, H. M., Dalgleish, B. J., and Pratt, P. L. (1981). Morphological

Development of Hydrating Tricalcium Silicate as Examined by Electron

Microscopy Techniques. Journal of Americal Ceramic Society. 64 (10), 567-572.

Jha, J. N. and Gill, K. S. (2006). Effect of Rice Husk Ash on Lime Stabilization of

Soil. Journal of the Institution of Engineers (India). 87, 33-39.

JMG (1985). Geological Map of Peninsular Malaysia [Eighth Printing]. Malaysia:

JMG.

Joshi, M. S., Joshi, V. V., Choudhari, A. L., and Kasture, M. W. (1997). Structural

Studies of Natural Heulandite using Infrared Spectroscopy. Materials Chemistry

and Physics. 48, 160-163.

Kaish, A. B. M. A., Jamil, M., Alam, M.R., and Zain, M.F.M. (2012). A Theoretical

Approach for Determining Optimum Percentage of Rice Hush Ash Replacement

in Concrete Materials. Proceedings of The ICONCESS 2012. 4-5 April 2012.

Johor Bahru. Paper ID: MSE 103.

Kassim, K. A., Hamir, R. and Kok, K. C. (2005). Modification and Stabilization of

Malaysian Cohesive Soils with Lime. J. of The Southeast Asian Geotechnical

Society. August. 123- 132.

Keller Ground Engineering (2014). Lime Cement Dry Soil Mixing. Australia: Keller

Ground Engineering Pty. Ltd.

Kitsopoulos, K. P., and Dunham, A.C. (1996). Heulandite and mordenite-rich tuffs

from Greece: a potential source for pozzolanic materials. Mineralium Deposita

31, 576–583.

282

Kokotailo, G. T. and Fyfe C. A. (1995). Zeolite Structure Analysis with Powder X-

Ray Diffraction and Solid-State NMR Techniques. The Rigaku Journal. 12 (1),

3-10.

Kolay, P. K., Sii, H. Y. and Taib, S. N. L. (2011). Tropical Peat Soil Stabilization

using Class F Pond Ash from Coal Fired Power Plant. International Journal of

Civil, Environmental, Structural, Construction and Architectural Engineering.

5(2), 1-5.

Koslanant, S., Onitsuka, K., and Negami T. (2006). Influence of Salt Additive in

Lime Stabilization on Organic Clay. J. of The Southeast Asian Geotechnical

Society. 37(2), 95 – 101.

Kujala, K., Makikyro, M. and Lehto, O. (1996). Effect of humus on the binding

reaction in stabilized soils. International conference on ground improvement

geosystems, 2, IS-Tokyo.96: Grouting and Deep mixing, Tokyo, May.

Proceeding. 1, 415-420.

Kuno, G., Kutara, K. and Miki, H. (1989). Chemical stabilization of soft soils

containing humic acid. Proc. 12th Inter. Conf. Soil Mech. Found. Eng, Rio de

Janeiro, Vol.2, pp.1381-1384.

Lai, J. (2014). Unconfined Compression Test. Advanced Geotechnical Laboratory

Instructions Sheet. Unpublished note, Chaoyang University of Technology,

Taiwan.

Lam, S. K. (1998), Quaternary Geology of the Sibu town area, Sarawak, Malaysia,

Geological Survey Department Malaysia, Map Report Series 10.

Landva, A. O., and Pheeney, P. E. (1980), Peat fabric and structure. Can. Geotech. J.

17(3), 416–435.

Lee, J., Kim, K. and Chun B. (2012). Strength Characteristics of Soils Mixed with an

Organic Acid Material for Improvement. Journal of Materials in Civil Eng.,

24(12), 1529-1533.

Little, D. N., Males, E. H., Prusinski, J. R., & Stewart, B. (2000). Cementitious

Stabilization. Unpublished note, A2J01: Committee on Cementitious

Stabilization, Transport Research Board (TRB).

Malvern (2013). Zetasizer Nano User Manual [Issue 11]. United Kingdom: Malvern

Instruments Ltd.

283

Mamba, B. B., Nyembe, D. W. and Mulaba-Bafubiandi, A. F. (2009). Removal of

copper and cobalt from aqueous solutions using natural clinoptilolite. Water SA.

35, No.3, pp. 307-314.

Mason, J. (2003). Sustainable Agriculture (Second Edition). Landlinks Press:

Australia.

Massazza, F. (1993). Pozzolanic cements. Cement & Concrete Composites. 15, 185-

214.

Massazza, F. (1998). Pozzolana and pozzolanic cements, in: Lea's Chemistry of

Cement and Concrete, 4th Edn.,Wiley, New York, 471- 632.

Mertens, G., Snellings, R., Van Balen, K., Bicer-Simsir, B., Verlooy, P., and Elsen, J.

(2009). Pozzolanic reactions of common natural zeolites with lime and

parameters affecting their reactivity. Cement and Concrete Research. 39, 233–

240.

Mesri, G., and Ajlouni, M. (2007), Engineering Properties of Fibrous Peats. J. of Geo.

and Geoenv. Eng., 133 (7), 850-866.

Md. Razali, M. A., Kamaruzaman, A. Z. and Ayob, D. (2009). Kajian Sempadan

Gambut dengan Menggunakan Kaedah “Transient Electromagnetic” (TEM) di

Selatan Daerah Pontian, Johor. Laporan No. JMG. BPT(GF) 11/2009.

Unpublished note, Mineral & Geosciences Malaysia (JMG).

Modmoltin, C., Lu, J. and Onitsuka, K. (2004). Influence of Humic Acid and Salt

Concentration on Lime-Stabilized Ariake Clays and Microstructure Research.

Chinese Journal of Geotechnical Engineering. 26 No. 2, 281-286.

Mohd Hanapi, M. H. (2005). Pemetaan Geologi Kawasan Kukup, Johor.

Unpublished note, Mineral & Geosciences Malaysia (JMG).

Mohd Yunus, N. Z., Wanatowski, D., and Stace, L. R. (2011). Effect of Humic Acid

on Physical and Engineering Properties of Lime-Treated Organic Clay. World

Academy of Science, Engineering and Technology. 59, 1820 – 1825.

Mohd Yunus, N. Z., Wanatowski, D., and Stace, L. R. (2013a). Lime Stabilisation of

Organic Clay and the Effects of Humic Acid Content. Geotechnical Engineering

Journal of the SEAGS & AGSSEA. 44, No.1, 19 – 25.

Mohd Yunus, N. Z., Wanatowski, D., Stace, L. R., Norliana Abdullah & Rini

Asnida Abdullah (2013b). Effect of Humic Acid on Microstructure of Lime-

Treated Organic Clay. International Journal of Engineering Research &

Technology (IJERT). 2, Issue.11, 1827 – 1833.

284

Mulyukov, È. I. (2008). Alkaline Swelling and Consequences of Alkalization of

Clayey Bed Soils. Soil Mechanics and Foundation Eng. 45 (5), 182 – 185.

Mumpton, F. A. (1999). La roca magica: Uses of natural zeolites in agriculture and

industry. Proc. Natl. Acad. Sci. USA, 96, 3463-3470.

Naceri, A., and Hamina, M. C. (2009). Use of waste brick as a partial replacement of

cement in mortar. Waste Management, 29, No. 8, 2378– 2384.

National Lime Association (2004). Lime-Treated Soil Construction Manual: Lime

Stabilization & Lime Modification. Bulletin 326, January.

National Lime Association (2006). Technical Brief : Mixture Design & Testing

Procedures for Lime Stabilized Soil. Arlington: National Lime Association.

Nontananandh, S., Thakon, Y., and Sanupong, B. (2005). “Scanning electron

microscopic investigation of cement stabilized soil.” In Proceeding of the 10th

National Convention on Civil Engineering, 2-4 May. Pattaya, Thailand, 23-26.

Noori, M., Zendehdel, M. and. Ahmadi, A. (2006). Using natural zeolite for the

improvement of soil salinity and crop yield. Toxicological & Environmental

Chemistry. 88(1), 77-84.

O’Kelly, Brendan C. (2015). Effective Stress Strength Testing of Peat.

Environmental Geotechnics. 2(EG1), 34-44.

O’Kelly, Brendan C. and Zhang, L. (2013). Consolidated-drained Triaxial

Compression Testing of Peat. Geotechnical Testing Journal, 36(3), 310-321.

Ohio Environmental Protection Agency (2004). Geotechnical and Stability Analyses

for Ohio Waste Containment Facilities. Chapter 4. Materials Testing Program

Methods and Assumptions [Policy book].Columbus, Ohio: Ohio Environmental

Protection Agency

Onitsuka, K., Modmoltin, M., Kouno, M. and Negami, T. (2003). Effect of organic

matter on lime and cement stabilized Ariake clay. J. Geotech Eng., JSCE, No.

729/III-62, 1-13.

Orlov, D. S. (1986). Humus Acids of Soils. Rotterdam: Balkema.

Ortega, E. A., Cheeseman, C. Knight, J. and Loizidou, M. (2000). Properties of

alkali-activated clinoptilolite. Cement & Concrete Research, 30: 1641–1646

Osman, A.A.-M and Al-Tabbaa, A. (2006). Effect of zeolite and bentonite on the

mechanical properties of cement-stabilised soft clay. Proceedings of the 4th

International Conference on Soft Soil Engineering, Vancouver. Taylor &

Francis, London, 681-690.

285

Osman, A.A.-M and Al-Tabbaa, A. (2009). Effect of cement-zeolite grouts on the

durability of stabilised clays. Proceedings of the 17th International Conference

on Soil Mechanics and Geotechnical Engineering, Egypt. IOP Press, London, 3-

6.

Parbery, D.B., and Venkatachalam, R. M. (1964). Chemical Analysis of South

Malaysian Peat Soil. The Journal of Tropical Geography, 125-133.

Prasanphan, S., Sanguanpak, S., Wansom, S. and Panyathanmaporn, T. (2010).

Effects of Ash Content and Curing Time on Compressive Strength of Cement

Paste with Rice Husk Ash. Suranaree J. Sci. Technol., 17(3), 293-302.

Perraki, Th., Kakali, G. and Kontoleon, F. (2003). The Effect of Natural Zeolites on

the Early Hydration of Portland Cement. Microporous and Mesoporous

Materials, 61, 205 – 212.

Poon, C. S., Lam, L., Kou, S. C. and Lin, Z. S. (1999). A Study on the Hydration

Rate of Natural Zeolite Blended Cement Pastes. Construction and Building

Materials, 13, 427 – 432.

Powrie, W. (1997). Soil Mechanics Concepts and Application. Melbourne, Australia:

University of Southampton.

Puppala, A. J., Pokala, S. P., Intharasomba, N. and Williammee R. (2007). Effects of

organic matter on physical, strength and volume change properties of compost

amended expansive clay. J. Geote. Geoenv. Eng., 133 (11), 1449-1461.

Rajimin, M. Fauzi (2005). Data Lubang Gerudi Kuaterner (Cetek dan Dalam) Syit

133 (Kukup, Pontian). Unpublished note, Mineral & Geosciences Malaysia

(JMG).

Rao, S. M. and Shivananda, P. (2005). Role of Curing Temperature in Progress of

Lime-Soil Reactions. Geotechnical and Geological Engineering. 23, 79–85.

Ruis, M. and Hansson, T. (2001). Stabilization of Organic Soil with The Limix

System. The Deep Foundations Institute’s Soil Mixing Committee Specialty

Seminar: Soil Mixing, Oct. 3, 2001. New Jersey, U.S.A. 41 – 49.

Sabir, B., Wild, S., and Bai, J. (2001). Metakaolin and calcined clays as pozzolans

for concrete: a review. Cement and Concrete Composites. 23, No.6, 441–454.

Saikia, Bhaskar J. and Parthasarathy, G. (2010). Fourier Transform Infrared

Spectroscopic Characterization of Kaolinite from Assam and Meghalaya,

Northeastern India. J. Mod. Phys., 1, 206-210.

286

Sakr, M. A., Shahin, Mohammed A., and Metwally Y. M. (2009). Utilization of lime

for Stabilizing Soft Clay soil of High Organic Content. Geotech Geol Eng. 27,

pp.105-113.

Schumacher, B. A. (2002). Methods for the determination of Total Organic Carbon

(TOC) in Soils and Sediments. US. Environmental Protection Agency.

Shao, Y. F., Gong, X. N., Xu, R. Q. & Liu Z. Y. (2007). Experimental Study on

Stabilization of Humus-Containing Soft Soil. Journal of Zhejiang University

[Engineering Science]. 41, No.9, 1472-1476.

Sharma, N., E. Ramash, and Klam, K. (2014). An artificial soil ingredient substitute

for the earthworm toxicity testing (Coco peat). International Journal of

Environmental Science and Toxicology. 2(6), pp. 81-87.

Shi, C. and Day, R. L. (2000). Pozzolanic reaction in the presence of chemical

activators. Part 1: Reaction kinetics. Cement and Concrete Research, 30, 51-58.

Shimadzu Corporation (2000). Solid Sample Module - SSM 5000a for TOC-V Series

Total Organic Carbon Analyzer [User’s manual]. Japan: Shimadzu Corporation.

Soane, B. D. (1990). The role of organic matter in soil compactibility: A review of

some practical aspects. Soil and Tillage Research,16 (1-2), 179-201.

Staub, J. R., Among, H. L. and Gastaldoc, R. A. (2000), Seasonal sediment transport

& deposition in the Rajang River delta, Sarawak, East Malaysia. Sedimentary

Geology, 133(3-4), 249-264.

Stevenson, F. J. (1994). Humus Chemistry: Genesis, Composition, Reactions. 2nd

Edition. New York: Wiley and Sons. Ltd.

Subsurface Engineering (2009). Site investigation final report: To continuously

sampling of peat/organic soil at Pontian, Johor with peat auger up to 10m and

laboratory testing for geotechnical properties for Pusat Penyelidikan Tanah

Lembut (RECESS), Fakulti Kejuruteraan Awam dan Alam Sekitar, Universiti

Tun Hussein Onn Malaysia. Unpublished note, Subsurface Engineering.

Sugita, R. and Marumo, Y. (2001). Screening of soil evidence by a combination of

simple techniques: validity of particle size distribution. Forensic Science

International, 122, 155-158.

Tan, K. H. (1998). Principles of Soil Chemistry. (3rd Edition). New York: Marcell

Dekker, Inc.

Taylor, H. F. W. (1997). Cement Chemistry (2nd Edition). London: Thomas Telford.

287

Texas Department of Transportation (2000). Test Method TEX-620-J. Determining

Chloride and Sulfate Content in Soils [Technical Memorandum]: Texas: Texas

Department of Transportation.

Thompson, M. R. (1966). Lime reactivity of Illinois soils. Journal of Soil Mechanics

and Foundations Div., ASCE, 92(5), 67-92.

Tremblay, H., Duchesne, J. Locat, J. and Lroueil, S. (2002). Influence of the nature

of organic compounds on fine soil stabilization with cement. Can. Geotech. J.,

39, 535-546.

Tuller, M. and Or, D. (2003). Retention of Water in Soil and The Soil Water

Characteristic Curve. Unpublished note: University of Connecticut.

Umesha, T. S., Dinesh, S. V., and Sivapullaiah, P.V. (2009). Control of Dispersivity

of Soil using Lime and Cement. International Journal of Geology. 3 (1), 8-16.

U. S. Dept. Agriculture (1993). Soil Survey Handbook 18. United States: U. S. Dept.

of Agriculture.

Utomo, W. H. and Dexter, A. R. (1981). Age hardening of agricultural top soils.

Journal of Soil Science. 32, 335-350.

Uzal, B., Turanli, L. Yücel, H., Göncüoğlu, M. C. and Çulfaz, A. (2010). Pozzolanic

activity of clinoptilolite: A comparative study with silica fume, fly ash and a

non-zeolitic natural pozzolan. Cement and Concrete Research. 40, 398–404.

Weatherley, L. R. and Miladinovic, N. D. (2004). Comparison of the ion exchange

uptake of ammonium ion onto New Zealand clinoptilolite and mordenite. Water

Research, 38, 4305–4312

Williams, D. B., Goldstein, J. I., and Fiori, C. E. (1986). Principles of X-Ray Energy-

Dispersive Spectrometry in The Analytical Electron Microscope. In: Edited by:

Joy, D. C., Romig, A. D., and Goldstein, J. I.. Principles of Analytical Electron

Microscopy. New York: Plenum Press, 123-154.

Xu, R.Q, Guo, Y. and Liu Z. Y. (2008). Mechanical Properties of Stabilized

Artificial Organic Soil. Front. Archit. Civ. Eng. China 2008, 2(2), 161–165

Yilmaz, B., Ucar, A., Oteyaka, B. and Uz, V. (2007). Properties of zeolitic tuff

(clinoptilolite) blended portland cement. Building and Environment, 42, 3808 -

3815.

Yu, T. R. (1997). Chemistry of Variable Charge Soils. London: Oxford University

Press.

288

Zainorabidin, A. (2001). Sifat-sifat Kejuruteraan Tanah Gambut Jenis Hemik di

Johor Barat. M. Eng. Thesis of Universiti Teknologi Malaysia.

Zhang, H. (1994). Organic matter incorporation affects mechanical properties of soil

aggregates. Soil and Tillage Research, 31 (2-3), 263-275.

Zhu, W., Chiu, C. F., Zhang, C. L. and Zeng, K. L. (2009). Effect of Humic Acid on

the Behaviour of Solidified Dredged Material. Canadian Geotech. J. 46, 1093-

1099.

PHYSICO-CHEMICAL AND MICROSTRUCTURE OF ARTIFICIAL … · Kebolehkesanan campuran kapur zeolit telah...

Documents

Transcript of PHYSICO-CHEMICAL AND MICROSTRUCTURE OF ARTIFICIAL … · Kebolehkesanan campuran kapur zeolit telah...