Handbook on Characterization of Biomass, Biowaste and Related By-products ||

Preface Contents Contributors 1 Biomass Categories Abstract 1.1 Introduction 1.2 Woody Biomass 1.2.1 Forest and Plantation Wood 1.2.2 Wood Processing By-products and Residues 1.2.3 Used Wood 1.3 Agricultural Residues and Waste 1.3.1 Crop Residues 1.3.2 Animal Dung 1.4 Municipal Waste 1.5 Sewage Sludge 1.6 Microalgae and Aquatic Plants 1.6.1 Microalgae 1.6.2 Aquatic Plants 1.7 Conclusion References 2 Generic and Advanced Characterization Techniques Abstract 2.1 General Introduction 2.2 Sampling and Storage 2.2.1 Sampling 2.2.2 Storage and Preparation 2.2.3 Example 2.3 Precision and Accuracy 2.4 Proximate Analysis 2.4.1 Moisture Content Analysis 2.4.1.1 Introduction 2.4.1.2 Standard Method: “Loss of Drying” 2.4.1.3 Chemical Determination 2.4.2 Volatile Matter Analysis 2.4.2.1 Introduction 2.4.2.2 Measurement Method 2.4.3 Ash Content Analysis 2.4.3.1 Definition 2.4.3.2 Method Issues During the Ash Content Determination Notes for Experimental Procedure: 2.4.4 Fixed Carbon Analysis 2.4.5 Examples of Proximate Analysis 2.5 Ultimate Analysis 2.5.1 CHNSO Analysis 2.5.1.1 Introduction 2.5.1.2 Principle of the Measurement 2.5.1.3 Oxygen Quantification 2.5.1.4 Sample Preparation Preparation of Solid Samples Preparation of Liquid Samples 2.5.1.5 Sample Analysis 2.5.1.6 Examples 2.5.2 Elemental Analysis by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) 2.5.2.1 Measurement Principle 2.5.2.2 Sample Preparation Open Digestion Closed Digestion Digestion Vessels Materials Sample Digestion for ICP-OES Analysis of Different Kinds of Samples Digestion Method Development 2.5.2.3 Sample Analysis 2.5.2.4 Examples 2.5.3 Elemental Analysis by X-ray Fluorescence (XRF) 2.5.3.1 Introduction 2.5.3.2 Analysis Principle 2.5.3.3 X-ray Fluorescence Intensity 2.5.3.4 Measurement Error 2.5.3.5 Sample Preparation 2.5.3.6 Semi-quantitative Measurement 2.5.3.7 Quantitative Measurement 2.5.3.8 General Comments 2.5.3.9 Examples Semi-quantitative Analysis Analysis with a Calibrated Method 2.5.4 Total Organic Carbon Analysis 2.5.4.1 Introduction and Principle of Measurement 2.5.4.2 Liquid Sample 2.5.4.3 Solid Sample 2.5.4.4 Commercial Apparatus 2.5.4.5 Examples 2.5.5 Halogen Analysis by Calorimetric Bomb-Ionic Chromatography Coupling 2.5.5.1 Introduction and Principle of Measurement 2.5.5.2 Ionic Chromatography 2.5.5.3 Procedure of Calorimetric Bomb-Ionic Chromatography Coupling Procedure for Combustion and Sample Preparation Determination of Dissolved Anions Cl−, Br− and F− by Liquid Ion Chromatography Equipment Calibration Analytical Series Calculation 2.5.5.4 Example 2.6 Thermal Analysis 2.6.1 Thermogravimetric Analysis 2.6.1.1 Introduction 2.6.1.2 Choice of Thermal Analysis Technique 2.6.1.3 General Description of TGA, TDA and DSC 2.6.1.4 Commercial Apparatus 2.6.1.5 Experimental Conditions Device Installation Signals Correction Atmosphere Crucible and Basket Temperature Program Importance of the Blank Curve 2.6.1.6 Sample Preparation 2.6.1.7 Examples 2.6.2 Kinetic of TG-DSC Analysis 2.6.2.1 Chemical Kinetics Modeling 2.6.2.2 Model-Free Methods—Isoconversional Methods Isothermal Data Non-isothermal Data Identification of the Reaction Mechanism {\varvec f}\left({\varvec \alpha}\right) Isothermal or Non-Isothermal Experiments 2.6.2.3 Model-Fitting Methods Selection of the Model Linear Regression Non-linear Regression Application 2.6.2.4 Deconvolution Procedures (Model-Free and Model Fitting Methods) 2.6.3 High and Low Heating Value Determination 2.6.3.1 Introduction 2.6.3.2 Bomb Calorimetry Description Controller Measuring Cell 2.6.3.3 Cooling Unit 2.6.3.4 Sample Preparation 2.6.3.5 Bases of Expressing Biomass Heating Value 2.6.3.6 Correcting for Extraneous Energy 2.6.3.7 Igniter and Combustion Aids 2.6.3.8 Acid Correction 2.6.3.9 Calibration of Bomb Calorimeter General Description Halogens Calculations During Calibration 2.6.3.10 Determining Heating Value Experimental Conditions Calculations During Experiments 2.6.3.11 Complete Combustion 2.6.3.12 Example 1: Agroforestry Species and Bio-based Industry Residues Introduction Sample Preparation Analysis Procedure Results 2.6.3.13 Example 2: HHV Analysis of Solid Recovered Fuel (SRF) Introduction Sample Preparation Analysis Procedure Calculation of HHV Results 2.6.4 Heat Capacity Measurement 2.6.4.1 Introduction 2.6.4.2 Heat Capacity Measurement by a Calorimeter Measurement Principle Apparatus Indicative Cp values Measurement and Precautions Programming of the Method Example: Cp Measurement of a WWT (Waste Water Treatment) Dry Sludge 2.6.4.3 Heat Capacity Measurement with Modulated DSC Introduction and Theory Apparatus Analysis Conditions Preparation of the Sample Analysis Method of Analysis Temperature Modulation Duration of the Isotherm Repeatability Recommendation Results Treatment Examples of Results 2.7 Physical Characterizations 2.7.1 Particle Size Distribution Determination Using Laser Scattering 2.7.1.1 Introduction 2.7.1.2 Principle of the Technique 2.7.1.3 Theory 2.7.1.4 Sphere of Equivalent Volume 2.7.1.5 Laser Granulometer 2.7.1.6 Sample Preparation and Analysis Type of Dispersion Sample Preparation Depending on Type of Dispersion 2.7.1.7 Making Accurate Measurements with a Laser Granulometer 2.7.1.8 Results Presentation 2.7.1.9 Examples of Results Liquid Dispersion: Characterisation of Sewage Sludge Before and After Digestion Solid Dispersion: Characterisation of Agricultural Residues in the Manufacture of Terracotta Products 2.7.2 Density Analysis 2.7.2.1 Introduction 2.7.2.2 Tap-Density Definition Apparatus and Principle of Measurement 2.7.2.3 Triple-Weighing 2.7.2.4 True Density Introduction Principle of Measurement Equipment Conditions for Analysis Sample Preparation Examples Example 1: Determination of the True Density of a Rice Sample Example 2: Determination of the True Density of a Coffee Powder Example 3: Determination of the Density of Maritime Pine Wood Chips 2.8 Physico-chemical Characterizations 2.8.1 Infrared and Ultraviolet—Visible Spectroscopies 2.8.1.1 Introduction to the IR and UV-Vis Spectroscopic Methods Electromagnetic Radiation Absorption of Radiation Absorption Spectrum 2.8.1.2 IR Spectroscopy Interest of IR Spectroscopy Different Vibrational Modes Infrared Active Bonds Factors Affecting the Vibrational Frequencies in IR The IR Absorption Range Apparatus Sample Techniques IR Spectroscopy Measurement by Transmission Mode IR Spectroscopy Measurement by Reflection Example of Infrared Spectroscopy Application 2.8.1.3 UV-Vis Spectroscopy Introduction to UV-Vis Spectroscopy Electronic Transitions Effect of Solvents on a UV-Vis Spectrum Conjugated Systems Measurement Quantitative Analysis Apparatus Light Sources Monochromator Sample Container Detectors Example of UV-Vis Spectroscopy Application 2.8.1.4 Raman Spectroscopy Introduction Theory Raman Analysis Method 2.8.2 Zeta Potential Determination 2.8.2.1 Introduction 2.8.2.2 Principle of Measurement of the Zeta Potential Electronic Double Layer Zeta Potential Measurement Electrophoresis 2.8.2.3 Application Apparatus and Sample Preparation Measurement Cell Experimental Protocol for Zeta Potential Measurement by the Titration Method Example of Measurement 2.8.3 Cation Exchange Capacity Determination 2.8.3.1 Introduction 2.8.3.2 Methods Method Using Ammonium Acetate Method Using Sodium Acetate Method Using Hexammine Cobalt Trichloride Method Using Barium Chloride Solution 2.8.3.3 Typical Values of CEC 2.8.3.4 Comparison of the Standard Methods for CEC Determination and Examples 2.8.4 Surface Acido-basic Composition Determination Using Boehm Titration 2.8.4.1 Introduction 2.8.4.2 Boehm Titration Method and Principle 2.8.4.3 Boehm Titration: Calculation of Acidic Sites 2.8.4.4 Issues During Boehm Titration: CO2 Dissolving and Release 2.8.4.5 Adaptations of Boehm Titration Procedure for Biochars and Related Pyrocarbons Solid Sample Pretreatment: Removal of Base-Soluble Acidic Compounds and Ashes Solid Sample Pretreatment: Barium Procedure 2.8.4.6 Experimental Recommendations Standardization of NaOH Solution Samples Containing High Amounts of Ashes 2.8.4.7 Examples 2.8.5 Determination of Polycyclic Aromatic Hydrocarbons (PAH) Content 2.8.5.1 Introduction 2.8.5.2 Measurement Methodology Part 1: Extraction of PAHs Extraction Method 1 (Acetone and Agitation) for Dry Samples Extraction Method 3 (Acetone and Agitation) for Wet Samples Extraction Method 2 (Toluene and Soxhlet) for Dry Samples Part 2: Identification and Quantification of PAHs Direct Preparation of the Extracts Preparation of the Extracts with Cleaning Procedures General Comments About the Analytical Techniques Analysis with GC-MS Analysis with HPLC 2.8.5.3 Example of Single and Total PAH Contents 2.8.5.4 PAH Bioavailability 2.8.6 Surface Area Determination Using Vapor Sorption 2.8.6.1 Introduction 2.8.6.2 Principles of DVS Measurement 2.8.6.3 Experimental Recommendations to Perform an Experiment Sample Pan Microbalance Vapor Solvent Partial Pressure Measurement for DVS Advantage 2.8.6.4 Defining a Method to Run an Experiment 2.8.6.5 Example of an Experiment 2.8.6.6 Characterization Options 2.8.6.7 Other DVS Instruments 2.8.7 Specific Surface Area and Pore Size Determination by Gas Adsorption 2.8.7.1 General Introduction to Gas Adsorption Definition of Specific Surface Area Definition of Porosity Adsorption Isotherm Applied Models 2.8.7.2 Apparatus Models and Suppliers Measurement Principle 2.8.7.3 Preparation of the Sample and the Measuring Cell 2.8.7.4 Sample Degassing Degassing Temperature Degassing Duration Required Vacuum Analysis Conditions Microporous Sample Gas Increments Number of Acquisition Points Equilibrium Time Dead Volume Non-microporous Sample Gas Increments Equilibrium Time Dead Volume Recommendations 2.8.7.5 Exploitation of the Results 2.8.7.6 Graphical Construction of Adsorption/Desorption Isotherm 2.8.7.7 Determination of the Specific Surface Area Langmuir Model BET Model Rouquerol transformation Application of the BET Model to Microporous Materials Application of the BET Model to Non-microporous Materials 2.8.7.8 Determination of Porous Volume and Pore Size Distribution of Microporous Materials t-Plot Method Basis of t-Plot method Calculation of the Thickness t Examples of Application of the t-Plot Method Limit of the t-Plot Method Horvath and Kawazoe Model Basis of Horvath and Kawazoe Model Procedure for the Application of HK Model 2.8.7.9 Determination of Porous Volume and Pore Size Distribution of Non-microporous Materials Introduction Principle Procedure for the Analysis of a Mesoporous Materials Using the BJH Model 2.8.7.10 Summary on Gas Adsorption Analysis 2.8.7.11 Examples 2.8.7.12 Microporosity Determination Using Carbon Dioxide Adsorption Isotherm Calculation from Density Functional Theory (DFT) Local Isotherms Calculation with Grand Canonical Monte-Carlo Model (GCMC) Pore size Distribution Examples and Experimental Recommendations 2.8.8 Determination of Macropores by Mercury Porosimetry 2.8.8.1 Principle of the Measurement 2.8.8.2 Penetrometer Choice of Penetrometer Calibration of Penetrometer Mercury 2.8.8.3 Analysis Sample Preparation Pressure Increments Program 2.8.8.4 Example 2.8.9 Temperature Programmed Techniques 2.8.9.1 Introduction 2.8.9.2 Instruments 2.9 Structural and Textural Characterization 2.9.1 X-Rays Diffraction (XRD) 2.9.1.1 Crystallography 2.9.1.2 Powder XRD Principle XRD Production Diffraction Instrumentation 2.9.1.3 Sample Preparation 2.9.1.4 XRD Powder Diffractograms 2.9.2 Pair Distribution Function (PDF) Analysis 2.9.2.1 Introduction 2.9.2.2 Basics of an Elastic Scattering Experiment 2.9.2.3 Data Collection 2.9.2.4 Producing the Pair Distribution Function 2.9.3 Scanning Electron Microscopy (SEM) 2.9.3.1 Introduction 2.9.3.2 SEM Characteristics: Resolution and Depth of Field Resolution Depth of Field Apparatus Electron Guns Electromagnetic Lenses Apertures Vacuum System 2.9.3.3 Imaging Principle 2.9.3.4 Field of View/Magnification, Resolution and Lens Aberrations in a SEM Field of View and Magnification Resolution Lens Aberrations 2.9.3.5 Interaction Between Electron Beam and Sample 2.9.3.6 Detected Signals and Corresponding Image Contrasts Secondary Electrons (SE): Topographic Contrast Back-Scattered Electrons (BSE): Chemical Contrast 2.9.3.7 Controllable Parameters Electron Beam Parameters Probe Diameter Probe Current The Accelerating Voltage Other Parameters Working Distance Frame Time/Scanning Speed (Signal-to-Noise Ratio) Contrast/Brightness 2.9.3.8 Sample Requirements and Preparation Sample and Vacuum Conditions Thermal Conductivity and Damage Electrical Conductivity and Charging Effect Sample Coating 2.9.3.9 Environmental Scanning Electron Microscope (ESEM)—Low Vacuum Scanning Electron Microscope (LV-SEM) ESEM Principle Environmental Mode and Imaging Resolution Example of Dynamic Observation: Heating Experiment Using Heating Stage Equipment Sample Requirement Parameters Under Control of the Operator Example Low Vacuum SEM Basic Operation Procedure for Imaging Sample Introduction and Field of View Selection Focus Adjustment Aperture Alignment Astigmatism Correction Chamber Pressure Adjustment in Environmental or Low Vacuum Mode Image Optimization Before Saving: Brightness/Contrast and Scan Speed 2.9.4 Energy Dispersive Spectroscopy (EDS) 2.9.4.1 Introduction 2.9.4.2 Theory 2.9.4.3 Spectrum Spectrum Structure Characteristic X-ray Nomenclature Energy and Intensities of X-ray Lines General Rules Effect of Accelerating Voltage on the Line Intensities 2.9.4.4 Equipment Main Components of an EDS Parameters Under Control of the Operator Time Constant and Dead Time Collection Time Spectral Artifacts Resolution Spatial Resolution Energy Resolution Accuracy and Detection Limit Accuracy Detection Limit Analysis Modes Qualitative Analysis Quantitative Analysis 2.9.4.5 Sample Preparation and Requirements for EDS Analysis Sample Preparation for Qualitative Analysis Specific Sample Requirement and Preparation for Quantitative Analysis Sample Must Be Homogeneous Sample Must Be Well Polished 2.9.4.6 Basic Procedures for EDS Analysis Check SEM Conditions Acceleration Voltage Working Distance (WD) Aperture and Spot Sizes Select the Analysis Mode: Point/area Analysis Select the Analysis Mode: Mapping or Line Scan 2.9.5 Micro-tomography 2.9.5.1 Introduction 2.9.5.2 Theory Beer-Lambert Law Inverse Radon Transform 2.9.5.3 Device of X-Ray Microtomography Conventional Experimental Device Monochromator Detector Architecture of an Industrial X-ray Tomograph (TIX) Acquisition System Image Reconstruction and Analysis System 2.9.5.4 Applications Thermal Test Mechanical Test 2.9.5.5 Illustration Comparison Between Observation Using SEM and X-Ray Microtomography Observation of Pore Size of Materials 2.9.6 Transmission Electron Microscopy 2.9.6.1 Introduction and Principle 2.9.6.2 Preparation of the Sample General Points Preparation of Biomass and Biowaste Sample for TEM Analysis Preparation of Sample for TEM from Char, Post-treated or not, Produced by Pyrolysis 2.9.6.3 Preliminary Procedure for TEM Characterization Introduction of the Sample Holder Into the Specimen Stage Focus the Sample TEM Analysis 2.9.6.4 TEM Operating Modes Conventional Imaging (Bright Field and Dark Field) Energy Dispersive Spectroscopy (EDS) Selected Area Electron Diffraction (SAED) High Resolution Transmission Electron Microscopy (HRTEM) Scanning Transmission Electron Microscopy (STEM) Electron Nanotomography 2.9.6.5 Examples of Sample Analysis 2.10 Mechanical Characterization 2.10.1 Thermomechanical Analysis 2.10.1.1 Introduction 2.10.1.2 Principle of the Measurement and Apparatus 2.10.1.3 Experimental Conditions Atmosphere Crucibles Probes Charges Samples Temperature TMA Correction Without a Sample 2.10.1.4 Instrument 2.10.1.5 Experimental Protocols 2.10.1.6 Examples and Exploitation of the Results TMA Analysis of a Refused Derivative Fuels (RDF) TMA Analysis of a Monolithic Ceramic Prepared from Clay and RDF 2.10.2 Compressive and Tensile Strength Analysis 2.10.2.1 Introduction 2.10.2.2 Apparatus Description 2.10.2.3 Sample Preparation 2.10.2.4 Test Procedure 2.10.2.5 Calculation 2.10.2.6 Example of Tensile Strength Measurement Sample Preparation Measurement Procedure Results 2.10.2.7 Example of Compressive Strength Measurement Sample Preparation Measurement Procedure Results 2.10.3 Flexural Resistance Analysis 2.10.3.1 Introduction 2.10.3.2 Apparatus Description Flexure Fixture Rollers/Three and Four Point Flexure Test Span Dimensions 2.10.3.3 Sample Preparation Cutting Polishing 2.10.3.4 Dimensions Measurement Number of Test Samples Test procedure 2.10.3.5 Calculations 2.10.3.6 Example of Flexural Strength Measurement Sample Preparation Measurement Procedure Results 2.10.4 Young Modulus Determination 2.10.4.1 Introduction 2.10.4.2 Impulse Excitation Technique 2.10.4.3 Sample Preparation Dimensions and Mass Measurements Recommendations 2.10.4.4 Test Procedure 2.10.4.5 Calculations 2.10.4.6 Damping 2.10.4.7 Example 1 on Young Modulus Measurement Sample Preparation Measurement Procedure Results 2.10.4.8 Example 2 on Young Modulus Measurement 2.11 General Conclusions References 3 Lignocellulosic Biomass Abstract 3.1 Introduction 3.2 Cellulose 3.2.1 General Description 3.2.2 Compositional Analysis Methods 3.2.3 Structural Analysis 3.2.3.1 Crystallinity Index of Cellulose 3.2.3.2 Degree of Polymerization 3.3 Hemicelluloses 3.3.1 General Aspect 3.3.1.1 Xylans 3.3.1.2 Mannans 3.3.1.3 Xyloglucans 3.3.1.4 Glucans 3.3.1.5 Arabinogalactans 3.3.2 Compositional Analysis 3.3.2.1 Hemicelluloses Content 3.3.2.2 Pentosan Content 3.3.3 Structural Characterization 3.3.3.1 Sugar Composition 3.3.3.2 Glucosidic Linkage 3.3.3.3 Uronic Acid 3.3.3.4 Acetyl Group Content 3.3.3.5 Degree of Polymerization 3.4 Lignin 3.4.1 General Aspect 3.4.2 Structural Characterization 3.4.3 Compositional Analysis Methods 3.5 Proteins and Lipids 3.5.1 Proteins 3.5.2 Lipids 3.6 Extractives 3.6.1 General Aspects 3.6.2 Compositional Analysis Methods References 4 Microalgal Biomass of Industrial Interest: Methods of Characterization Abstract 4.1 Introduction 4.2 Methods for Biomass Global Characterization 4.2.1 Introduction 4.2.2 Dry Weight Method 4.2.2.1 Centrifugation or Filtration 4.2.2.2 Washing the Biomass 4.2.2.3 Biomass Dewatering 4.2.3 Ash and Ash-Free Dry Weight Method 4.2.3.1 Classical Gravimetric Method 4.2.3.2 Thermogravimetric Analysis 4.2.4 Cell Counts Methods 4.2.4.1 Hemocytometry 4.2.4.2 Flow Cytometry 4.2.4.3 Image-Based Cytometry 4.2.5 Elemental Analysis 4.3 Methods for Protein Determination in Microalgae 4.3.1 Introduction 4.3.2 Applications of Algal Proteins 4.3.2.1 Human Nutrition 4.3.2.2 Industrial Application High Value Metabolites: Phycobiliproteins Functional Food-Ingredients Animal Feed Recombinant Proteins By-Product of Biofuel Consumption 4.3.3 Protein Extraction and Quantification 4.3.3.1 Pre-treatment Prior to Extraction 4.3.3.2 Protein Extraction 4.3.3.3 Protein Content Determination Total Nitrogen Content Colorimetric Methods Amino Acids Analysis Validation of Protein Quantification Methodology 4.3.3.4 Extraction and Purification of High Value Phycobiliproteins from Microalgae Phycoerythrin Phycocyanin 4.3.4 Proteomics 4.3.4.1 Gel-Based Approach Sample Preparation Protein Separation and Quantification Protein Identification and Characterization 4.3.4.2 Gel Free Approach 4.3.4.3 Obtention of Peptides and Identifying Proteins from Peptides Peptides Obtention Identifying Proteins from Peptides 4.3.5 Challenges and Future Perspectives 4.4 Methods for Polysaccharides Determination in Microalgae 4.4.1 Introduction 4.4.2 Polysaccharides Sampling and Extraction Strategies 4.4.2.1 Alcoholic Precipitation of Polysaccharides as Conventional Extraction Processes 4.4.2.2 Tangential Ultrafiltration Process for EPS Purification 4.4.2.3 Specific Treatments for the Extraction of Cell-Bound Exopolysaccharides 4.4.2.4 Specific Treatments for the Extraction and Quantification of Starch 4.4.2.5 Specific Treatments for the Extraction of Fibrillar Polysaccharides 4.4.3 How to Determine the Global Composition of Polysaccharides? 4.4.3.1 Total Carbohydrates 4.4.3.2 Uronic Acids and Neutral Sugars 4.4.3.3 Substituents and Non-carbohydrate Content 4.4.3.4 Identifying Groups by Infrared Spectroscopy 4.4.4 How to Determine the Monosaccharides Composition of Polysaccharides? 4.4.4.1 Preliminary Solvolysis 4.4.4.2 Chromatography 4.4.5 How to Elucidate the Branching Patterns of Polysaccharides? 4.4.5.1 Absolute Configuration Analysis 4.4.5.2 NMR Analysis 4.4.5.3 Mass Spectrometry Analysis 4.4.5.4 Conclusion 4.5 Methods for Lipids Determination in Microalgae 4.5.1 Preparation of Microalgal Samples 4.5.2 Analysis of Total Lipid Content 4.5.3 Separation and Analysis of Lipid Classes 4.5.4 Analysis of Fatty Acid Composition and Content 4.5.5 Hydrocarbon Analysis 4.5.6 Phytosterol Analysis 4.6 Methods for Pigments Determination in Microalgae 4.6.1 Extraction 4.6.1.1 Centrifugal Partition Extraction 4.6.1.2 Supercritical CO2 Extraction 4.6.1.3 Milking 4.6.1.4 Accelerated Solvent Extraction 4.6.1.5 High-Speed Homogenization 4.6.1.6 Microwave Assisted Extraction (MAE) 4.6.1.7 Sonication 4.6.1.8 Pulsed Electric Field 4.6.1.9 Enzyme Assisted Extraction 4.6.1.10 Bead Milling 4.6.1.11 Soaking 4.6.1.12 Instant Controlled Pressure Drop 4.6.1.13 Chemical Treatment 4.6.1.14 Others 4.6.1.15 Biorefinery 4.6.2 Pigment Analysis 4.6.2.1 Spectrophotometric Analysis 4.6.2.2 Other Techniques for Structural Characterization and Identification 4.7 Methods for Secondary Metabolites Determination in Microalgae 4.7.1 Introduction 4.7.2 Sampling and Preconditioning 4.7.3 Extraction Techniques 4.7.3.1 Cell Disruption 4.7.3.2 Secondary Metabolite Extraction Conventional Solvent Extraction Non-conventional Extraction Technique 4.7.4 Chemical Characterization 4.7.4.1 Chromatographic Techniques Thin Layer Chromatography (TLC) High Performance Thin Layer Chromatography (HPTLC) Gas Chromatography (GC) High Performance Liquid Chromatography (HPLC) 4.7.4.2 Spectroscopic Techniques Fluorescence Spectroscopy Nuclear Magnetic Resonance (NMR) 4.7.4.3 Hyphenated Techniques 4.7.4.4 Genome Mining 4.7.5 Summary Acknowledgements References 5 Methods to Assess Biological Transformation of Biomass Abstract 5.1 Introduction 5.2 Enzymatic Hydrolysis (Saccharification) 5.2.1 Fundamentals 5.2.2 Lignocellulosic Biomass 5.2.3 Starch-Based Biomass 5.2.3.1 Starch Swelling and Gelatinization 5.2.3.2 Starch Enzymatic Hydrolysis (Liquefaction and Saccharification) Starch Liquefaction (1st Enzymatic Hydrolysis) Starch Saccharification (2nd Enzymatic Hydrolysis) 5.2.4 Methods and Assays for Enzymatic Hydrolysis of Biomass 5.2.4.1 Preparation of Biomass for Compositional Analysis 5.2.4.2 Determination of Total Solids in Biomass 5.2.4.3 Determination of Ash in Biomass 5.2.4.4 Determination of Protein in the Biomass 5.2.4.5 Compositional Analysis of Biomass 5.2.4.6 Determination of Extractives in the Biomass 5.2.4.7 Determination of Structural Carbohydrates and Lignin in the Biomass 5.2.5 Theoretical Saccharification Potential 5.2.6 Enzymes Available and Activity Assays 5.2.6.1 Available Enzymes 5.2.6.2 Enzyme Activity Assays 5.2.6.3 Determination of Resistant Starch, Non-resistant Starch and Total Starch 5.2.7 Model of Enzymatic Saccharification 5.2.7.1 Cellulose Model 5.2.7.2 Starch Model 5.3 Biochemical Methane Potential (BMP) 5.3.1 Fundamentals: Anaerobic Digestion and BMP 5.3.2 Methods for BMP Measurement 5.3.2.1 BMP Measurement in Batch Anaerobic Reactors 5.3.2.2 BMP Assessment by NIRS Calibration 5.3.3 Ways to Interpret BMP Measurement (Index of Biodegradability, Kinetics Parameters, Modeling) 5.4 Biohydrogen Potential (BHP) 5.4.1 Fundamentals 5.4.2 Methods for BHP Measurement 5.4.2.1 Βioreactors Set-up 5.4.2.2 Substrate, Nutrients and pH 5.4.2.3 Inoculum Origin of Inoculum Pretreatment of Inoculum Substrate to Inoculum Ratio (S/I), F/M Ratio 5.4.3 Modelling 5.5 Respirometry 5.5.1 Fundamentals: Respiration and Biodegradation 5.5.2 Respirometric Methods 5.5.2.1 Classification Criteria of the Existing Respirometric Methods 5.5.2.2 Static Methods 5.5.2.3 Dynamic Methods 5.5.3 Respiration Indices for Biomass Biodegradability Determination 5.5.4 Modelling of Respiration Kinetics to Determine Biodegradability 5.5.4.1 Respirometric Modelling Based on a Simple Fractionation of the Biodegradable Organic Matter 5.5.4.2 Factors Influencing Kinetics 5.6 Assessment of the Agronomic Value of Organic Residues: Amendment and Fertilizer Potentials 5.6.1 Fundamentals: Why Assessing Carbon and Nitrogen Fate on Soil? 5.6.2 Methods for Organic Carbon and Nitrogen Mineralization Assessment: Laboratory Scale Soil Incubation 5.6.2.1 Substrate Preparation 5.6.2.2 Soil Preparation 5.6.2.3 Incubation for C Mineralization 5.6.2.4 Incubation for Nitrogen Mineralization 5.6.3 Modelling of Biological Tests 5.6.3.1 Carbon Mineralization Curves Models 5.6.3.2 Nitrogen Mineralization Models 5.6.3.3 Fast Analysis and Regression Models for Carbon Mineralization Indicator of Residual Organic Carbon Spectral Techniques References 6 Municipal Solid Waste Abstract 6.1 Sampling and Preconditioning 6.1.1 Sampling 6.1.1.1 Before Sampling: Pre-investigation General Description of the Area Under Investigation General Population Information and Waste Management Information 6.1.1.2 Sampling Process Design and Planning Sampling Strategy Number and Type of Strata Level of Sampling Determination of Sampling Unit, Number and Size Sampling Period 6.1.1.3 After Sampling: Execution and Evaluation of Waste Analyzis 6.1.2 Size Reduction 6.1.2.1 High-Speed, Low-Torque Grinders (The Hammer Mills) 6.1.2.2 Low-speed, High-torque Grinders (Shear Shredders) 6.1.2.3 MSW Size Reduction Equipment Operation and Selection 6.1.3 Separation 6.1.3.1 MSW Source Separation 6.1.3.2 MSW Automated Sorting Techniques 6.1.4 Drying 6.1.4.1 MSW Thermal Drying 6.1.4.2 MSW Bio-Drying 6.1.4.3 Selection of Drying Technologies and Equipment 6.2 Physical and Mechanical Characterization of Municipal Solid Waste 6.2.1 Physical Composition 6.2.1.1 Test Methods for Physical Composition 6.2.1.2 Studies on Physical Composition 6.2.2 Particle Size 6.2.3 Bulk Density 6.2.4 Moisture Content 6.2.5 Compressibility 6.2.6 Permeability 6.3 Chemical Characterization of Municipal Solid Waste 6.3.1 Elemental Composition 6.3.1.1 Definition 6.3.1.2 Analytical Methods 6.3.1.3 Elemental Composition of MSW 6.3.2 Biochemical Composition 6.3.2.1 Definition 6.3.2.2 Analytical Methods Total Organic Matter Fat Protein Starch Total Cellulose 6.3.2.3 Biochemical Composition of the Solid Waste 6.3.3 Mineral Composition 6.3.3.1 Definition 6.3.3.2 Analytical Methods X-Ray Diffraction Scanning Electron Microscopy (SEM) Transmission Electron Microscopy (TEM) Electron MicroProbe Analyzis (EMPA) Other Methods 6.3.3.3 Typical Mineral Composition of Municipal Solid Waste and Its Residues After Treatment 6.3.4 Heavy Metal Speciation 6.3.4.1 Definition 6.3.4.2 Analytical Methods 6.3.4.3 Heavy Metal Speciation of the Byproducts from MSW Treatment 6.3.5 pH 6.3.5.1 Definition 6.3.5.2 Analytical Methods 6.3.5.3 The pH of Municipal Solid Waste 6.3.5.4 The pH of by-Products of Municipal Solid Waste Treatment 6.3.6 Leaching Toxicity 6.3.6.1 Definition 6.3.6.2 Analytical Methods 6.3.6.3 Leaching Toxicity of Municipal Solid Waste 6.3.6.4 Leaching Toxicity of Residues from Municipal Solid Waste Incineration 6.4 Thermal Characterization of Municipal Solid Waste 6.4.1 Proximate and Ultimate Analyzis 6.4.1.1 Proximate Analyzis Standards Moisture Content Volatile Matter Ash Fixed Carbon 6.4.1.2 Ultimate Analyzis Elemental Analyzers Gas Chromatograph (GC) Configuration 6.4.2 Lower and Higher Calorific Value 6.4.2.1 Standards 6.4.2.2 Heating Value Background 6.4.2.3 Calorimetry 6.4.3 Loss on Ignition 6.4.4 Thermogravimetry/Thermogravimetric Analyzis (TGA) 6.4.5 Differential Scanning Calorimetry 6.5 Characteristics Database of Municipal Solid Waste 6.5.1 Physical and Mechanical Characteristics 6.5.2 Chemical Characteristics 6.5.3 Biochemical Characteristics 6.5.4 Thermal Characteristics References 7 Extraction and Characterization of Nanomaterials from Agrowaste Abstract 7.1 Introduction 7.2 Extraction of Cellulose Nanofibers (CNFs) 7.2.1 Cryocrushing Treatment 7.2.2 Grinding Procedure 7.2.3 Electrospinning Technique 7.2.4 Enzymatic Pretreatments 7.2.5 Ultrasonic Technique 7.2.6 Steam Explosion Coupled with Mild Acid Hydrolysis 7.2.7 Homogenization via High Pressure 7.3 Isolation of Cellulose Nanocrystals (CNCs) 7.3.1 Mechanical Size Reduction 7.3.2 Alkali Treatment 7.3.3 Bleaching Treatment 7.3.4 Acid Hydrolysis 7.4 Extraction of Chitin Nanofibers and Crystals 7.5 Extraction of Starch Nanoparticles 7.6 Characterization of Nanoparticles from Agrowastes 7.6.1 FTIR (Fourier Transform Infrared Spectroscopy) 7.6.2 XPS (X-Ray Photoelectron Spectroscopy) 7.6.3 Contact Angle Studies 7.6.4 Zeta Potential Measurements of Agro-Based Nanoparticles 7.6.5 Morphological Characterization of Agrowaste Based Nanoparticles 7.6.5.1 Atomic Force Microscopy (AFM) 7.6.5.2 Transmission Electron Microscopy (TEM) 7.6.6 Thermal Analysis of Agro-Based Nanoparticles 7.6.6.1 Nanocellulose and Micro Cellulose from Agrowaste 7.6.6.2 Cellulose Nanofibrils (CNF) 7.6.6.3 Nanocrystals and Nanofibers from Agrowastes 7.6.6.4 Kinetics Parameters 7.6.7 Small Angle Neutron and X-Ray Analysis of Agro-Based Nanoparticles 7.6.7.1 Small Angle Scattering Definition 7.6.7.2 Examples of SAXS and SANS Measurements 7.6.7.3 Dynamic Light Scattering Techniques of Agro-Based Nanoparticles 7.6.7.4 Dynamic Light Scattering Theory 7.6.7.5 Examples of DLS Measurements 7.7 Conclusion References 8 Food Waste and Manure Abstract 8.1 Generation of Food Waste and Manure and Need for Characterization 8.2 Introduction of Sampling and Preconditioning of Food Waste 8.2.1 Sampling Method 8.2.2 Sampling Conditioning Before Analysis 8.3 Physico-Chemical Characteriza Descripción del editor: "This book provides authoritative information, techniques and data necessary for the appropriate understanding of biomass and biowaste (understood as contaminated biomass) composition and behaviour while processed in various conditions and technologies. Numerous techniques for characterizing biomass, biowaste and by-product streams exist in literature. However, there lacks a reference book where these techniques are gathered in a single book, although such information is in increasingly high demand. This handbook provides a wealth of characterization methods, protocols, standards, databases and references relevant to various biomass, biowaste materials and by-products. It specifically addresses sampling and preconditioning methods, extraction techniques of elements and molecules, as well as biochemical, mechanical and thermal characterization methods. Furthermore, advanced and innovative methods under development are highlighted. The characterization will allow the analysis, identification and quantification of molecules and species including biomass feedstocks and related conversion products. The characterization will also provide insight into physical, mechanical and thermal properties of biomass and biowaste as well as the resulting by-products." (Springer)