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Biofuel Extraction Techniques:
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Lalit Prasad
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Biofuel Extraction Techniques
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Biofuel Extraction Techniques
Edited by
Lalit Prasad
Subhalaxmi Pradhan
and
S.N. Naik
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Library of Congress Cataloging-in-Publication Data
ISBN 97811199829324
Background image: Green Algae; Somprasong Wittayanuakorn | Dreamstime.com

Biofuel Plant Storage: Patchamon Thainmanee | Dreamstime.com
Research Scientist: One Photo | Dreamstime.com
Biodiesel Production: Piyapong Thongdumhyu | Dreamstime.com
Cover design by Kris Hackerott
Set in size of 11pt and Minion Pro by Manila Typesetting Company, Makati, Philippines
Printed in the USA
10 9 8 7 6 5 4 3 2 1
Contents
Preface xix
1 Plant Seed Oils and Their Potential for Biofuel Production
in India 1
L. C. Meher and S. N. Naik
1.1 Introduction 1
1.2 Background 2
1.3 Non-Edible Oil as Feedstock for Biodiesel 4
1.3.1 Jatropha 7
1.3.2 Pongamia 10
1.3.3 Mahua 12
1.3.4 Nahor 14
1.3.5 Rubber 16
1.3.6 Lesser Explored Non-Edible Oils for Biodiesel
Feedstock in India 17
1.4 Fuel Qualities 17
1.4.1 Cetane Number 18
1.4.2 Acid Value 18
1.4.3 Ester Content, Glycerides, and Glycerol 18
1.4.4 Phosphorus Content 18
1.4.5 Iodine Value 19
1.4.6 Oxidation Stability 19
1.4.7 Linolenic Acid Methyl Esters 20
1.4.8 Polyunsaturated (≥ 4 Double Bonds) Methyl Esters 20
1.5 Conclusion 20
Author Contributions 21
References 21
2 Processing of Feedstock in Context of Biodiesel Production 25
Durgawati and Rama Chandra Pradhan
2.1 Introduction 26
v
vi Contents
2.2 Feedstock in Context of Biodiesel 28

2.3 Processing of Oilseeds 29
2.3.1 Pretreatment 30
2.3.2 Decortication 31
2.3.2.1 Characteristics of Oilseeds Required
for Decortication 31
2.3.2.2 Decortication Method 32
2.4 Oil Extraction Methods 34
2.4.1 Aqueous Method 34
2.4.2 Hydraulic Press 34
2.4.3 Ghani (Animal or Power-Driven) 35
2.4.4 Solvent Extraction Method 35
2.4.5 Mechanical Extraction Method 37
2.4.6 Microwave Assisted Oil Extraction 38
2.4.7 Ultrasonic Assisted Oil Extraction 39
2.4.8 Supercritical Assisted Oil Extraction 39
2.5 Catalyst 40
2.5.1 Homogeneous Catalyst 40
2.5.2 Heterogeneous Catalyst 41
2.5.3 Biocatalyst 42
2.6 Production Process of Biodiesel 42
2.7 Techniques for Biodiesel Production 44
2.7.1 Catalytic Transesterification Technique 44
2.7.2 Pyrolysis 44
2.7.3 Microwave Assisted 45
2.7.4 Ultrasonic Assisted 46
2.7.5 Supercritical Assisted 46
2.8 Advantages & Disadvantages of Using Biodiesel 47
2.9 Current Challenges and Future Perspectives
of Biodiesel 48
2.10 Summary 48
References 49
3 Extraction Techniques for Biodiesel Production 51
Soumya Parida and Subhalaxmi Pradhan
3.1 Introduction 51
3.2 Direct Use and Blending 53
3.3 Microemulsion 54
3.4 Pyrolysis 56
Contents vii
3.5 Transesterification 57
3.5.1 Homogeneous Catalyzed Transesterification 59
3.5.2 Heterogeneous Catalyzed Transesterification 64
3.5.3 Enzyme Catalyzed Transesterification 69
3.5.4 Supercritical Alcohol Transesterification 70
3.6 Intensification Methods for Biodiesel Production 73
3.6.1 Ultrasonic Method 73
3.6.2 Microwave Method 75
3.6.3 Cosolvent Method 77
3.6.4 Membrane Technology 78
3.6.5 Reactive Distillation 80
3.7 Conclusions 82
References 82
4 Role of Additives on Anaerobic Digestion, Biomethane
Generation, and Stabilization of Process Parameters 101
Adya Isha, Bhaskar Jha, Tinku Casper D’ Silva, Subodh Kumar,
Sameer Ahmed Khan, Dushyant Kumar, Ram Chandra
and Virendra Kumar Vijay
4.1 Introduction 102
4.2 Anaerobic Digestion Process 103
4.3 Metallic Additives 105
4.4 Alkali Additives 106
4.5 Biological Additives 106
4.5.1 Microorganisms 107
4.5.2 Enzymes 107
4.6 Carbon-Based Additives 108
4.6.1 Graphene 108
4.6.2 Carbon Nanotubes 109
4.6.3 Activated Carbon 109
4.6.4 Biochar 110
4.7 Nanoparticles 113
4.7.1 Fe Nanoparticles 113
4.7.2 Nanoparticles of Ag and ZnO 114
4.7.3 Nanoparticles of Fe2O4 114
4.8 Other Natural Additives 115
4.9 Conclusions 115
Acknowledgment 116
References 116
viii Contents
5 An Overview on Established and Emerging Biogas

Upgradation Systems for Improving Biomethane Quality 125
Tinku Casper D’ Silva, Adya Isha, Subodh Kumar,
Sameer Ahmad Khan, Dushyant Kumar, Ram Chandra
5.2 Available Biogas Upgradation Techniques 126
5.3 Microbial Methane Enrichment 128
5.4 Bioelectrochemical System 134
5.5 Photosynthetic Biogas Upgradation 137
5.6 Techno-Economics of Biological Biogas Upgradation
Technologies 140
5.7 Conclusion 141
Acknowledgement 142
References 142
6 Renewable Feedstocks for Biofuels 151
Monika Chauhan, Vanshika, Ajay Kumar, Diwakar Chauhan
and Arvind Kumar Jain
6.2 Sugar Containing Plant Crops 153
6.2.1 Sugar Cane (Saccharum officinarum) 154
6.2.2 Sugarbeet (Beta vulgaris L.) 155
6.2.3 Sweet Sorghum (Sorghum bicolor (L.) Moench) 155
6.3 Crops 156
6.3.1 Corn (Zea mays) 156
6.3.2 CASSAVA (Manihot esculenta) 158
6.4 Oilseed 159
6.4.1 Soybean (Glycine max) 159
6.4.2 Palm (Elaeis guineensis) 160
6.4.3 Canola Oil 161
6.4.4 Sunflower Oil 162
6.4.5 Castor Oil 162
6.4.6 Cottonseed Oil 163
6.4.7 Jatropha Oil (Jatropha curcas) 164
6.4.8 Jojoba Oil 165
6.4.9 NEEM (Azadirachta indica) 166
6.5 Lignocellulosic Waste 166
6.5.1 Sugarcane Bagasse 167
6.5.2 Rice Husk 168
6.5.3 Corn Stover 168
Contents ix
6.5.4 Wheat Straw 169

6.6 Sea Waste 170
6.6.1 Algae Biomass and Oil 170
6.7 Liquid Waste 171
6.7.1 Vinasse 171
6.7.2 Glycerol 171
6.7.3 POME (Palm Oil Mill Effluent) 172
6.8 Conclusion 173
References 174
7 Extraction Techniques of Gas‑to‑Liquids (GtL) Fuels 177
Sonali Kesarwani, Divya Bajpai Tripathy and Pooja Bhadana
7.2 History and Origin of Gas to Liquid Technology 178
7.3 What is Gas to Liquids (GtL) Fuel? 179
7.4 Need and Benefits from Gas to Liquid Technology 180
7.5 Extraction or Conversion Techniques of Gas
to Liquid Fuels 182
7.5.1 Gas to Liquid by Direct Conversion 183
7.5.2 Gas to Liquid by Indirect Conversion 185
7.5.2.1 Natural Gas Reforming or Methane
Reforming (Syngas) 185
7.5.2.2 Fischer-Tropsch (FT) Synthesis 188
7.5.2.3 Conversion 190
7.6 Advancements in Gas to Liquid Technology 196
7.7 Conclusions 197
References 198
8 Second Generation Biofuels and Extraction Techniques 207
Prashant Kumar, Praveen Kumar Sharma, Shreya Tripathi,
Deepak Kumar, Ashween Deepak Nannaware,
Shivani Chaturvedi and Prasant Kumar Rout
List of Abbreviations 208
8.2 Pre-Treatment of Lignocellulosic Biomasses 210
8.2.1 Physical Pre-Treatment Methods 211
8.2.2 Chemical Pre-Treatment Methods 212
8.2.3 Physico-Chemical Pre-Treatment Methods 214
8.2.4 Biological Pre-Treatment Methods 215
8.3 Extraction of Biofuel from Lignocellulosic Biomass 215
8.3.1 Pyrolysis 216
8.3.2 Hydrothermal Liquefaction 218
x Contents
8.4 Bioethanol 221

8.4.1 Aromatic Lignocellulosic Biomass as Potential
Candidate for Bioethanol 222
8.4.2 Enzymatic Saccharification 223
8.4.3 Ethanol Conversion Processes 224
8.4.4 Process for the Production of Ethanol from
Sugary Crops 226
8.4.5 Process for the Production of Ethanol from
Starchy Crops 226
8.4.6 Process for the Production of Bioethanol from
Cellulosic Biomass and Spent Aromatic Crops 226
8.4.7 Purification of Bioethanol 226
8.5 Biodiesel Production from Fatty Acids 227
8.5.1 Chemical Catalytic Process 227
8.5.1.1 Homogeneous Base-Catalysed
Transesterification 227
8.5.1.2 Homogeneous Acid-Catalysed
Transesterification 229
8.5.1.3 Heterogeneous Catalysts 230
8.5.1.4 Alkali Earth Metal Oxides 231
8.5.1.5 Acid/Base Zeolites 231
8.5.1.6 Heteropolyacids 232
8.5.1.7 Waste Biomass Derived Heterogeneous
Catalysts 235
8.5.1.8 Heterogeneous Nanocatalysts 236
8.5.2 Biochemical Catalysts 237
8.6 Levulinic Acid (LA) 240
8.6.1 Extraction of Levulinic Acid (LA) from Waste
and Lignocellulosic Biomass 240
8.7 Conclusions 244
References 245
9 Bio-Alcohol: Production, Purification, and Analysis Using
Analytical Techniques 257
Smrita Singh, Susanta Roy, Lalit Prasad
and Ashutosh Singh Chauhan
9.2 Biomethanol Extraction 259
9.2.1 Thermochemical Conversion Process 259
9.2.2 Biochemical Conversion Process 260
9.2.3 Anaerobic Digestion 261
Contents xi
9.3 Bioethanol Extraction 266

9.3.1 Extraction of Bioethanol from the Waste Flower
(Starchy Material) 266
9.3.2 Analytical Methods for Determination of Bioethanol 267
9.3.3 Bioethanol Extraction from Sugarcane 268
9.4 Biopropanol Extraction 269
9.5 Bioglycerol Extraction 271
9.6 Bioethylene Glycol Extraction 271
9.7 Branched-Chain Bioalcohols Extraction 271
9.8 Purification of Bioalcohol 272
9.8.1 Distillation 272
9.8.2 Adsorption 273
9.8.3 Ozonation 274
9.8.4 Gas Striping 275
9.8.5 Pervaporation 275
9.8.6 Vaccum Fermentation 276
9.8.7 Solvent Extraction 276
9.9 Quantification of Bioalcohols 277
9.9.1 Gas Chromatography (GC) 277
9.9.2 High-Performance Liquid Chromatography (HPLC) 278
9.9.3 Infrared Spectroscopy (IR) 279
9.9.4 Olfactometry 279
9.10 Recent Perspective of Bioalcohol Production 280
9.11 Conclusion and Future Trends of Bioalcohol 281
References 281
10 Studies on Extraction Techniques of Bio-Hydrogen 291
C. S. Madankar, Priti Borde and P. D. Meshram
10.2 Bio-Hydrogen Production Process 293
10.2.1 Fermentation 293
10.2.1.1 Dark Fermentation 293
10.2.1.2 Photo Fermentation 295
10.2.1.3 Sequential Dark and Photo
Fermentation 297
10.3 Bio-Photolysis 298
10.3.1 Direct Bio-Photolysis 299
10.3.2 Indirect Bio-Photolysis 300
10.4 Microbial Electrolysis Cell 301
10.5 Conclusion 303
References 304
xii Contents
11 Valorization of By-Products Produced During the Extraction

and Purification of Biofuels 307
Subodh Kumar, Tinku Casper D’ Silva, Dushyant Kumar,
Adya Isha, Sameer Ahmad Khan, Ram Chandra,
Anushree Malik and Virendra Kumar Vijay
11.2 Biodiesel Production Process and Its Byproducts 308
11.2.1 Valorization of De-Oiled Seed Cakes 310
11.2.1.1 Valorization of De-Oiled Cake
via Anaerobic Digestion Route 310
11.2.2 Valorization of Glycerol 312
11.2.2.1 Valorization of Glycerol via Anaerobic
Digestion Route 312
11.2.2.2 Valorization of Glycerol via Biological
Conversion Route 315
11.2.2.3 Valorization of Glycerol via Chemical
11.2.2.4 Valorization of Glycerol via Catalytic
11.2.2.5 Valorization of Glycerol via
Thermochemical Conversion Route 318
11.3 Biorefinery Concept Based on Utilization
of Whole Oilseed Plant 319
11.4 Valorization of Byproducts Obtained in the Bioethanol
Fermentation Process 321
11.5 Valorization of Byproducts Obtained in Anaerobic
Digestion Process 322
11.5.1 Valorization of CO2 Content in Biogas 323
11.5.2 Valorization of Digestate 324
11.6 Conclusion 325
Acknowledgment 325
References 325
12 Valorization of Byproducts Produced During Extraction
and Purification of Biodiesel: A Promising Biofuel 333
Gunjan, Radhika Singh and Subhalaxmi Pradhan
List of Abbreviations 334
12.2 Glycerol 336
12.2.1 Properties of Glycerol 336
12.2.2 Classifications of Glycerol 338
Contents xiii
12.2.3 Global Glycerol Market 339

12.2.4 Applications 340
12.2.4.1 Conversion of Glycerol into Value-Added
Product340
12.2.4.2 Oxidation 342
12.2.4.3 Hydrogenolysis 343
12.2.4.4 Pyrolysis/Gasification 343
12.2.4.5 Dehydration 344
12.2.4.6 Oligomerization/Polymerization 344
12.2.4.7 Etherification 344
12.2.4.8 Carboxylation 345
12.2.4.9 Transesterification/Esterification 345
12.3 Glycerol Carbonate 346
12.3.1 Applications of Glycerol Carbonates 347
12.3.2 Synthetic Routes of Glycerol Carbonate 348
12.3.2.1 Direct Synthetic Routes 349
12.3.2.2 Indirect Routes of Synthesis 350
12.3.3 Catalytic Production of Glycerol
Carbonate 352
12.3.3.1 Homogenous Catalysts 352
12.3.3.2 Enzyme as Biocatalyst 354
12.3.3.3 Heterogeneous Catalyst 355
12.4 Conclusions 357
References 358
13 Biofuel Applications: Quality Control and Assurance,
Techno-Economics and Environmental Sustainability 367
Sameer Ahmad Khan, Dushyant Kumar, Subodh Kumar,
Adya Isha, Tinku Casper D’ Silva, Ram Chandra
13.2 Solid Fuel 369
13.2.1 Applications of Briquettes 369
13.2.2 Biomass Briquettes 369
13.2.2.1 Ash Content 369
13.2.2.2 Moisture Content 373
13.2.2.3 Volatile Matter 373
13.2.2.4 Ultimate Analysis 374
13.2.2.5 Other Minor Elements 374
13.2.2.6 Calorific Value 374
13.2.2.7 Bulk Density 375
xiv Contents
13.2.2.8 Mechanical Durability 375

13.2.2.9 Environmental Sustainability and
Techno-Economics of Biomass Briquettes 376
13.2.3 Biochar Briquettes 376
13.2.3.1 Calorific Value 378
13.2.3.2 Moisture Content 379
13.2.3.3 Volatile Matter 379
13.2.3.4 Ash Content 379
13.2.3.5 Fixed Carbon 380
13.2.3.6 Granulation 380
13.2.3.7 Binder 380
13.2.3.8 Bulk Density 380
13.2.3.9 Burning Rate 380
13.2.3.10 Compressive Strength 381
13.2.3.11 Environmental and Techno-Economics
of Biochar Briquettes 381
13.3 Liquid and Gaseous Biofuel 382
13.3.1 Application of Liquid and Gaseous Biofuel 384
13.3.1.1 Combined Heat and Power (CHP)
Generation384
13.3.1.2 Heat Generation 385
13.3.1.3 Transportation Fuel 385
13.3.2 Bioethanol 386
13.3.2.1 Water Content 389
13.3.2.2 Ethanol and Methanol Content 389
13.3.2.3 Gum Content 389
13.3.2.4 Acidity 392
13.3.2.5 pHe 392
13.3.2.6 Appearance 392
13.3.2.7 Vapor Pressure 392
13.3.2.8 Relative Density/Specific Gravity 393
13.3.2.9 Copper, Sulfur, Benzene, Aromatics,
and Olefins 393
13.3.2.10 Environmental Sustainability
and Techno-Economics of Bioethanol 394
13.3.3 Biodiesel 395
13.3.3.1 Density and Viscosity 404
13.3.3.2 Sulphated Ash, Flash Point, and Carbon
Residue 404
Contents xv
13.3.3.3 Cold Flow Properties 405

13.3.3.4 Water, Sediment, and Total
Contamination 406
13.3.3.5 Copper-Strip Corrosion, Content
of Phosphorus and Metals 406
13.3.3.6 Distillation, Iodine Value, Oxidation
Stability, and Acid Value 407
13.3.3.7 Free Glycerine, Total Glycerine,
Cetane Number and Lubricity 407
and Techno-Economics of Biodiesel 408
13.3.4 Biogas 409
13.3.4.1 Biogas Analysis 411
13.3.4.2 Wobbe Index (WI) 412
and Techno-Economics of Biogas 413
13.4 Conclusion 414
Acknowledgment 414
References 414
14 Role of CO2 Triggered Switchable Polarity Solvents
and Supercritical Solvents During Biofuel Extraction 421
Anupama Sharma, Pinki Chakraborty, Karthikay Sankhyadhar,
Sandeep Kumar and Monisha Singh
14.2 Role of Solvent during Bio-Fuel Extraction 423
14.3 CO2 Triggered SPS for Extraction of Bio-Fuels 424
14.3.1 SPS for Production of Syngas 426
14.3.2 SPS for the Production of Biodiesel 427
14.3.3 SPS for the Production of Bio-Oil 428
14.3.4 SPS for the Production of Bio-Oil from
Antarctic Krill 429
14.4 Supercritical Solvents and Bio-Fuel Extraction 430
14.4.1 SC-CO2 in Extraction of Algal Bio-Oil 430
14.4.2 Supercritical Ethanol as Solvent in Extraction
of Bio-Oil from Sugarcane Bagasse 432
14.5 Challenges and Future Considerations 433
14.6 Conclusion 435
References 435
xvi Contents
15 Efficiency of Catalysts During Biofuel Extraction 441

Gajanan Sahu, Sudipta Datta, Sujan Saha,
Prakash D. Chavan, Deshal Yadav and Vishal Chauhan
15.2 Biofuels 444
15.3 Biodiesel 445
15.4 Transesterification Reaction 448
15.5 Catalyst Used for Biodiesel Extraction 450
15.5.1 Chemical Catalyst 451
15.5.1.1 Homogeneous Catalyst 451
15.5.1.2 Heterogeneous Catalyst 459
15.5.2 Biological Catalyst/Enzyme Catalyst 470
15.5.2.1 Free Lipase 475
15.5.2.2 Traditionally Immobilized Lipase 477
15.5.2.3 Lipase Immobilized on MNPs 478
15.5.3 Nanocatalyst 479
15.6 Catalyst Used for Bioalcohol Extraction 480
15.7 Conclusion 484
References 486
16 Microorganisms as Effective CO2 Assimilator
for Biofuel Production 495
Chandreyee Saha and Subhalaxmi Pradhan
16.2 Microorganisms as Carbon Dioxide Assimilators 497
16.2.1 Algae 498
16.2.1.1 Mechanism of Carbon Capture by Algae 498
16.2.1.2 Carbon Sequestration by Algae 500
16.2.1.3 Biosynthesis of Lipids by Algae 501
16.2.2 Cyanobacteria 502
16.2.2.1 Carbon Capture and Sequestration
by Cyanobacteria 502
16.2.3 Clostridia 503
16.2.3.1 Carbon Capture and Sequestration
by Clostridia 503
16.2.4 Proteobacteria 504
16.2.5 Archaea 505
16.3 Biofuel Production by Microorganisms
Using Carbon Capture 506
16.3.1 Biodiesel 507
Contents xvii
16.3.2 Bioethanol 509

16.3.3 Biobutanol 510
16.3.4 Biogas and Biohydrogen 511
16.4 Recent Advancements in Biofuel Production 512
16.4.1 Nano-Additives 512
16.4.2 Genetic Engineering 513
16.4.3 UV Mutagenesis 513
16.4.4 Nuclear Radiation Mutagenesis 513
16.4.5 Adaptive Laboratory Evolution 514
16.5 Conclusion 514
References 515
17 Global Aspects of Biofuel Extraction 523
Shilpi Bhatnagar and Shilpi Khurana
17.2 Biodiesel 524
17.3 Biogas 529
17.4 Bioethanol 534
17.5 Bio-Oil from Biomass 536
17.6 Conclusion 537
References 537
18 New Advancements of Biofuel Extractions and Future Trends 543
Rita Sharma, Kuldip Dwivedi, Bhavna Sharma
and Shashank Sharma
18.1.1 Major Advances in Production of Various
Generations of Biofuels 545
18.1.2 Conventional and Advanced Biofuels 545
18.2 Extraction and Purification of Biofuels 546
18.2.1 Sugar and Starch-Based Ethanol 546
18.2.2 Conventional Biodiesel 547
18.2.3 Biogas Production 548
18.2.4 Cellulosic Ethanol 549
18.2.5 Syngas 550
18.2.6 Advanced Biodiesel 550
18.3 Application of Biofuels 551
18.3.1 Energy Production 551
18.3.2 Transportation 551
18.3.3 Heat Production 552
xviii Contents
18.3.4 Charging Electronics 552

18.3.5 Clean Oil Spills and Grease 552
18.3.6 Cooking 552
18.3.7 Remove Paint and Adhesive 552
18.4 Advantages Associated with Biofuels 553
18.4.1 Fuel Efficiency 553
18.4.2 Effective 553
18.4.3 Durability of Vehicle Engine 553
18.4.4 Availability of Source 553
18.4.5 Renewable 553
18.4.6 Reduce Greenhouse Gases 553
18.4.7 Economic Security 554
18.4.8 Reduced Pollution 554
18.5 Disadvantages Associated with Biofuels 554
18.5.1 High-Cost Production 554
18.5.2 Monoculture 554
18.5.3 Fertilizer Usage 554
18.5.4 Industrial Pollution 555
18.5.5 Future Rise in Price 555
18.6 Future Trends 555
18.7 Conclusion 555
References 556
About the Editors 559
Index 561
Preface
Biofuels are viable alternatives to petroleum-based fuel because they are

produced from organic materials such as plants and their wastes, agri-
cultural crops, and their by-products. The development of cutting-edge
technology has increased the need for energy significantly, which has
resulted in an overreliance on fossil fuels. Renewable fuels are the subject
of research because of their biodegradability, eco-friendliness, decrease in
greenhouse gas (GHG) emissions, and favorable socioeconomic conse-
quences to counteract imitations of fossil fuels.
Depending upon their physical state, biofuels can be classified into
solid, liquid, or gas. Examples of solid biofuels are briquettes of biomass
and briquetted biochar. Liquid biofuels include bioethanol and biodiesel,
and gaseous biofuels include biogas and biomethane, among others. These
are only a few examples.
Different extraction techniques are used for the production of biofu-
els from renewable feedstocks. Biodiesel is a promising biofuel which is
produced by the transesterification of plant-based oils. Extraction of
oil includes older traditional methods, solvent extraction, mechanical
extraction, microwave-assisted, and ultrasonic-assisted methods. The sol-
vent extraction method is more efficient and produces good quality oil.
The limitation of this method is time-consuming and very tedious. Many
innovative techniques are also used to overcome the limitations of con-
ventional methods. Microwave-assisted and ultrasonic-assisted are some
of the new techniques which include the pre-treatment of the raw material
using either ultrasonic waves or radio waves which helps in increasing the
efficiency of the extraction of oil and improves the final quality of the oil.
This new book covers the prospects and processing of feedstocks for
biofuels, extraction techniques, catalysts and solvents used during pro-
duction of biofuel, optimization of reaction techniques, carbon captur-
ing during biofuel extraction, value addition to biofuel wastes, and their
techno-economic and environmental acceptability. A total of 18 chapters
are included in this book.
xix
xx Preface
Chapter 1 is an introductory part which covers different plant seeds and

their potential for biofuel production.
Chapters 2 and 3 cover the processing of feedstock in context of bio-
diesel production and extraction techniques for biodiesel production.
Chapters 4 and 5 include biomethane generation, stabilization of pro-
cess parameters, upgradation systems for biogas and improving biometh-
ane quality.
Chapters 6 and 7 cover renewable feedstocks for biofuels production
and extraction techniques of gas to liquids (GtL) fuels respectively.
Chapters 8–10 incorporate bio-alcohol, bio-hydrogen extraction, puri-
fication, and analysis.
Chapters 11–13 include valorization of by-products produced during
the extraction of biofuels, their purification, quality control, assurance,
techno-economics and environmental sustainability.
Chapters 14 and 15 include the role of supercritical solvents and cata-
lysts used during biofuel extraction and their efficiency.
Chapters 16 covers carbon capturing by microorganisms during the
biofuel extraction process.
Chapters 17 and 18 include global aspects, new advancements of biofuel
extractions and future trends.
It is expected that this book will spark the interest of numerous inves-
tigators in the academic universe towards biofuel research. It will provide
new information about the recent advancements in the extraction tech-
niques of biofuels, value addition to biofuel wastes and economic and envi-
ronmental acceptability, sustainability and viability.
1
Plant Seed Oils and Their Potential
for Biofuel Production in India
L. C. Meher1,2 and S. N. Naik1*
1
Centre for Rural Development and Technology, Indian Institute of Technology,
Delhi, Hauz Khas, New Delhi, India
2
Defence Institute of Bio-Energy Research, DRDO, Haldwani, Nainital,
Uttarakhand, India
Abstract
Many tree-borne oilseed plants are grown in India which produce non-food
grade oil. Some of these have the potential to produce feedstock for biodiesel.
Plants such as Pongamia and Jatropha are found throughout the country, whereas
Mahua, Rubber, and Nahor are found in specific regions. The oilseeds are collected
to a lesser extent by the local population for traditional uses as medicine, to fuel
lamps, etc. and for the preparation of soap in industries. The National Mission on
Biofuel has focused to grow Jatropha, whereas the existing tree born oilseeds are
also potential sources for biodiesel feedstock. Non-edible oils with their potential
as biodiesel feedstock in the country is discussed in this chapter. The oilseed plants
less explored for biodiesel have also been discussed.
Keywords: Biodiesel, vegetable oil, non-edible oil, transesterification, methyl

esters, jatropha, pongamia
1.1 Introduction
Presently, petroleum fractions are the preferred fuels for internal composi-
tion engines used for transport, as well as in the industrial and agricultural
sectors. The global consumption of fossil based liquid fuels was above 100
million barrels per day during 2019 and forecasted to continue at the same
rate during 2021 [1]. The contribution of CO2 to the atmosphere is about
*Corresponding author: snn@rdat.iitd.ac.in
Lalit Prasad, Subhalaxmi Pradhan, and S.N. Naik (eds.) Biofuel Extraction Techniques, (1–24) © 2023
Scrivener Publishing LLC
1
2 Biofuel Extraction Techniques
3.1-3.2 times the consumption of fossil fuel. The exhaust emissions as a

result of widespread use of fossil fuel are a global concern for the present
time. The level of unburnt hydrocarbon and oxides of nitrogen, along with
CO2, are gradually increasing in the atmosphere. The research and devel-
opment activities have been focused for the last few decades in search of
alternative fuel from renewable sources for the nations to be self-reliant
for energy sources and much effort is being done by countries with no oil
reserves.
Biodiesel is the fatty acid methyl esters derived from renewable lipid
feedstocks, such as vegetable oils, as an alternative to diesel fuel. The inven-
tion of diesel engines and compression ignition engines dates back to the
19th century and the vegetable oils were used as fuel. The high viscosity and
poor volatilities of vegetable oils, as well as the availability of middle dis-
tillate, i.e., diesel fuel, did not attract much interest for vegetable oil based
fuel during those days.
The research and development activities on vegetable oil based biodiesel
were initiated at the beginning of this century. The transesterification of
vegetable oil reduces the viscosity by one-tenth, lower molecular weight of
the triglyceride molecule by one-third, and improves the volatility along
with the physical properties of the biodiesel. Worldwide biodiesel indus-
tries are set up and biodiesel blended diesel fuel is technically suitable for
use in existing diesel engines with slight or no engine modifications. There
is a scarcity of biodiesel feedstock for countries like India where the domes-
tic demand of edible oil is met by import. The present article describes the
potential non-food grade vegetable oil sources as feedstock for biodiesel in
Indian context.
1.2 Background
India ranks third in terms of consumption of fossil fuels after China and
the USA. Consumption grew by 2.3% in 2019 with a global share of 5.8%.
Petroleum based fuel is the second largest energy source (239.1 million
tons oil equivalent) after coal (452.2 million tons oil equivalent). The trans-
portation fuel in India is mainly petroleum based diesel and the consump-
tion is recorded at 83.5 million tons during 2018-19 [2].
The recent BS-VI in India, effective from 2020, is a stringent emission
norm for diesel engines. The new pollution norm involves the reduction
of NOx by 68% and particulate matter by 82-93% [3]. The fuel for diesel
engines should burn clearly, which can be achieved by the inclusion of oxy-
genated fuel, i.e., biodiesel in petroleum based diesel fuel.
Oil Seed Plants for Biofuels 3
In the global context, the surplus of edible oils such as Rapeseed in

Europe, Canola in Canada, Soybean in the USA, and Palm oil in Malaysia
and Indonesia are the available feedstocks for biodiesel. In the Indian sce-
nario, the requirement of edible oil is met by import. India imports Palm
oil from Malaysia and Indonesia, and Soybean from Argentina and Brazil,
and Sunflower from Ukraine and Russia. The import of vegetable oil was
150.02 lakh tons during 2017-18, which increased to 155.49 lakh tons
during 2018-19 [4]. The import of edible oils for the last five years is shown
in Table 1.1 [5]. The non-food vegetable oils may be a potential source of
biodiesel feedstock.
There are over 300 different species of oilseed plants grown in India.
Various tree borne oilseed derived oils are not suitable for human con-
sumption due to the presence of toxic components, for example karanjin
and pongamol in Pongamia oil, azadirachtin in neem oil, ricin in Castor
oil, and phorbol esters in Jatropha oil. These tree-borne oilseeds require
agricultural inputs in the initial period and rarely require any expense asso-
ciated with its maintenance once fully grown. It can also be a cost-effective
way to produce oilseed. The production for tree borne oilseed is about 3.0-
3.5 million metric tons whereas 0.5-0.6 million tons of seed are collected
[6]. The potential non-edible oilseed plants are Jatropha (Jatropha curcas),
Karanja (Pongamia pinnata), Mahua (Madhuca indica), Nahor (Mesua
ferrea), Rubber (Hevea brasiliensis), Castor (Castor communis), Neem
(Azadirachta indica), Sal (Shorea robusta), Undi (Calophyllum inophyl-
lum), Simarouba (Simarouba glauca), etc. Oil derived from tree born oil-
seed plants such as Neem, Castor, and Sal find specific applications. Neem
oil containing azadirachtin is a natural pesticide and emulsifier in the agri-
cultural sectors. The Castor oil with ricinoleic acid in the triglyceride has
Table 1.1 Import of major edible oil by India (in Lakh Tons) [s].
Palm oil Soybean Sunflower
Year Crude Refined Crude Refined Crude Refined
2015-16 71.1 25.7 39.6 0.0 14.9 0.0
2016-17 53.6 29.4 34.6 0.0 17.3 0.0
2017-18 67.5 27.7 31.5 0.0 22.5 0.0
2018-19 64.2 25.2 31.7 0.3 25.8 2.0
2019-2020 30.2 19.0 16.8 0.2 10.8 0.0
(April-Sept)
high viscosity and finds commercial application as a precursor for polyure-

thane, lubricant, binder, etc. Fat derived from the Sal tree is used as cocoa
butter substitute for manufacturing of chocolates. With these exceptions,
the rest of the oilseeds may be feedstock for biodiesel.
Various missions at national and state levels were made to promote the
cultivation of oilseed crops. Pongamia and Jatropha were selected as suit-
able oilseed plants for plantation in the waste and degraded lands, ave-
nue plantations, and perimeter fencing. Massive plantation of Jatropha has
been carried out in the Chhattisgarh state and similarly, Pongamia in the
Karnataka state of India. These are in addition to the existing potential of
oilseed in the country.
1.3 Non-Edible Oil as Feedstock for Biodiesel

The biodiesel derived from vegetable oil should have properties as per EN
14214:2012 A1:2014 or IS 15607:2016 specifications. Properties such as
iodine value, linolenic acid methyl ester, and oxidation stability are depen-
dent upon the qualities of the feedstock. The physico-chemical properties
of oils are listed in Table 1.2 [7, 8] and their fatty acid compositions in
Table 1.3 [7, 9–12]. The saponification value (SV) and the iodine value (IV)
are indicative of structures such as chain length of fatty acid and degree
of unsaturation of fatty acids in the triglyceride. The cetane index (CI) is
related to the saponification value and iodine value as per Equation (1.1)
and the cetane number (CN) is related to the cetane index as per Equation
(1.2) [9]. The MWoil (weight average molecular weight of the oil) is calcu-
lated from the saponification value as per Equation (1.3) and the require-
ment of methanol for transesterification is calculated based on the MWoil.
5458
CI 46.3 0.225 IV (1.1)
SV
CN CI 1.5 to 2.6 (1.2)
56100
MWoil (1.3)
SV
Table 1.2 Physico-chemical characterisation of potential non-edible oils for biodiesel feedstock.
Physical appearance at Iodine Saponification Unsaponifiable
Sl. no. Oil room temperature Acid value value value matter (%)
1. Jatropha Yellowish clear liquid 5-8 93-107 188-196 0.4-1.1
2. Pongamia Dark yellow to orange 1-11 85-90 185-195 3.0
clear liquid
3. Mahua Pale yellow with semi Up to 20 58-70 187-196 1-3
solid fat
4. Nahor Dark brown or red 100 87 193-209 2.9
viscous liquid
5. Rubber Dark brown liquid 84 131-148 190-195 1.83
Table 1.3 Fatty acid composition of potential non-edible oils for biodiesel
feedstock.
Percent fatty acid composition of oils
Rubber
Fatty acids Jatropha Pongamia Mahua Nahor seed
Myristic acid - - 0.13 2.72 -
(C14:0)
Palmitic acid 13.4 11.65 19.6 9.76 9.3
(C16:0)
Palmitoleic acid 0.3 - - - -
(C16:1)
Stearic acid 5.8 7.50 25.9 13.45 8.4
(C18:0)
Oleic acid (C18:1) 40.9 51.59 37.3 58.12 25.4
Linoleic acid 39.6 16.64 15.8 12.64 41.1
(C18:2)
Linolenic acid - - - - 15.3
(C18:3)
Arachidic acid - 1.35 0.21 3.14 -
(C20:0)
Eicosenoic acid - - 0.15 - -
(C20:1)
Behenic acid - 4.45 - - -
(C22:0)
Lignoceric acid - 1.09 - - -
(C24:0)
The non-edible oils have been reported to have unsaponifiable matters

and the lipid associates, as shown in Table 1.2, are required to remove these
either by pretreatment or post-transesterification process.
The industrial scale of biodiesel production units set up worldwide
employs homogeneous catalysts (methoxides or hydroxides of sodium or
potassium) for transesterification, which is an efficient and cost-effective
method for production of biodiesel in order to meet the fuel qualities as

per biodiesel specifications. Among the homogeneous alkali catalytic pro-
cess, sodium methoxide and potassium methoxide result in higher selectiv-
ity of the product with rare formation of byproducts [13]. The methoxide
catalyzed transesterification of vegetable oils requires a low reaction tem-
perature, about 60–65oC at atmospheric pressure, and the reaction is com-
pleted in a short reaction time. The methoxide catalyzed process results in
complete conversion of the triglyceride oil in order to ascertain that pro-
duced biodiesel attains methyl ester content > 96.5% and the free glycerol
and total glycerol within the limits specified by EN 14214 and IS 15607
biodiesel specifications. The catalytically active species is the methoxide
ion, which is generated by dissolution of hydroxides in methanol [9]. The
biodiesel feedstock, i.e., vegetable oil for the methoxide catalyzed trans-
esterification mush, have free fatty acid less than 0.1%, moisture less than
0.1%, and phosphorus content less than 10 ppm as per the requirements
specified by biodiesel manufacturers such as Lurgi and Desmet Ballestra
[9]. The phosphorus content in biodiesel is permissible up to 4 ppm, as
per revised specifications, and the pretreated oil should have the phospho-
rous content accordingly. The required specification of feedstocks may be
achieved by pretreatment of the crude vegetable oil. The feedstock of the
above mentioned specification, methanol, and catalyst sodium methox-
ide solution are allowed to act as the reaction vessel for transesterifica-
tion. The required molar ration of methanol to triglyceride is 3:1, whereas
100% excess methanol is used during the process in order to ascertain the
completion of reaction and the excess alcohol is recovered for further use.
The completion of reaction is necessary to have methyl ester content above
96.5% and the triglycerides and partial glycerides within the maximum
specified limit. The transesterification vessels are designed so that the reac-
tion is accomplished in two or three steps. The glycerol formed in between
the steps is removed and as a result, the reaction proceeds towards comple-
tion in a short time. The transesterification products are allowed to stand
so that glycerol is separated due to high polarity and density and the bio-
diesel layer containing excel methanol and the residual catalyst is further
washed and dried. The B-20 blend of biodiesel and diesel with a volume
ratio of 20:80 is being used in the unmodified diesel engines and the targets
are made to use B20 fuel as per the National Mission of Biofuels.
1.3.1 Jatropha
Jatropha (Jatropha curcas) is a shrub native to the tropical areas of Mexico
and Central America and is presently being naturalized in the different parts
of the globe as a potential plant to produce biodiesel feedstock. Jatropha is a

small tree that starts flowering after one year and the economic yield starts
after the third year of plantation. The plant starts flowering (Figure 1.1a)
during summer and monsoon and male and female flowers are produced
on the same inflorescence. The green fruits ripen, changing to yellow and
are dried to black, contain three seeds, and its shape resembles castor seeds
(Figures 1.1b and 1.1c). As an initiative for biodiesel in India, Jatropha
plantation was carried out in an area of about 0.5 million hectares of
low-quality wasteland [14]. Commercial scale plantations of Jatropha were
carried out in low-quality and degraded land in the state of Chhattisgarh
and the produced oil is being utilized as feedstock for biodiesel. The oil
content in the Jatropha seed varies from 24 to 40%. The major fatty acids
are palmitic acid, stearic acid, oleic acid, and linolenic acid, with the last
two accounting for more than 80% w/w. The physico-chemical qualities of
Jatropha oil are listed in Table 1.2 and the fatty acid composition is shown
in Table 1.3. The Jatropha oil contains phorbol esters generally known for
tumor promoting activities, making the oil toxic.
The preparation of biodiesel involves pretreatment to remove the fatty
acids. The homogeneous alkali-transesterification of pretreated Jatropha
oil is conducted where the hydroxide or methoxide of sodium or potas-
sium is used as catalyst. The post transesterification process involves the
separation of excess methanol, catalyst, glycerol, and moisture to get the
biodiesel. The fuel qualities of Jatropha based biodiesel have been reported
to be as per IS 15607 specifications. The high cetane number, favorable
fatty acid composition, and fuel qualities as per specifications make the
Jatropha a potential candidate for biodiesel feedstock and therefore, mas-
sive cultivation has been initiated in the country. The vulnerable qualities
of biodiesel are the oxidative stability and the acid value. Processes have
been developed to prepare biodiesel with low acid value [15] and enhanced
oxidative stability by suitable additives.
In India, the government initiated the National Mission on Biofuels in
2003 and selected Jatropha as a potential biofuel crop since the plant has a
low gestation period, hardy nature, is resistant to draught and flood, is not
browsed by cattle, and requires a small plant to collect seeds. It has been
observed that Jatropha cultivation lead to improved soil fertility, contrib-
uted to the reduction of soil erosion, helped in the rehabilitation of lands
through greening, and created jobs for the local population in the rural
areas.
(a)
(b)
(c)
Figure 1.1 (a) Jatropha flowers. (b) Jatropha fruits. (c) Jatropha seeds.
1.3.2 Pongamia
Pongamia (Pongamia pinnata) or Karanja is a fast-growing medium size
evergreen oilseed plant (shrub or tree) found throughout India as well as
in the sub-Indian continent. The plant is found in tropical and temper-
ate Asia, including Malaysia, Indonesia, Thailand, Japan, Australia, and
the Pacific Islands. The plant is quite hardy and adaptable to dry climates
and is used for afforestation in the dry and wastelands in Karnataka state.
The plant bears beautiful flowers (Figure 1.2a) and thus is preferred for
avenue plantation. The fruiting occurs during April-June (Figure 1.2b).
The mature fruits or pods fall on the ground and are also collected from
the tree. The ripe pods are elliptic and flat and contain one to two kidney
shaped brown kernels (Figure 1.2c). The estimated potential of Pongamia
oil has been reported to be 135,000 tons per year [8], whereas large scale
afforestation and avenue plantations have not been taken into account.
The kernel contains 27-39% oil, the yield is 24-27% in the mechanical oil
expeller. The major fatty acids are palmitic acid, stearic acid, oleic acid, and
linolenic acid, with the last two accounting for about 70% w/w.
The Karanja oil contains lipid associates, i.e., karanjin and pongamol,
and a few more flavonoids which make the oil un-suitable for human
consumption. The oil has been reported to treat various skin diseases, to
fuel lamps, and for manufacture of soap and fatty acids. The preparation
of Karanja based biodiesel has been reported since 1999 [10, 16–19]. The
biodiesel preparation from Karanja oil using heterogeneous catalyst was
also studied [20–22]. The biodiesel synthesis in pilot scale, fuel character-
ization, and cross-country trials of Karanja based biodiesel was initiated
by IIT Delhi. The free fatty acid FFA present in the Indian non-traditional
oilseeds and oils make the oil quality poor for industrial applications. The
FFA content depends upon the collection of the condition of seed collec-
tion, storage of oilseed, oil extraction process, etc. Karanja oil with high
FFA was made by the addition of oleic acid and acid catalyzed esterifica-
tion was studied. The lowering of FFA during the esterification is shown in
Figure 1.3. Further alkali-transesterification produces Karanja oil methyl
esters [19].
The National Mission of Biodiesel initiated by the Government of India
emphasized this as a potential plant for biodiesel along with Jatropha.
The large-scale plantation is carried out in the southern Indian states, i.e.,
Karnataka, for the purpose of biodiesel. The biodiesel had been used by the
state transport corporation with 26 B100 and 1500 B20 buses [23].
(a)
(b)
(c)
Figure 1.2 (a) Pongamia flower. (b) Pongamia pods. (c) Pongamia kernels.
45
40
Acid Value (mgKOH/g) 35
30 6.5 mgKOH/g
25 20 mgKOH/g
40 mgKOH/g
20
9.9 mgKOH/g
15
10
0
0 15 30 45 60 75 90 105 120
Time (Min)
Figure 1.3 Effect of FFA during acid catalyzed esterification of high FFA karanja oil.
1.3.3 Mahua
The Mahua (Madhuca indica) trees are found in the central part of India.
The matured plant with an age of about 8-10 years bears the flowers (Figure
1.4a) and the fruits (Figure 1.4b) and continue fruiting up to 60 years. The
mature fruits fall on the ground during May-July in northern Indian and
August-September in the south. Annual seer yield is 20-40 kg per plant
[24]. The ripe fruit contains a fleshy outer coat and 3-5 cm long elliptical
seed that is flattened on one side, as shown in Figure 1.3c, that contains
34-37% oil [8]. The estimated potential of Mahua oil is four lakh tons per
annum and finds use as an ointment and in rheumatism to prevent and
treat cracking skin during cold, for the production of lubricating grease,
fatty alcohols, and stearic acid [25]. The fatty acid composition reveals that
the oil contains more than 45% saturated fatty acid, i.e., palmitic acid and
stearic acid, and the rest is mainly oleic acid and linoleic acid. The sapo-
nins present in the oil are the toxic factor that make the oil unsuitable for
human consumption. The oil contains up to 20% free fatty acid [26–30]
and requires a two-step process where the free fatty acids are esterified to
methyl ester using acid catalysts such as H2SO4 followed by alkali transes-
terification. The Mahua oil methyl esters have high cetane number, 61.5, on
the other hand, the pour point is 21oC [27].
(a)
(b)
(c)
Figure 1.4 (a) Mahua flowers. (b) Mahua fruits. (c) Mahua seeds.
15
Molar Ratio of Butanol to Oil: 6:1
12 Reaction Temperature: 60°C
Reaction Time: 60 min
Stirring Speed: 500 rpm
FFA value (%) 9
0
0 0.5 1 1.5 2 2.5
Amount of H2SO4 %(w/w)
Figure 1.5 Butyl esterification of mahua oil, effect of FFA on percent of acid catalyst.
Kumar and Prasad [31] reported a two-step process to prepare Mahua

oil butyl ester. The first step involved the acid catalyzed esterification and
the free fatty acid FFA value reduced from 19.8% to 1.1%. The variation
of FFA with catalyst concentration during the first step is shown in Figure
1.5. It was followed by alkali-transesterification with butanol (alcohol to oil
molar ratio 6:1), 1.5% (w/w) KOH as catalyst, reaction temperature 80°C,
stirring rate of 500 rpm, and reaction time 90 min as optimized conditions
resulting in a 94.8% yield of butyl esters of Mahua oil.
The performance and emission studies on mahua oil methyl ester have
been reported with slight modification in the diesel engine. The B20
blend of Mahua based biodiesel with diesel fuel is efficient for the engine
[27]. The biodiesel derived from Mahua oil has oxidative stability [31]
as per EN14214 and IS 15607 specifications for biodiesel, whereas the
biodiesel derived from other non-edible oils require additive, i.e., syn-
thetic antioxidant, in order to attain the oxidation stability in terms of
induction period.
1.3.4 Nahor
Nahor (Mesua ferrea) is a beautiful evergreen tree with conical crown
found in the forests of north-east India, Karnataka, and Kerala [8].
The fruit contains round or conical brown seeds (Figures 1.6a, b, c). The
oil content in the kernel is about 70% and on the base of the seed it is
45%. The estimated annual potential of Nahor oil is 6,200 tons in Assam
and 680 tons in Kerala.
(a)
(b)
(c)
Figure 1.6 (a) Nahor flower. (b) Nahor seed. (c) Nahor kernel.
Nahor oil has been used as feedstock for the preparation of biodiesel
by alkali-transesterification [16]. The methyl esters from Nahor oil were
further subjected to distillation under a vacuum in order to get the methyl
esters fraction leaving the triglyceride and other partial glycerides. The
transesterification of Nahor oil with short chain alcohol such as methanol
and ethanol has been reported in the literature [32, 33]. Lipase-catalyzed
transesterification of Nahor oil with methanol has been reported in the
literature where the removal of free fatty acid is not required during its
conversion to biodiesel since the immobilized lipases are employed for
converting free fatty acid as well as triglyceride to methyl esters [34]. The
engine performance and emission characteristics from Nahor based bio-
diesel blended with diesel were studied. The B20 blend (20% Nahor methyl
ester with 80% diesel) produced identical results with that of diesel. The
B30, B40, and B50 are suitable blends to lower the emission of NOx, CO,
and unburnt hydrocarbons.
1.3.5 Rubber
Rubber (Hevea brasiliensis) is native to the Amazon and is being cultivated
in the state of Kerala with a potential of 4500 tons per year. The seed resem-
bles Castor in shape and is slightly larger in size. The seed deteriorates
quickly and the lipase present in the seed contributes to a sharp rise in the
free fatty acid and the acid value [35]. The oil contains lipid associates up to
1.83% [36]. It contains nearly one-fifth saturated fatty acid of C16 and C18,
more than 80% unsaturated C18-fatty acids, linolenic acid about 15%, and
varies up to 26%. The rubber seed oil contains lipase that causes gradual
hydrolysis of the oil during storage resulting in high acidic value of the oil.
The oil contains linamarin as a lipid associate, which on decomposition by
hydrolysis forms hydrogen cyanide and acetone and the oil is toxic [35].
The two-step process from preparation of biodiesel (methyl esters) from
high free fatty acid content rubber seed oil involving acid catalyzed ester-
ification followed by alkaline-transesterification has been reported in the
literature [37, 38]. The in situ method for synthesis of biodiesel from rub-
ber seed has been reported to improve the yield of biodiesel up to 91% by
acidic catalyst [39] and up to 96% using alkali catalyst [40]. The oil con-
taining 39% free fatty acid has been converted to biodiesel by the use of
lipase as a biocatalyst with a yield above 99% at optimized conditions [41].
Studies have been conducted for conversion of rubber seed oil to methyl
esters by the use of heterogeneous catalysts [42, 43] in order to reduce the
losses due to unwanted reactions. The neat B100 biodiesel has been used
as fuel and the emission profiles of CO and CO2 were better compared to
diesel fuel. The specific fuel consumption in the case of B100 fuel was 10%
higher than diesel fuel and at low engine speed, the break thermal effi-
ciency of B100 was higher compared to that of diesel [44]. The rubber seed
oil is a potential feedstock for biodiesel.
1.3.6 Lesser Explored Non-Edible Oils for Biodiesel Feedstock

in India
In addition to the above discussed oilseed plants, there are many known
oilseed plants like Simarouba, Undi, Kukum, etc. Simarouba (Simarouba
glauca) originated from Central and South America and has been intro-
duced in India by the National Bureau of Plant Genetic Resources in 1960,
as the oil content in the seed is 60 to 75%. Flowering has been observed
4-6 years after plantation. The tree has the potential to produce 2000-
2500 kg oil per hectare per year. Calophyllum inophyllum (Undi) is an
evergreen plant of the tropics and grown in southern coastal India. The
five year old plant produces about 11-12 kg seed per year and gradually
increases to about 100 kg once the plant is 20 years old. The oil content in
the kernel is about 70%. Salvadora (Pilu) is a shrub that is grown in the
tropics of Asia and Africa. It matures in 8-12 years and produces 47,000
tons of seed per year. The kernel of Salvadora contains 35-50% oil and is
rich in saturated fatty acid, revealed from iodine value ~10 g iodine per
100g. Kokum (Garcinia indica) is a small evergreen oilseed plant found
in the forests of Western Ghats from Konkan to Mysore. A matured plant
produces 60-80 kg seed per tree per year and the seed contains about 44%
oil. Kusum (Schleichera trijuga) is another oilseed plant that grows to a
medium to large sized tree. The estimated annual potential of Kusum is
66,000 tons and the oil content is 51-62% in the seed. Similarly, many less
explored oilseed plants are in India which may collectively be a potential
source for biodiesel feedstock.
1.4 Fuel Qualities

The qualities of biodiesel listed in the specifications include the physical char-
acteristics as well as a few properties specific to vegetable oils. These prop-
erties and their limits in the latest specification IS 15607:2016 is discussed
under this section. The specifications for vegetable oil-based properties spec-
ified in IS15607:2016 are similar to those of EN14214:2012 + A1:2014.
1.4.1 Cetane Number

The cetane number of biodiesel should be at least 51. As discussed above,
the cetane number is dependent upon the structure of fatty acid methyl
esters derived from the oil, i.e., saponification value and iodine value of
the oil. The cetane number of Jatropha based biodiesel is above 57 and
expected to be higher in the case of Pongamia, Mahua, and Nahor oil-
based biodiesel. The biodiesel from rubber seed oil may not satisfy the
cetane number and the oil blended with an oil with low iodine value may
serve as a biodiesel feedstock.
1.4.2 Acid Value

The acid value is a parameter that is liable to increase and even exceed its spec-
ified limit upon storage for long times. The acid value of the biodiesel should
be less than 0.50 mg KOH/g, whereas the value is kept between 0.30-0.35 mg
KOH/g at the site of production. The acid value of biodiesel is dependent upon
the acid value of the feedstock before transesterification. The pre-treatment of
the oil should be done in order to lower the acid value of the oil below 0.2 mg
KOH/g to get biodiesel with the same or slightly higher acid value. The acid
value has been lowered up to 0.1 mg KOH/g in case of Jatropha based biodiesel
[45] and is possible with the rest of the feedstocks.
1.4.3 Ester Content, Glycerides, and Glycerol

The methyl ester content of the biodiesel should be at least 96.5% and the
same is being achieved in the industrial scale biodiesel manufacturing units.
It ascertains the formation of methyl esters, as well as the conversion of tri-
glycerides. The maximum permissible level of triglyceride, diglyceride, and
monoglycerides in the biodiesel are specified to be 0.7, 0.2, and 0.2% respec-
tively. The maximum limits of free glycerol and the total glycerol are spec-
ified to be 0.02 and 0.25%, respectively. All these parameters are achieved
during the transesterification and post-transesterification processes.
1.4.4 Phosphorus Content

The phosphorus content of biodiesel is specified to be less than 4 ppm. The
phosphorus content in the feedstock oil can be reduced by the process of
refining, involving degumming. The industrial process, i.e., degumming
using phosphoric acid is practised to efficiently reduce the phosphorus
content.
1.4.5 Iodine Value

Iodine value of biodiesel is an important parameter and should be less than
120g iodine/100g. The iodine value of the oil remains unchanged during
the conversion to biodiesel. The iodine value is an important parameter
related with the cetane number and oxidative stability. The iodine value
of rubber seed oil is higher than the required level and the oil needs to be
blended with low iodine value oil to make the feedstock suitable for pro-
duction of quality biodiesel. The other oils discussed have iodine value in
accordance with the requirement.
1.4.6 Oxidation Stability

The induction period should be more than or equal to 8 hours when the
biodiesel is subjected to 110oC at an air flow of 10 litre per hour. The sta-
bility is dependent upon unsaturation in the methyl ester since the allylic
hydrogen are reactive and initiate free radical reactions. Suitable synthetic
antioxidants such as pyrogallol, propyl gallate, tert-butylhydroxyquinone,
3-tert-butyl-4-hydroxyanisole, and 2,6-di-tert-butyl-4-methyl-phenol are
required to achieve the required oxidative stability.
The effect of synthetic antioxidants on the oxidative stability of Karanja
oil has been reported by Meher et al. [46]. The biodiesel was prepared
at the optimized reaction conditions of catalyst 1% KOH, methanol/oil
35
30
PY
Induction Period (h)
25 PG
BHA
20 TBHQ
15 BHT
10
0
0 100 200 300 400 500
Antioxidant Concentration (ppm)
Figure 1.7 Effect of antioxidant concentration on oxidative stability of karanja oil methyl
esters.
molar ratio 6:1, reaction temperature 65°C, and rate of stirring 600 rpm,
which yielded 97 to 98% of methyl esters. The oxidative stability has been
improved significantly in the case of pyrogallol as the additive and 50 ppm
of pyrogallol is sufficient to attain required stability, as depicted in Figure
1.7.
1.4.7 Linolenic Acid Methyl Esters

The linolenic acid methyl esters should be less than 12% in biodiesel and
this is related to the stability of the product. The same is nil in the case of
Jatropha, Pongamia, Mahua, and Nahor oil, whereas rubber seed oil con-
tains up to 15.3%.
1.4.8 Polyunsaturated (≥ 4 Double Bonds) Methyl Esters

The polyunsaturated fatty acids having double bonds more than or equal
to four are nil in the case of the non-edible oils discussed in this article
and all these oils satisfy the maximum permissible limit. The parameter is
specified as it is related with ensuring the oxidative stability.
1.5 Conclusion
The Indian non-edible oils discussed here are suitable feedstocks for bio-
diesel. The oils from Jatropha, Pongamia, Mahua, and Nahor are suitable
feedstock for biodiesel, whereas the feedstock with iodine value >120 g
iodine/100g and linolenic acid content >15% needs to be blended with low
iodine value feedstock such as Palm stearin (Iodine value 35 g iodine/100g)
or Mahua oil to make a feedstock technically suitable to prepare biodiesel
in order to achieve qualities as per the specifications. In terms of large-
scale use, the non-edible oils are supposed to have less importance and
should be collected in order to be used as biodiesel feedstock. The activi-
ties of collection of these oilseeds are labour intensive. Most of these tree
borne oilseeds mature during or before monsoon, resulting in the wastage
of these oilseeds. The further plantation of these oilseed plants should be
done in the low-quality wastelands. The activities starting from plantation
to maintenance and harvesting requires manpower at the local rural level
and it will improve the socio-economic status of the rural populace.
Author Contributions
Dr. L. C. Meher has contributed for the literature review and the practical
experience gained during his doctoral degree and serves biodiesel indus-
tries in India on the research and development of biodiesel derived from
Pongamia, Palm, and Jatropha oil. He has been involved in the research
and development of the conversion of Indian non-edible oils to biodiesel
and to improve the qualities by use of suitable additives.
Prof. S. N. Naik has framed the overview of the book chapter with prac-
tical research experience on oleochemicals in the industries and at the
research institute. Prof. Naik has thoroughly checked and revised as per
the requirement to make the article in accordance with the topic of the
book chapter and done the proofreading.
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BY JAMES C. WILSON, M.D.
Next in order to alcohol, opium and morphine are habitually abused

to a greater extent than any other narcotic. Chloral is used in the
same way by a large number of individuals. Paraldehyde, cannabis
indica, ether, chloroform, and cocaine are also used to a less extent.
The scope of this article does not include the consideration of acute
poisoning by these drugs.
The habit of taking narcotics, whether medicinally or as a mere

matter of indulgence, is apt speedily to become confirmed. The
physiological dose more or less rapidly loses its power to affect the
nervous system in the ordinary way. Tolerance increases with
increasing doses, and in a comparatively short space of time
poisonous doses are taken with impunity as far as immediate danger
to life is concerned. The toxic effects of the poison are shown in
characteristic perversion of the functions of the nervous system and
of the mind. A condition is established in which the ordinary functions
of life are properly performed only under the influence of the habitual
narcotic, and in which its absence results in languor, depression, and
derangement of bodily and mental processes. The habit, once
established, thus makes for itself a constantly recurring plea for its
continuance. Especially is this true of opium and morphia.
Opium and Morphine.
Opium-eating is chiefly practised in Asia Minor, Persia, and India. It

is also prevalent in Turkey. It has been practised in India from very
ancient times. The prevalence of this habit in the East is probably
largely due to the restrictions placed upon the use of alcoholic
beverages among the Mohammedans, and to some extent also to
the long religious fasts observed by the Buddhists, Hindoos, and
Moslems, during which opium is often used to allay the pangs of
hunger. The prevalence of the opium habit in India is shown by the
fact that the license fees for a single year amounted to nearly five
hundred thousand pounds sterling. It is stated that in Samarang, a
town of 1,254,000 inhabitants, the average quantity of opium
consumed monthly is 7980 pounds. The town of Japava, with
671,000 inhabitants, consumed in fifteen days 5389 pounds of
opium. In 1850, 576,000 pounds of opium were imported into Java,
besides an unknown quantity smuggled.1
1 Archiv für Pharmazie, 1873, cited by Von Beck, Ziemssen's Cyclopædia, vol. xvii.
The habit is not confined to Oriental countries, but is also practised

in various forms in the West. It is by no means rare on the continent
of Europe. In certain districts of England, especially in Lincolnshire
and Norfolk, more opium is consumed than in all the rest of the
United Kingdom. Shearer2 states that the increase in the practice of
opium-eating among the workpeople of Manchester is such that on
Saturday afternoons the druggists' counters are strewed with pills of
opium of one, two, and three grains, in preparation for the known
demand of the evening. The immediate occasion is said to be the
lowness of wages, opium being used as a cheap substitute for
alcohol or as a food substitute, or with the view of removing the
effects of disease and depression. According to the same observer,
laudanum is more or less in use as a narcotic stimulant in the cotton-
spinning towns, where female labor is in requisition and is well paid.
Children are accustomed to it from their earliest infancy. Their
parents drug them with daily potions of Godfrey's cordial, Dalby's
carminative, soothing syrup, and laudanum itself, during the long
hours of their absence from home. While the habit of opium-eating
cannot be said to be generally prevalent in any part of the United
States, instances of it are frequently encountered in all classes of
society, and particularly among people of means and refinement.
The preparations employed in this country are crude opium, tincture
of opium or laudanum, camphorated tincture of opium or paregoric,
McMunn's elixir, Dover's powder, and the salts of morphia. All of
these preparations are used by the mouth; opium is very frequently,
especially among women of the better classes of society, habitually
taken in the form of suppositories; finally, the acetate and sulphate of
morphine are used by means of the hypodermic syringe. While it will
be necessary to point out some differences in the effects of these
drugs due to the preparation used or to the method in which it is
employed, the distinction between the opium habit and the morphine
habit, in itself an artificial one, will not be regarded in the course of
the present article.
2 Opium-smoking and Opium-eating, their Treatment and Cure, by George Shearer,
M.D., F. R. S.
Opium-smoking is chiefly practised by the inhabitants of China and

of the islands of the Indian Archipelago. It has been imported into
those countries where Chinese labor is largely employed. The
Chinese have transmitted it, to an extent which is fortunately very
limited, to the inhabitants of certain of our cities. Opium-smoking is
habitually practised in this country only among the more debased
orders of society.
SYNONYMS.—Opiophagia, Morphiopathy, Morphinism,

Morphinomania, Morphiomania, Morpheomania, are terms
occasionally employed to designate the opium or morphia habit.3
Landowski, Levinstein, Jouet, and others use the term morphinism to
denote the condition of the body; morphinomania, the condition of
the mind in chronic morphine-poisoning. This distinction may be
misleading. In effect, the pathological condition is complex, including
derangements both somatic and psychical.
3 The word morphiomania, used by writers, is contrary to all etymological rule
(Zambaco, De la Morphéomania, Paris, 1883).
ETIOLOGY.—A. Predisposing Influences.—Pain holds the chief place

among the influences which predispose to the formation of the opium
habit. By far the greater number of cases have taken origin either in
acute sickness, in which opium administered for the relief of pain has
been prolonged into convalescence until the habit has become
confirmed, or in chronic sicknesses, in which recurring pain has
called for constantly repeated and steadily increasing doses of
opiates. In view of the frequency and prominence of pain as a
symptom of disease, and the ease and efficiency with which opium
and its preparations control it, the remote dangers attending the
guarded therapeutic use of these preparations are indeed slight.
Were this not so, the number of the victims of the opium habit would
be lamentably greater than it is. In a considerable proportion of
cases of painful illness the relief afforded by opiates is attended by at
least some degree of malaise, nausea, vomiting, and vertigo—
symptoms which render the speedy discontinuance of the remedy
scarcely less desirable than the control of the pain for which it was
administered. Occasionally these symptoms are so distressing as to
render opium wholly inadmissible. In other instances each
successive dose is attended by an aggravation of the distress. More
commonly, especially in acute illnesses, decreasing pain may be
controlled by diminishing doses, thus rendering practicable entire
discontinuance of the drug before those modifications of the nervous
system, and especially before that tolerance for large doses, which
constitutes the beginning of the opium habit, are established. For
these reasons the use of opiates in acute sickness, if properly
regulated, is attended with but little danger. Far different is it,
however, in chronic painful illnesses. Here to procure relief by opium
is too often to pave the way not only to an aggravation of the existing
evils, but also to others which are often of a more serious kind.
Opium is at once an anodyne and a stimulant. The temptations to its
use are of a most seductive character. To the overworked and
underfed mill-operator it is a snare more tempting than alcohol, and
less expensive. It allays the pangs of hunger, it increases the power
of endurance, it brings forgetfulness and sleep. If there be myalgia or
rheumatism or neuralgia, and especially the dispiriting visceral
neuralgias so common and so often unrecognized among the poorer
classes of workpeople, opium affords temporary relief. The medical
man suffering from some painful affection, the worst symptoms of
which are relieved by the hypodermic injection of morphine, falls an
easy prey to the temptation to continue it—a danger increased by
the fact that he is too often obliged to resume his work before
convalescence is complete. Indeed, the self-administered daily
doses of physicians sometimes reach almost incredible amounts. To
women of the higher classes, ennuyée and tormented with
neuralgias or the vague pains of hysteria and hypochondriasis,
opium brings tranquillity and self-forgetfulness.
Of 100 cases collected by Jouet,4 the habit followed the therapeutic

use of morphine in 32 cases of ataxia, 24 of sciatica and other
neuralgias, 8 of asthma, 2 of dyspepsia, 4 of hypochondriasis, 2 of
madness, 9 of painful tumors, 2 of prostatic inflammation, 7 of
nervous conditions (not specified), 1 of peritonitis, 2 of periostitis, 1
of gastro-enteralgia, 4 of pleuritic pains, 1 of contracture, and 1 case
of hæmoptysis.
4 Étude sur le Morphinism chemique, Thèse de Paris, 1883.
The responsibility of the physician to his patient becomes apparent

when we reflect that with very few exceptions the opium habit is the
direct outcome of the use of the drug as a medicine.
The decade of life at which the opium habit is most common is

between thirty and forty. But it may be developed at any age. Even
infants are not rarely made the subjects of chronic opium narcotism
by the use of soothing syrups and other poisonous nostrums.
Sex in itself exerts very little influence as a predisposing cause.

Owing to collateral circumstances, the number of women addicted to
opium is greater than the number of men. Kane5 states that females
more frequently fall victims to these drugs than males, in the
proportion of three to one, and attributes this excess to the fact that
women more often than men are afflicted with diseases of a nervous
character in which narcotic remedies are used for long periods. This
observer suggests as an additional explanation the occasional
preference on the part of women for opium as a stimulant in place of
alcohol, its effects being less noticeable and degrading. On the other
hand, Levinstein observed in 110 cases 82 men and 28 women. He
does not, however, regard the conclusion that the use is more
common among men as warranted by these figures. The habit
resulted in these 110 cases from the following causes: In 20 men
and 6 women after acute affections; in 46 men and 17 women after
chronic affections, these diseases being in each instance
accompanied by great pain. One man began to use morphine as an
antiaphrodisiac. Either to produce mental excitement simply or to
cause forgetfulness of the ordinary cares of daily life, 15 men and 5
women indulged to an uncontrollable extent.
5 Drugs that Enslave, Philadelphia, 1881. I refer with pleasure to the early labors of
this observer. His later publications tell their own story.
Occupation has in some respects much to do in favoring the

development of the opium habit. Familiarity with the use of drugs
exerts a powerful influence. Of Levinstein's 110 cases, 47 occurred
in persons belonging to the medical profession or dependent upon it;
thus, 32 physicians, 8 wives of physicians, 1 son of a physician, 4
nurses, 1 midwife, and 1 student of medicine.
A predisposing influence of more importance than would at first sight

appear is found in sensational popular writings upon the subject. As
Kane has well said, “At the time in which De Quincey, Coleridge, and
Southey lived the people and the profession knew little of the opium
habit save among foreign nations. The habitués were few in number,
and consequently when De Quincey's article appeared it created a
most decided impression upon the popular mind—an impression not
yet effaced, and one which bore with it an incalculable amount of
harm. Men and women who had never heard of such a thing,
stimulated by curiosity, their minds filled with the vivid pictures of a
state of dreamy bliss and feeling of full content with the world and all
about, tried the experiment, and gradually wound themselves in the
silken meshes of the fascinating net, which only too soon proved too
strong to admit of breaking.” There can be no question that a
percentage of cases of the opium habit, small though it be, is even in
our day to be attributed to this cause.
Somewhat analogous in its etiological importance is the influence of

example upon persons of idle and luxurious habits. Nowhere in
Western countries, with the exception of the opium-smoking dens of
the Chinese and their depraved associates, are there public places
of resort devoted to the practice of the opium and morphine habits,
as there are in Turkey and the East. According to Jouet—whose
statements are corroborated by occasional statements in French
newspapers—the habitual injection of morphine is to-day, in France
at least, almost a matter of fashion. Landowski states that friendship
is occasionally pushed to the extent of the exchange of pretty
syringes in silver cases as presents, and that a patient received
upon his birthday a hypodermic syringe as a present from his sister.
Zambaco, whose observations were made at Constantinople, states
that among the Moslems the opium habitués prefer the crude drug,
either alone or associated with certain aromatic substances, such as
ambergris, canella, or saffron, which are used for their aphrodisiac
effect. These mixtures are prepared openly in the family, and carried
upon the person in the form of pills in rich boxes of gold and enamel
among the better classes. This observer further says that the ladies
of the better classes carry jewelled cases containing hypodermic
syringes and artistic flaçons for the seductive solution, and that they
avail themselves of favorable opportunities to take an injection of
morphine even when together.
In addition to the predisposing influences already mentioned, it has

been customary to regard insanity as a cause of the opium habit.
Laehr6 and Fidler7 have gone so far as to class the morphine habit
among the psychoses. This view appears to be no longer tenable.
The opium habit must be classed with the taste for alcohol,
gambling, avarice, and lust as among human passions. That nervous
subjects, invalids, and individuals wanting in moral and physical tone
are specially prone to it is obvious. It constitutes in these cases,
however, an expression of the morbid constitution rather than a
substantive affection in itself. In the same manner, the opium habit in
insane persons must be looked upon as an epiphenomenon of the
morbid mental condition.
6 Allgemeine Zeitschrift für Psychiatrie, 1872.
7 Jahresb. der Gesellschaft für Natur und Heilkunde, Dresden, 1876.
Levinstein has with reason insisted upon the essential difference

between the disturbances resulting from chronic poisoning by
alcohol, lead, arsenic, etc., and that produced by morphine. In the
former group the mental conditions are expressions of physical and
chemical alterations of the central nervous system, which, once
established, persist for an indefinite period, whereas in
morphinomania the troubles of the nervous system are chiefly
functional and of a transitory character. He regards the nervous
disorders developed from the prolonged use of morphine as the
result simply of depression of the nervous system, and the extreme
suffering experienced on the withdrawal of the regular dose to which
the subject has been accustomed as a trouble of innervation rather
than as a psychical derangement. This physical suffering and the
mental depression which accompanies it have their analogues in the
angina occasionally seen in paroxysmal affections of the heart, the
blood-vessels, and the respiratory organs. Certain it is that
individuals addicted to opium and morphine excesses in a high
degree not only frequently retain full possession of their intellect, but
occasionally achieve and maintain great distinction in professional
and scientific life. Furthermore, subjects of the opium habit,
notwithstanding the gravest mental disturbance manifested during
the continuance or upon the cessation of the habit, usually exhibit
when cured no further indication of mental disorder.
B. The Exciting Cause.—In addition to the usual constituents of

vegetable substances, mucilage, albumen, proteids, fat, volatile
substances, and salts of ammonium, calcium, and magnesium,
opium contains a number of alkaloids, two neutral substances, and
meconic acid. Some of the alkaloids are probably derivatives from
morphia. The three most important alkaloids are morphine, codeine,
and thebaine. The neutral substances are meconin and meconiasin.
Morphinæ hydrochloras, acetas, and sulphas, codeina, and
apomorphinæ hydrochloras are officinal in the United States
Pharmacopœia. Opium and its alkaloids act principally on the central
nervous system, and in mammals on the brain. The functions of the
nervous system, as Brunton has pointed out, are abolished in the
order of their development, the highest centres being the first
affected. In man the action of opium is chiefly manifested upon the
brain. With small doses a stage of excitement, attended by increased
activity of the circulation, augmented nervous energy, and under
favorable circumstances an agreeable languor, followed by quiet
sleep, constitute the effects of the drug; with larger doses, of from
one to two grains, the transient stage of excitement is followed by
deep sleep, the awakening from which is marked by headache,
nausea, and evidences of gastro-intestinal catarrh; with still larger
doses, of three grains or more, deep sleep is produced, which
speedily passes into coma. The drug has an especial action on the
vaso-motor system, which is manifested in its power to diminish
congestion and relieve inflammation. With the exception of the urine
and the sweat, the secretions of the body are diminished by opium.
The action of the drug upon the intestines varies with the dose. In
moderate doses it diminishes peristalsis and causes constipation; in
very small doses it increases peristalsis; in large doses peristaltic
action ceases. Morphine is eliminated unchanged by the kidneys. It
is eliminated also by the gastro-intestinal mucous membrane, having
been found in the stomach after hypodermic injection. The action of
opium and its derivatives, as that of other narcotics, is much
influenced by habit. In those accustomed to the drug large (and
sometimes enormous) quantities are required to induce the
characteristic manifestations. Not rarely these manifestations are
much retarded. The enormous amount of two pints of tincture of
opium has been taken in the course of a day; a female patient
afterward successfully treated by the writer took habitually for a long
period of time from ten to twelve grains of morphine per diem,
hypodermically. Diedriech8 assumes that a portion of the morphine
introduced into the organism is converted into oxydimorphine or
other analogous substances which have the property of
counteracting to some extent the toxic effects of the morphine.
8 Ueber oxydimorphine, Inaug. Diss., Göttingen, 1883.
Levinstein concludes as a result of experiments upon animals that
morphine, besides its influence upon the nervous system, exerts an
especial action upon two sets of organs: first, upon the digestive
tube; and second, upon the sudoriferous glands. Taken by the
mouth, it irritated the gastric mucous membrane. Whether taken by
the mouth or hypodermically, it diminishes the secretion of gastric
juice and the peristaltic movements of the intestine. These
disturbances serve to explain not only certain of the phenomena of
the opium habit itself, but even more fully some of the symptoms
manifested upon its discontinuance. The nausea, vomiting, and
constipation occurring during the continuance of the habit must be
looked upon as a result of the derangement of function of the gastro-
intestinal glandular apparatus and the chronic catarrh which
accompanies it. The abrupt discontinuance of the drug is followed by
the sudden return of functional activity, hence salivation, persistent
vomiting, anorexia, and diarrhœa.
The effects of habitual excesses in opium and morphine upon the

nervous system are in essential particulars the same. Upon the
functions of the digestive system and upon nutrition they differ to a
considerable extent. Opium, as a rule, soon produces gastro-
intestinal derangements of a marked kind. These derangements
consist in loss of appetite, enfeebled digestion, nausea, vomiting,
and constipation alternating with occasional diarrhœa. The anorexia
is usually persistent and of a high degree, and has much to do with
the development of the wasting which is so common and so marked.
The occasional excessive appetite for food manifested by opium-
eaters is of brief duration. Its gratification aggravates the functional
disturbances, provokes gastro-intestinal catarrh, and thus tends to
increase the general malnutrition. On the other hand, morphine is
much better borne. At the present time almost all morphine habitués
use the hypodermic syringe, and, notwithstanding the elimination of
the drug in part by the gastric mucous membrane, thus escape in
part its evil effects upon the organs of digestion, and remain for a
long time, often despite enormous excesses, free from the nutritive
disturbances which are almost characteristic of the habitual abuse of
crude opium.
SYMPTOMATOLOGY.—The symptoms of the confirmed opium habit may
be divided into two principal groups: first, the symptoms of chronic
opium- or morphine-poisoning; and second, the symptoms due to the
withdrawal of the drug.
I. Symptoms of Chronic Poisoning.—A considerable percentage of

the individuals addicted to the opium habit preserve for a longer or
shorter period of time the appearance of health; indeed, it is possible
for very large doses of opium to be occasionally taken by certain
individuals without appreciable impairment of the functions either of
the body or the mind. These cases must, however, be looked upon
as exceptional. It is estimated that from one-fourth to three-tenths of
the entire population of China are addicted to the habit of opium-
smoking. The statements of travellers concerning the effect of this
habit are somewhat conflicting. When practised within bounds it
appears to resemble in its effects the moderate use of alcoholic
stimulants, increasing the ability to endure fatigue and diminishing
for a time the necessity for food. In moderation it appears to have
little injurious effect upon the general health. On the other hand, in
the greater number of individuals the confirmed opium habit causes
in a variable period of time symptoms of the most decided character;
the appetite and general nutrition fail; emaciation is often rapid,
commonly marked, and sometimes extreme. There are thirst and
anorexia; a little later the patient begins to suffer from nausea with
occasional vomiting. At this time a loathing for food alternates with
boulimia. These occasional excesses in food are followed by
epigastric distress, heartburn, and great mental depression. The skin
becomes relaxed, inelastic, and dull. Exceptionally, especially in
women who use morphine hypodermically, embonpoint is preserved
and the skin retains its normal tension and appearance. The
countenance is pale, muddy, and sometimes slightly cyanotic. There
is increased tendency to perspiration. Acne and urticaria are
common. Herpes zoster is encountered with considerable frequency
among opium subjects. In cases in which morphine is administered
by means of the hypodermic syringe the resulting lesions of the skin
are of importance. If the habit be concealed or denied, they are of
diagnostic value. Not rarely they constitute serious affections in
themselves. They are of all grades, from mere inflammatory points to
coarse infiltration and ulceration. The wounds are frequently so thick
set over the greater part of a limb as to present the appearance of a
continuous eruption. In other cases scattered points of ulceration
occur or extensive surfaces are occupied by a series of ulcerations
varying in size from a split pea to an inch or more in diameter.
Purulent inflammation of the subcutaneous tissues, with burrowing,
also occurs. Numerous scars bear witness to the duration and extent
of the habit. These lesions are usually due to unclean needles and
impure solutions; in certain cases they are to be explained by the
peculiarities of the individual as regards the tendency to
inflammation of the integumentary structures; finally, instances are
related in which immunity from skin lesions has existed in spite of
rusty needles and carelessly kept solutions.
The expression of the countenance is sometimes dull, much more

frequently furtive and timid. The repetition of the dose renders it
eager and bright. The pupils are commonly contracted, sometimes
enlarged, and occasionally unequal. Diminished power of
accommodation is common, and diplopia has been occasionally
observed.
The action of the heart is often irregular and weak. Disturbances of

the vaso-motor system give rise to flushing of the face, irregular
sensations of heat over the body, and sweating. It is probable that
the albuminuria hereafter to be described is due to disturbance of the
circulation in the kidneys. The pulse is variable; it is sometimes tense
and full, sometimes small and thready, often irregular. The volume,
tension, and rhythm of the pulse depend largely upon the state of the
vaso-motor and general nervous systems. They vary according to
the periods of stimulation, following doses or the periods of
depression characterizing the intervals between the doses.
Palpitations occasionally occur. Respiration is, as a rule, normal.
Transient dyspnœa sometimes occurs after doses a little larger than
usual. Subacute bronchitis is common. The urine is often diminished
in quantity. Its specific gravity varies within extreme limits, being
influenced rather by collateral circumstances than by the dose of
opium or morphine consumed. In grave cases albuminuria occurs.
Casts of various kinds are also encountered. As Levinstein9 has
pointed out, these changes in the urine are often transitory,
disappearing upon the suppression of the opium habit.
9 La Morphiomanie, 2d ed., Paris, 1880.
In confirmed cases uric acid is increased and urea diminished. The

chlorides are also diminished in amount. Vesical irritation is likewise
common. It is apt to be accompanied by neuralgia of the urethra and
of the rectum. Strangury and retention of urine also occur in old
cases. These complications are often followed by vesical catarrh.
Derangements of the central nervous system are constant and

serious. The disorders which originally led to the use of opiates are
in many instances intensified. The temper is capricious, fanciful, and
discontented. There are giddiness, headache, and vertigo. Disturbed
sleep, irregular flying neuralgic pains, and hyperæsthesia also occur.
Spinal tenderness is occasionally encountered, with characteristic
painful spots. Reflex excitability is augmented, but in aggravated
cases the tendon reflexes are often impaired. Itching is common and
troublesome. It may be local or general. Trembling of the hands and
of the tongue also occurs. This tremor resembles in all particulars
the tremor of chronic alcoholism, and, as many individuals addicted
to the opium habit also abuse alcohol, it is not always easy to say to
which of these poisons the symptom in question is to be referred: it
may be due to their combined action. Disturbances of speech are not
very uncommon. Sleeplessness is troublesome, but absolute
insomnia is rare. The sleep which is obtained is late, irregular, and
unrefreshing. In several cases that have occurred under the
observation of the writer there has been habitual inability to sleep
during the night, the patients wandering about, occupying
themselves in attempts to read or write until toward morning, and
then, under the influence of repeated doses, falling into a more or
less profound slumber, which has often been prolonged till after
midday. The effects of the dose upon the mind are in the early
periods of the habit agreeable exhilaration, increased activity of
imagination, and stimulation of the powers of conversation. These
effects are sometimes manifested for a long period, and in many
instances the most brilliant conversation, and among professional
men and public speakers the ablest efforts, have followed the taking
of large doses of opiates, and been followed in turn by periods of the
most profound physical and mental depression. In the absence of
the necessity for intellectual effort, and in individuals incapable of it,
the mental condition produced by the dose is one of profound revery,
largely influenced by the mental organization of the subject. This
state is described, and in many particulars much exaggerated, in the
writings of De Quincey, Coleridge, and others.
The voluptuous play of the imagination ascribed to the action of the

drug by Orientals is for the most part absent among opium-takers in
this country. If present at all, it occurs only to a limited degree. The
corresponding fact is also worthy of note—namely, so long as the
habit is continued the depression between the doses is less
profound than that described as occurring in the East. One of the
mental peculiarities of individuals addicted to the opium habit is
secretiveness concerning their vice. Not infrequently, the real cause
of the grave derangements of health thus produced is wholly
unsuspected by the family or friends of the patient. When the habit is
suspected or admitted, the amount and frequency of the dose are
rarely fully known, patients almost invariably deceiving their friends
in regard to the particulars of their indulgence. Individuals above
reproach in other matters, and previously of unquestioned veracity,
lie without any hesitation in this matter. A patient under my care who
had secreted in her room a quantity of morphine when about to
undergo treatment, denied either having taken or then having in her
possession any opium or morphine whatever, using the expression,
“I call God to witness that I neither now have, nor have had since I
began the treatment, any preparation of opium or morphine
whatever.” Within ten minutes sixty quarter-grain pills of morphine
were discovered secreted under the bolster. This patient was a
devout, refined, and, in regard to other matters, a trustworthy person.
The functions of the reproductive organs both in the male and in the
female are seriously deranged. In the male sex enfeeblement of the
sexual function is manifested in all degrees, even to complete loss of
sexual desire and sexual power. In certain individuals opium and
morphine in moderate doses produce some increase of sexual
desire and power, which is, however, speedily lost on the
continuance of the habit. Some doubt exists whether this is of
psychical or physical origin—a question at once difficult to decide by
reason of the reticence of opium-habitués upon this subject, and
unimportant in itself. Levinstein makes the interesting statement that
in no cases coming under his observation did the wives of
morphomaniacs who had injected as high as fifteen grains of
morphine a day reach the full term of pregnancy for two years prior
to the treatment, notwithstanding the fact that they were still young,
that they had borne children before their husbands had become
addicted to morphine, and that they had not, up to the time of the
formation of the habit by their husbands, suffered from premature
accouchements.
Among women the morphine habit invariably produces derangement

of the menstrual function. Menstrual irregularity, both as regards time
and amount, is succeeded after a time by amenorrhœa. Vicarious
hemorrhages do not occur. Complete amenorrhœa is sometimes
established abruptly, and married women not infrequently suspect for
this reason that they have conceived. In several cases of this kind
under the observation of the writer the absence of enlargement of
the breasts, of alteration of the areola, and of softening of the os
after several months, indicated the improbability of these fears,
notwithstanding the irregular appetite, the morning vomiting, the
occasional palpitations and faintness, the hysterical condition, and
the mental peculiarities of the individuals—phenomena
unquestionably due to the action of the morphine itself. The
amenorrhœa of the morphine habit is associated with sterility—a fact
that renders probable the supposition that it is dependent upon
absence of ovulation. Women addicted to the opium habit are
capable of conceiving so long as menstruation persists, those only,
however, going to full term who use very moderate quantities. In
women using large doses abortion invariably occurs. The functional
integrity of the reproductive system is re-established upon the
permanent cessation of the habit. Women who are cured may again
menstruate regularly and may again bear children. Morphine in
women, as in men, is said to increase, when first habitually taken,
the capacity for sexual pleasure.
Levinstein and others have described certain febrile conditions

observed in individuals addicted to morphine. First, a form of
intermittent fever closely resembling malarial fever. This fever of
intermittent type occurs in individuals neither living in malarious
regions nor previously exposed to malaria. In addition to periodicity,
it presents other points of resemblance to malarial intermittent. The
earlier paroxysms cease after the administration of quinine. They are
favorably influenced by change of residence, and recur with intensity
after over-exertion, exposure, and upon the occurrence of acute
maladies. The favorable influence of quinine is only transient; the
febrile paroxysms recur after a time, notwithstanding the continued
use of the medicament. This fever disappears without special
treatment upon the discontinuance of the habit. It is more frequently
of the tertian than of the quotidian type. Its paroxysms are marked by
the symptoms of paludal intermittent. Neuralgias of various kinds,
especially supraorbital, intercostal, and præcordial neuralgias, are
apt to occur. The temperature during the paroxysm ranges from
102.5° to 104°. The area of splenic dulness is increased. More or
less mental and physical depression follows the paroxysm,
continuing in most cases through the period of apyrexia. These
observations require further confirmation. Secondly, confirmed
opium-habitués are peculiarly liable to transient febrile disturbances
from slight causes. Finally, ephemeral fever, ushered in by chills or
rigors and accompanied by headache, vertigo, thirst, malaise,
restlessness, and even mild delirium, and terminating with profuse
perspiration, occasionally occurs immediately after the injection of
large doses of morphine.
The course of the opium habit, when once established, is,

notwithstanding its occasional transient interruptions, gradual and
progressive. Certain individuals endure enormous doses of opium or
morphine for years without serious symptoms. In others moderate
doses give rise in the course of a few months to anorexia,
disturbances of nutrition, neuralgias, fitful and difficult sleep, and
serious mental derangement. These symptoms are usually
controlled by increasing doses and diminution of the intervals.
Finally, however, the drug fails to produce either excitement or
repose, and enormous doses are taken with but insignificant relief.
This is the period of grave derangement of the mental and physical
functions and of nutrition amounting to a true dyscrasia. The
phenomena are analogous to those produced by the withdrawal of
the dose. They are the symptoms of inanition, which in the absence
of well-directed and energetic treatment speedily terminates in
death.
II. Symptoms Due to the Withdrawal of the Drug.—Opium-habitués,

differing as they do among themselves in the manifestations of the
effects of the drug so long as it is freely taken, all alike develop
characteristic symptoms upon its speedy or gradual withdrawal. The
apparent immunity exceptionally observed now comes to an abrupt
termination. The nervous system, whether it has been accustomed
for months merely or for years to the influence of opiates, is upon
their withdrawal forthwith thrown into derangement of the most
serious and widespread kind. In the course of a few hours after the
last dose the steadying influence of the drug disappears. General
malaise is associated with progressive restlessness; the ability to
perform the ordinary duties of life gives way to profound depression
and indifference; præcordial distress, accompanied by cough, is
followed by insomnia, hallucinations, and sometimes by mania. The
habitual pallor of the face is replaced by deep flushing or cyanosis.
The heart's action becomes excited and irregular, then feeble; the
pulse, at first tense, becomes slow, thready, and irregular.
Colliquative sweats appear. Attacks of yawning and sneezing are
followed by convulsive twitching and trembling of the hands. Speech
becomes hesitating, drawling, and stuttering. Troubles of the
accommodation and even diplopia occur, often accompanied by
excessive lachrymation. Transient and varying differences in the
pupils are very frequent. Retinal hyperæsthesia may occur. In the
amblyopia occasionally observed in subjects of the opium habit the
ophthalmoscope reveals persistent anæmia of the retina. These
phenomena are associated with a sense of perfect prostration which
obliges the patient to take himself to his bed. Pain in the back and
limbs, followed by neuralgias, now occurs. Complete anorexia, with
easily-provoked or even causeless vomiting and persistent nausea
and diarrhœa difficult to control, adds to the gravity of the condition.
The abrupt discontinuance of the drug is followed in many individuals
by mental phenomena of a marked character: hallucinations,
illusions, and delirium continue for several days. The hallucinations
relate to all of the senses, but especially to those of sight and
hearing. The sense of smell is also occasionally affected, that of
taste rarely. Syncopal attacks occur. These are usually transient;
occasionally, however, profound syncope calls for the active
interference of the physician. Epileptiform seizures also take place.
Women who have previously suffered from hystero-epilepsy are
prone to the recurrence of severe paroxysms. Trembling of the limbs,
and especially of the lower extremities, rhythmical in time and often
violent, must be ranked among the more characteristic phenomena
produced by the abstinence from the drug. Sweating, although by no
means constant, is among the earlier and more persistent
phenomena. Urticaria occurs. Dyspnœa is common. Sometimes it is
provoked by exertion; sometimes paroxysmal shortness of breath
occurs spontaneously. Irritable cough is frequent. It is in many cases
unattended by râles. Pre-existing bronchitis is of course
accompanied by its characteristic signs and symptoms. Præcordial
distress, with palpitation and a sense of oppression, is common.
During the earlier days of abstinence the evidences of cardiac failure
are marked. Enfeeblement of the first sound, irregularity of the
heart's action, and intermission are common. The pulse phenomena
correspond to the heart's action. Thirst is a very frequent symptom. It
is often out of proportion to the loss of fluid by perspiration and
diarrhœa. The urine does not contain sugar. Salivation is rare and of
moderate degree. Nausea is persistent. Œsophageal spasm,
provoked by every effort to swallow, occasionally occurs and
constitutes a distressing symptom. Many patients also complain of
spasmodic contraction of the anus. Neuralgia of the testicles also
occurs. The cure of the opium habit is followed by rehabilitation of
the sexual power in the male and by menstrual regularity and
fecundity in the female. Levinstein has observed sexual
hyperæsthesia during the first weeks of abstinence in both sexes.
Albuminuria occurs in a large proportion of the cases. The albumen
shows itself, as a rule, from the third to the sixth day after the
discontinuance of the morphine, and disappears in the course of a
very few days. It is usually of slight amount.
The behavior of patients undergoing the suffering attendant upon the

abrupt, or even the gradual, withdrawal of the drug is variable. It
depends upon the mental and physical organization of the different
individuals and upon their ability to endure pain. Some rest quietly in
bed, enduring with fortitude suffering from which there is no escape;
others, silent, uncomplaining, and apathetic, present the appearance
of utter despair; a few, more fortunate than their fellows, lapse into a
condition of almost continuous drowsiness. In the greater number of
cases, however, these states of repose are but momentary or absent
altogether. Restlessness is continuous, and very often intense; the
patients are with difficulty kept in bed; if left to themselves they move
frantically about the room, moaning, bewailing their condition, and
begging the attendants for that which alone is capable of relieving
their distress. This condition gradually subsides, giving way to a
state of the most profound exhaustion. The exhaustion due to the
reaction of the nervous system deprived of the stimulus of the drug
is, on the one hand, favored by pre-existent derangement of the
nutritive processes, and on the other increased by the pain,
wakefulness, diarrhœa, and vomiting which accompany it. The
appearance of the patient is now most pitiable; the countenance is
blanched and pinched, the body occasionally drenched with sweat;
the heart's action is feeble, and the pulse thready and irregular. This
condition of collapse is usually of short duration, disappearing in
favorable cases under the influence of appropriate nourishment
administered in small quantities and with regularity. Where, however,
the gastric irritability is unmanageable, an increasing tendency to
collapse may threaten life. In rare cases suddenly-developed fatal
collapse has occurred at a later period in the treatment, even after
the patient has become able to take and retain food. The
restlessness does not, however, always subside in this manner. In a
considerable proportion of cases it increases. Hallucinations and
delusions occur, and a condition of delirium tremens, scarcely
differing from the delirium tremens of chronic alcoholism, is
established. Tremor is a constant phenomenon of this condition.
Sometimes the gravest symptoms of the suppression of the drug are
developed with great rapidity. Jouet relates a case of a patient at the
Salpêtrière who during a temporary absence from the hospital forgot
her syringe and solution; her return being delayed from some cause,
she, notwithstanding her struggles against the symptoms caused by
the want of her habitual dose, suddenly fell in the street, her
countenance haggard and anxious, her hands shrivelled, and her
whole body bathed in drenching sweat. She immediately became
maniacal, and demolished the glass and lamps of the coupé in which
she was taken to the hospital. No sooner had she received her
ordinary hypodermic dose than she recovered her usual quietude.
This patient was neither hysterical nor had she previously suffered
from nervous paroxysms. She was, however, accustomed to
administer to herself at four o'clock every day a large hypodermic
dose of morphine, and it was at a few minutes past four that the
above-described seizure occurred.
DIAGNOSIS.—The diagnosis of the opium habit is in many cases

attended with considerable difficulty. Many habitués, it is true, do not
hesitate to admit the real cause of their symptoms; others, while
seeking to conceal it, do so in such an indifferent manner that
detection is not difficult; but the greater number for a long time
sedulously conceal their passion, not only from their friends, but also
from the physician whom they consult voluntarily or at the solicitation
of those interested in them. If inquiries be made upon the subject,
they deny the habit altogether, often with vehement protestations. If
forced to admit it, they are very apt to misstate the amount employed
or the frequency of the repetition of the dose. As a rule—to which
there are, however, not infrequent exceptions—emaciation is
marked, appetite is diminished and variable, the pulse is small, the

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Biofuel Extraction Techniques:

Biofuels, Solar, and Other Technologies

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Library of Congress Cataloging-in-Publication Data

Background image: Green Algae; Somprasong Wittayanuakorn | Dreamstime.com

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2.2 Feedstock in Context of Biodiesel 28

5 An Overview on Established and Emerging Biogas

6.5.4 Wheat Straw 169

8.4 Bioethanol 221

9.3 Bioethanol Extraction 266

11 Valorization of By-Products Produced During the Extraction

12.2.3 Global Glycerol Market 339

13.2.2.8 Mechanical Durability 375

13.3.3.3 Cold Flow Properties 405

15 Efficiency of Catalysts During Biofuel Extraction 441

16.3.2 Bioethanol 509

18.3.4 Charging Electronics 552

Biofuels are viable alternatives to petroleum-based fuel because they are

Chapter 1 is an introductory part which covers different plant seeds and

Keywords: Biodiesel, vegetable oil, non-edible oil, transesterification, methyl

*Corresponding author: snn@rdat.iitd.ac.in

3.1-3.2 times the consumption of fossil fuel. The exhaust emissions as a

In the global context, the surplus of edible oils such as Rapeseed in

high viscosity and finds commercial application as a precursor for polyure-

1.3 Non-Edible Oil as Feedstock for Biodiesel

CN CI 1.5 to 2.6 (1.2)

The non-edible oils have been reported to have unsaponifiable matters

method for production of biodiesel in order to meet the fuel qualities as

of the globe as a potential plant to produce biodiesel feedstock. Jatropha is a

Kumar and Prasad [31] reported a two-step process to prepare Mahua

1.3.6 Lesser Explored Non-Edible Oils for Biodiesel Feedstock

1.4 Fuel Qualities

1.4.1 Cetane Number

1.4.2 Acid Value

1.4.3 Ester Content, Glycerides, and Glycerol

1.4.4 Phosphorus Content

1.4.5 Iodine Value

1.4.6 Oxidation Stability

1.4.7 Linolenic Acid Methyl Esters

1.4.8 Polyunsaturated (≥ 4 Double Bonds) Methyl Esters

Next in order to alcohol, opium and morphine are habitually abused

The habit of taking narcotics, whether medicinally or as a mere

Opium and Morphine.

Opium-eating is chiefly practised in Asia Minor, Persia, and India. It

The habit is not confined to Oriental countries, but is also practised

Opium-smoking is chiefly practised by the inhabitants of China and

SYNONYMS.—Opiophagia, Morphiopathy, Morphinism,

ETIOLOGY.—A. Predisposing Influences.—Pain holds the chief place

Of 100 cases collected by Jouet,4 the habit followed the therapeutic

The responsibility of the physician to his patient becomes apparent

The decade of life at which the opium habit is most common is

Sex in itself exerts very little influence as a predisposing cause.

Occupation has in some respects much to do in favoring the

A predisposing influence of more importance than would at first sight

Somewhat analogous in its etiological importance is the influence of

In addition to the predisposing influences already mentioned, it has

Levinstein has with reason insisted upon the essential difference

B. The Exciting Cause.—In addition to the usual constituents of

The effects of habitual excesses in opium and morphine upon the

I. Symptoms of Chronic Poisoning.—A considerable percentage of

The expression of the countenance is sometimes dull, much more