Materials Innovations and Solutions in Science and Technology: With a Focus on Tropical Plant Biomaterials 3031266358, 9783031266355

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Advanced Structured Materials

Azman Ismail Fatin Nur Zulkipli Mohd Amran Mohd Daril Andreas Öchsner   Editors

Materials Innovations and Solutions in Science and Technology With a Focus on Tropical Plant Biomaterials

Advanced Structured Materials Volume 173

Series Editors Andreas Öchsner, Faculty of Mechanical Engineering, Esslingen University of Applied Sciences, Esslingen, Germany Lucas F. M. da Silva, Department of Mechanical Engineering, Faculty of Engineering, University of Porto, Porto, Portugal Holm Altenbach , Faculty of Mechanical Engineering, Otto von Guericke University Magdeburg, Magdeburg, Sachsen-Anhalt, Germany

Common engineering materials are reaching their limits in many applications, and new developments are required to meet the increasing demands on engineering materials. The performance of materials can be improved by combining different materials to achieve better properties than with a single constituent, or by shaping the material or constituents into a specific structure. The interaction between material and structure can occur at different length scales, such as the micro, meso, or macro scale, and offers potential applications in very different fields. This book series addresses the fundamental relationships between materials and their structure on overall properties (e.g., mechanical, thermal, chemical, electrical, or magnetic properties, etc.). Experimental data and procedures are presented, as well as methods for modeling structures and materials using numerical and analytical approaches. In addition, the series shows how these materials engineering and design processes are implemented and how new technologies can be used to optimize materials and processes. Advanced Structured Materials is indexed in Google Scholar and Scopus.

Azman Ismail · Fatin Nur Zulkipli · Mohd Amran Mohd Daril · Andreas Öchsner Editors

Materials Innovations and Solutions in Science and Technology With a Focus on Tropical Plant Biomaterials

Editors Azman Ismail Centre for Women Advancement and Leadership, Malaysian Institute of Marine Engineering Technology Universiti Kuala Lumpur Lumut, Perak, Malaysia Mohd Amran Mohd Daril Malaysian Institute of Industrial Technology Universiti Kuala Lumpur Masai, Johor, Malaysia

Fatin Nur Zulkipli School of Information Science, College of Computing, Informatics and Media Universiti Teknologi MARA Machang, Kelantan, Malaysia Andreas Öchsner Faculty of Mechanical and Systems Engineering Esslingen University Applied Sciences Esslingen am Neckar, Baden-Württemberg, Germany

ISSN 1869-8433 ISSN 1869-8441 (electronic) Advanced Structured Materials ISBN 978-3-031-26635-5 ISBN 978-3-031-26636-2 (eBook) https://doi.org/10.1007/978-3-031-26636-2 © The Editor(s) (if applicable) and The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 This work is subject to copyright. All rights are solely and exclusively licensed by the Publisher, whether the whole or part of the material is concerned, specifically the rights of translation, reprinting, reuse of illustrations, recitation, broadcasting, reproduction on microfilms or in any other physical way, and transmission or information storage and retrieval, electronic adaptation, computer software, or by similar or dissimilar methodology now known or hereafter developed. The use of general descriptive names, registered names, trademarks, service marks, etc. in this publication does not imply, even in the absence of a specific statement, that such names are exempt from the relevant protective laws and regulations and therefore free for general use. The publisher, the authors, and the editors are safe to assume that the advice and information in this book are believed to be true and accurate at the date of publication. Neither the publisher nor the authors or the editors give a warranty, expressed or implied, with respect to the material contained herein or for any errors or omissions that may have been made. The publisher remains neutral with regard to jurisdictional claims in published maps and institutional affiliations. This Springer imprint is published by the registered company Springer Nature Switzerland AG The registered company address is: Gewerbestrasse 11, 6330 Cham, Switzerland

Preface

This book describes the innovative idea and solution to the current issues discussed in diverse areas of research disciplines and industries. It covers a wide range of topics related to science, engineering, and technologies. The topics shared in this book will enable practitioners and innovators to develop subsequent novel ideas and methods for solving engineering and technological problems for organizations to sustain its operation in global challenges. Lumut, Malaysia Machang, Malaysia Masai, Malaysia Esslingen am Neckar, Germany

Azman Ismail Fatin Nur Zulkipli Mohd Amran Mohd Daril Andreas Öchsner

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Carbon Fibre Precursor from Oil Palm Biomass Lignin . . . . . . . . . . . Siti Khadijah Amran, Afiqah Liana Sazali, Norfahana Abd-Talib, Khairul Faizal Pa’ee, Mohd Razealy Anuar, and Tau-Len Kelly Yong 1.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1.2 Oil Palm Biomass . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1.3 Lignin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1.4 Conventional Lignin Refining Process . . . . . . . . . . . . . . . . . . . . . . . 1.5 Carbon Fibre . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1.6 Lignin as Carbon Fibre Precursor . . . . . . . . . . . . . . . . . . . . . . . . . . . 1.7 Deep Eutectic Solvent . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1.8 Lignin Isolation from Biomass Using DES . . . . . . . . . . . . . . . . . . . 1.9 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Potential Use of Nanotechnology to Reduce Postharvest Spoilage of Fruits and Vegetables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Abdallah Omar Hussein, Tong Woei Yenn, Leong Chean Ring, and Syarifah Ab Rashid 2.1 Food Spoilage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.1.1 Fruits . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.1.2 Vegetables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.2 Food Spoilage Caused by Microorganisms . . . . . . . . . . . . . . . . . . . 2.3 Food Sanitizers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.4 Nanoparticles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.4.1 Nanotechnology for Food Application . . . . . . . . . . . . . . . 2.5 Nanoencapsulation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

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Integrating a Hydrogen Fuel Cell in a Vehicle as a Hybrid for a Sustainable Energy Application . . . . . . . . . . . . . . . . . . . . . . . . . . . . Muhammad Amer Zahin Ahmad Dzaki, Ernie Mazuin Mohd Yusof, Siti Nor Zawani Ahmmad, Norziana Yahya, and Muhammad Remanul Islam 3.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3.2.1 Fuel Cell Process Flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3.2.2 Moving Driver Process Flow . . . . . . . . . . . . . . . . . . . . . . . 3.2.3 Communication Driver Process Flow . . . . . . . . . . . . . . . . 3.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3.3.1 The Prototype . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3.3.2 System Condition Status . . . . . . . . . . . . . . . . . . . . . . . . . . . 3.3.3 Analysis of Hydrogen Fuel Cell Reaction Time . . . . . . . 3.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Bio-Based Adhesive from Extracted Durian Seed Powder . . . . . . . . . Noor Faizah Che Harun, Muhamad Mohd Rosli, Mohd Aizuddin Shahmi A’zim, Haniza Kahar, and Mizah Ramli 4.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4.2.1 Preparation of Durian Seed Powder . . . . . . . . . . . . . . . . . . 4.2.2 Preparation of Bio-adhesive Without Roasting Raw Materials (Method A) . . . . . . . . . . . . . . . . . . . . . . . . . 4.2.3 Preparation of Bio-adhesive by Roasting Raw Materials (Method B) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4.2.4 Preparation of Bio-adhesive by Roasting Raw Materials with HCl (Method C) . . . . . . . . . . . . . . . . . . . . . 4.2.5 Preparation of Bio-adhesive by Roasting Raw Materials with HCl and H2 SO4 (Method D) . . . . . . . . . . 4.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Review of the Development of Palm Broom in Producing Food Packaging . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Mohamad Sazali Said, Jum’azulhisham Abdul Shukor, Mohamad Firdauz Mohamad Ridzuan, Muhammad Aman Azizi Saiful Azahar, and Muhammad Zikry Zamzuri 5.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

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Formulation of Emulsion Containing Chloramphenicol and Cinnamon Essential Oil for Topical Use . . . . . . . . . . . . . . . . . . . . . Siti Hajar Musa, Nurhanis Fasihah Muhamad, Fatin Fathia Mohd Ali, and Nur’Aisyah Rifhan Mohammad Shuhaimi 6.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6.2.1 Construction of the Calibration Curve . . . . . . . . . . . . . . . 6.2.2 Construction of the Ternary Phase Diagram . . . . . . . . . . . 6.2.3 Chloramphenicol Solubility Study . . . . . . . . . . . . . . . . . . . 6.2.4 Formulation of an Emulsion Containing Chloramphenicol and Cinnamon Essential Oil . . . . . . . . 6.2.5 Over-Time Stability Study . . . . . . . . . . . . . . . . . . . . . . . . . 6.2.6 Freeze–Thaw Cycle Stability Study . . . . . . . . . . . . . . . . . 6.2.7 Colony Count Study . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6.2.8 Rheology Study . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6.2.9 In Vitro Release Study . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6.2.10 Kinetic Release Study . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6.2.11 Statistical Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6.3.1 Ternary Phase Diagram Analysis . . . . . . . . . . . . . . . . . . . . 6.3.2 Chloramphenicol Solubility Analysis . . . . . . . . . . . . . . . . 6.3.3 Over-Time Stability Analysis . . . . . . . . . . . . . . . . . . . . . . . 6.3.4 Freeze–Thaw Stability Analysis . . . . . . . . . . . . . . . . . . . . . 6.3.5 Colony Count Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6.3.6 Rheology Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6.3.7 In Vitro Permeation Analysis . . . . . . . . . . . . . . . . . . . . . . . 6.3.8 Kinetic Release Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . 6.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Water Pollution Detection System for Illegal Toxic Waste Dumps . . Zuhanis Mansor and Nurul Nur Sabrina Abdul Latiff 7.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.2.1 Overall Systems Block Diagram . . . . . . . . . . . . . . . . . . . . 7.2.2 Project Hardware and Software . . . . . . . . . . . . . . . . . . . . . 7.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

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Alternative Processes for the Production of Bioactive Peptides . . . . . Norfahana Abd-Talib, Alia Shahiza Shaharuddin, Emmy Liza Anak Yaji, Nur Suraya Abd Wahab, Nadia Razali, Kelly Yong Tau Len, Jumardi Roslan, Fadzlie Wong Faizal Wong, Nazamid Saari, and Khairul Faizal Paée 8.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8.2 Conventional Process and Its Drawbacks . . . . . . . . . . . . . . . . . . . . 8.3 Alternatives Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8.3.1 High Hydrostatic Pressure . . . . . . . . . . . . . . . . . . . . . . . . . 8.3.2 Microwave-Assisted Processing . . . . . . . . . . . . . . . . . . . . . 8.3.3 Ultrasound . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8.3.4 Sub- and Supercritical Fluids . . . . . . . . . . . . . . . . . . . . . . . 8.3.5 Integrative Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Mode II Debonding Characterization of Adhesively Bonded Aluminum Joints . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Muhammad Noor Hazwan, Siti Faizah Mad Asasaari, Wong King Jye, Mohd Nasir Tamin, Mohd Shahrom Ismail, Mohamad Shahrul Effendy Kosnan, Mohd Al Fatihhi Mohd Szali Januddi, Mohd Anuar Ismail, and Mahzan Johar 9.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9.2 Cohesive Zone Model . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9.2.1 Cohesive Zone Model Formulation . . . . . . . . . . . . . . . . . . 9.3 Materials and Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9.3.1 Three-Point Bending End-Notched Fracture Test . . . . . . 9.3.2 Finite Element Simulation . . . . . . . . . . . . . . . . . . . . . . . . . 9.4 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9.4.1 Interfacial Fracture Adhesive Joints Under Mode II Debonding Loading . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9.4.2 Loading Rate Effect on Adhesive Joint Strain Energy Release Rate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9.4.3 Extraction of CZM Parameters Through an Experimental-FE Approach . . . . . . . . . . . . . . . . . . . . . . 9.4.4 FE Model Verification for CZM . . . . . . . . . . . . . . . . . . . . . 9.5 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

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10 Design Optimization of Shell and Tube Heat Exchangers: Effect of Baffles Design . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Siti Noor Zaerah Zazoly, Munir Faraj Mabrouk Alkbir, Adnan Bakri, Mahzan Johar, Shahrulzaman Shaharuddin, Mohamad Shahrul Effendy Kosnan, Ardiansyah Syahrom, and Mohd Al Fatihhi Mohd Szali Januddi 10.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10.2.1 Design Development . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10.2.2 Fluid Flow Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10.2.3 Mathematical Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11 The Performance of Palm Broom as Eco-friendly Paper . . . . . . . . . . Mohamad Sazali Said, Muhammad Iqbal Adnan, Mohamad Alif Akmal Mohd Khairi, Muhammad Izzat Kamarudin, Muhamad Salihin Abd Razak, and Mohd Shahrizan Yusoff 11.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11.2.1 Mechanical Testing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12 Mechanical and Thermal Properties of Polylactic Acid Composites Filled with Iron Particles . . . . . . . . . . . . . . . . . . . . . . . . . . . Muhammad Remanul Islam, Mohd Al-Fatihhi Mohd Szali Januddi, Mohd Haziq Zakaria, Sairul Izwan Safie, Ahmad Naim Ahamd Yahaya, Md Golam Sumdani, and Amin Firouzi 12.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

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13 Mechanical and Thermal Properties of Polylactic Acid/Carbon Fiber Composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Muhammad Remanul Islam, Mohd Al-Fatihhi Mohd Szali Januddi, Mohd Haziq Zakaria, Ahmad Naim Ahmad Yahaya, Sairul Izwan Shafie, and Amin Firouzi 13.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14 Antioxidant and Antibacterial Activities in Kaffir Lime (Citrus hystrix) Essential Oil Extracted by the Hydro-distillation Method . . Mazlin Mohideen, Nik Nur Syahidatul Jannah Mahadi, Nur Aina Nabilah Suhaimi, and Nur Azzalia Kamaruzaman 14.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14.2.1 Plants Material . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14.2.2 Essential Oil Screening for Antioxidant Potential . . . . . . 14.2.3 Antibacterial Screening . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14.3.1 Extraction of Essential Oil . . . . . . . . . . . . . . . . . . . . . . . . . 14.3.2 DPPH Radical Scavenging Activity . . . . . . . . . . . . . . . . . 14.3.3 Disc Diffusion Antibacterial Activity Assay . . . . . . . . . . 14.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15 Thermal and Microbiological Properties of Spray Dried Lactobacillus Plantarum-Banana Peel Powder . . . . . . . . . . . . . . . . . . . . Nurul Hafifah Abdul Wahid, Nur Ain Syuhada Zamri, Mohd Al-Fatihhi Mohd Szali Januddi, and Shahrulzaman Shaharuddin 15.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15.2.1 Preparation for Lactobacillus Plantarum ATCC8014 Growth . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15.2.2 Preparation of Banana Peel . . . . . . . . . . . . . . . . . . . . . . . . . 15.2.3 Preparation of Feed Solution for Spray Dry . . . . . . . . . . . 15.2.4 Spray Drying Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15.2.5 Microencapsulation Efficiency . . . . . . . . . . . . . . . . . . . . . . 15.2.6 Heat Exposure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15.2.7 Thermogravimetric Analysis (TGA) . . . . . . . . . . . . . . . . . 15.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15.3.1 Microencapsulation Efficiency . . . . . . . . . . . . . . . . . . . . . . 15.3.2 Heat Exposure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

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15.3.3 Thermogravimetric Analysis (TGA) . . . . . . . . . . . . . . . . . 158 15.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 160 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 160 16 Design of a Pre-crack Device for Environmental Stress Cracking (ESC) Studies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Muhamad Syafiq Mohamad Nor Azli, Muhammad Faris Mohd Radzi, Nur Ahza Che Nasir, and Mohd Shahneel Saharudin 16.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17 Analysis of Hydrophobic-Silver Nanoparticle Coating to Inhibit Cooling Water Corrosion in Cooling Systems . . . . . . . . . . . Hannah Madihah Zulkifli, Adnan Bakri, Mohd Zul-Waqar Mohd Tohid, Mohd Al-Fatihi Sajudi, Munir Al-Faraj Al Akbir, Mohamad Shahrul Effendy, Mohd Anuar Ismail, Zulhaimi Mohamad, Rahimah Kassim, Ahmad Nur Aizat Ahmad, and Izatul Husna Zakaria 17.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17.2 Experimental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17.2.1 Substrates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17.2.2 Hydrophobic-Silver Nanoparticle Coating Preparation . 17.2.3 Application of Coating . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17.2.4 Immersion Test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17.2.5 Tafel Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17.3.1 Cooling Water Corrosion Inhibition by Coating . . . . . . . 17.3.2 Effects of pH in Cooling System on the Rate of Cooling Water Corrosion . . . . . . . . . . . . . . . . . . . . . . . . 17.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18 Feature Presentation of Image Saliency Existence Based on Boundary Compactness Hypothesis . . . . . . . . . . . . . . . . . . . . . . . . . . Nur Zulaikhah Nadzri, Mohammad Hamiruce Marhaban, Siti Anom Ahmad, and Asnor Juraiza Ishak 18.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18.2 Related Work . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18.3 The Proposed Framework . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18.3.1 Pre-processing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18.3.2 Distance-Wise Matrix to Vector Presentation . . . . . . . . . . 18.3.3 Boundary Compactness Feature . . . . . . . . . . . . . . . . . . . . .

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164 165 168 170 174 175

176 177 177 178 178 178 178 179 179 184 186 187 189

190 191 192 193 193 194

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18.3.4 Features in Frequency Domain . . . . . . . . . . . . . . . . . . . . . . 18.3.5 Global Saliency Features . . . . . . . . . . . . . . . . . . . . . . . . . . . 18.4 Experimental Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18.4.1 Graphical Saliency Existence Presentation . . . . . . . . . . . . 18.4.2 Numerical Saliency Existence Presentation . . . . . . . . . . . 18.5 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19 Application of Reflectors for Improving the Output Performance of Solar Photovoltaic (PV) Modules . . . . . . . . . . . . . . . . . Nurul Hanis Azhan, Nur Azmina Nordin, and Nurul Afza Matshalleh 19.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19.2.1 Experimental Work . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19.2.2 Simulation Work . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20 Mechanism of Surface Construction of Palm Oil Mill Effluent Sludge Biochar-Based Catalytic for Peroxydisulfate Activation . . . . Sabrina Karim, Aida Humaira Sallehuddin, Muhammad Syukri Aminur Rashid, Noor Aina Mohd Nazri, and Mohamad Ali Ahmad 20.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20.2.1 Sample Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20.2.2 Characterization of Sample . . . . . . . . . . . . . . . . . . . . . . . . . 20.2.3 Batch Degradation Experiment . . . . . . . . . . . . . . . . . . . . . 20.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20.3.1 Chemical Functional Group of Biochar by FTIR Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20.3.2 Initial pH Determination on the Degradation of MB by PDS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20.3.3 Effect of N-doped Biochar Dosages on the Degradation of MB by PDS . . . . . . . . . . . . . . . . . . 20.3.4 Effect of PDS Concentration on the Degradation of MB by PDS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20.3.5 Degradation of Methylene Blue Under Optimized Condition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

196 199 200 200 204 205 207 209

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21 Characterization of Oil Palm Frond-Based Biochar-Filled-Recycled PET Bio-composites . . . . . . . . . . . . . . . . . . . . Khaliesah Abbas, Robert Thomas Bachmann, Siew Kooi Ong, Mohamad Fauzi Abraham, Wei Hong Wu, Jason Shiing Lik Ling, and Ho Cheng How 21.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21.2.1 Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21.2.2 Materials Characterization . . . . . . . . . . . . . . . . . . . . . . . . . 21.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21.3.1 Surface Morphology Examination . . . . . . . . . . . . . . . . . . . 21.3.2 FTIR Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21.3.3 XRD Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21.3.4 DSC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21.3.5 TGA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21.3.6 DMA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22 The Mandrel-Less Fixture Setup for Orbital Friction Stir Welding of Pipe Joining . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Ady Idham Zinodin, Azman Ismail, Fatin Nur Zulkipli, Bakhtiar Ariff Baharudin, and Darulihsan Abdul Hamid 22.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23 Joint Analysis of Mandrel-Less Friction Stir Welding on PVC Pipe Butt Joining . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Jayryan Jasni, Azman Ismail, Fatin Nur Zulkipli, Bakhtiar Ariff Baharudin, and Darulihsan Abdul Hamid 23.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23.4 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24 Innovative Aggregates Replacement in the Production of Cement-Based Mortar: A Review . . . . . . . . . . . . . . . . . . . . . . . . . . . . Nadia Razali, Nurriswin Jumadi, and Nadlene Razali 24.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24.2 Alternative Formulation and Mix Design . . . . . . . . . . . . . . . . . . . . 24.2.1 Water-Cement Ratio . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24.3 Alternatives Aggregates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

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234 235 235 236 237 237 238 240 244 244 246 247 248 251

252 253 258 259 260 261

262 263 266 266 268 271 271 272 273 275

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24.3.1 Fly Ash and Bottom Ash . . . . . . . . . . . . . . . . . . . . . . . . . . . 24.3.2 Glass . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24.3.3 Plastics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24.3.4 Construction Wastes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24.4 Carbon Footprint . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24.5 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25 Mechanical Properties of Dome Low Blow Impact on Spot Welded Joints . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Farizah Adliza Ghazali, Shahmal Fazzad Fakhrurrazey, and Zuraidah Salleh 25.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25.2 Literature Review . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25.3 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25.3.1 RSW Samples Preparation, Treatment, and Testing Equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25.3.2 Post-weld Treatment Using Dome Low Blow Impact . . . 25.3.3 Area of Deformation Measurement . . . . . . . . . . . . . . . . . . 25.3.4 Assessment of Tensile Shear . . . . . . . . . . . . . . . . . . . . . . . 25.3.5 Numerical Modeling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25.4 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25.4.1 Area of Deformation of Spot-Weld Impact Treatment . . 25.4.2 Correlation Between Area of Deformation and Stress Development . . . . . . . . . . . . . . . . . . . . . . . . . . . 25.5 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

275 275 276 277 279 279 280 285

286 287 287 288 288 289 290 290 291 291 293 294 294

Chapter 1

Carbon Fibre Precursor from Oil Palm Biomass Lignin Siti Khadijah Amran, Afiqah Liana Sazali, Norfahana Abd-Talib, Khairul Faizal Pa’ee, Mohd Razealy Anuar, and Tau-Len Kelly Yong

Abstract The interest in converting biomass into value-added products has increased dramatically. Oil palm industries generate approximately 75% of solid waste from palm trunks and fronds accessible on plantations. The remaining 25% are available at mills as empty fruit bunches, mesocarp fibres, and palm kernel shells. In plantations, a significant amount of biomass is typically discarded. As a result, this scenario demonstrates the substantial underutilisation of lignocellulosic feedstock. Lignocellulosic biomass is frequently used to produce biofuels, biochemicals, and other high-value products because of its low cost, abundance, and renewability. Despite the widespread usage of carbon fibre in industry, its applicability is restricted due to the expensive cost of the material. Interestingly, lignin has the potential to be utilised as a carbon fibre precursor with properties similar to those of polyacrylonitrile and pitch-based precursors. Deep eutectic solvents (DESs) are eutectic combinations of hydrogen bond acceptors (HBA) and hydrogen bond donors (HBD) with S. K. Amran · A. L. Sazali · K. F. Pa’ee · M. R. Anuar · T.-L. K. Yong (B) Malaysian Institute of Chemical and Bioengineering Technology, Universiti Kuala Lumpur, Taboh Naning, 78000 Alor Gajah, Melaka, Malaysia e-mail: [email protected] S. K. Amran e-mail: [email protected] A. L. Sazali e-mail: [email protected] K. F. Pa’ee e-mail: [email protected] M. R. Anuar e-mail: [email protected] N. Abd-Talib New Product Development, OHR Marketing Sdn Bhd., No 421, Jalan Perusahaan 6, Taman Bandar Baru Mergong, Lebuhraya Sultanah Bahiyah, 05150 Alor Setar, Kedah, Malaysia e-mail: [email protected] T.-L. K. Yong Centre for Women Advancement and Leadership, Universiti Kuala Lumpur, Kuala Lumpur, Malaysia © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 A. Ismail et al. (eds.), Materials Innovations and Solutions in Science and Technology, Advanced Structured Materials 173, https://doi.org/10.1007/978-3-031-26636-2_1

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much lower melting points than those of their components. DESs are versatile green solvents that can be chemically tailored to meet the requirements of various applications. The β–O–4 bond is the primary linkage in the chemical structure of lignin and is frequently targeted during lignin breakdown and pretreatment. DESs have an outstanding ability to break the β–O–4 bonds and extract lignin with high purity. Therefore, this review aims to determine the feasibility of using DESs as carbon fibre precursors to extract lignin from oil palm biomass. Keywords Deep eutectic solvent · Carbon fibre · Lignin · Precursor · Oil palm biomass

1.1 Introduction As a result of the renewable nature and accessibility of biomass, many researchers have focused their attention in recent years on the effective conversion of biomass into high-value products, which is a promising area of study. The quantity of lignocellulosic biomass generated by palm oil plantations in Malaysia has long been a concern due to the underutilisation of biomass and inappropriate waste disposal procedures on the plantations’ lands. Currently, biomass waste is disposed of in landfills, burned, or left out in the open, contributing to environmental issues. Despite these concerns, Malaysia’s oil palm industry is undergoing rapid growth, which has a substantial impact. Consequently, optimising biomass conversion into high-value products is economically and environmentally beneficial. Cellulose, hemicellulose, and lignin are the three primary elements of lignocellulosic biomass, with cellulose being the most abundant. Lignin is a by-product of the pulping process used in the paper industry and biomass refineries, and it may be recovered either physically or chemically from the pulp. Lignin is a key of lignocellulosic materials, serving as a plant adhesive and structural support for the material. Typically, the lignin structure is targeted for breakdown primarily via the formation of β–O–4 bonds. Lignin has the potential to be used as a precursor for carbon fibres since it is both cheaper and more environmentally friendly. However, the challenges associated with lignin extraction represent barriers to lignin utilisation. Currently, there is no efficient approach for isolating high-purity lignin due to the structural complexity of the compound. It is vital to utilise sustainable raw materials and effective extraction processes to convert lignin into viable end-products to maximise profits (Mohamad Ibrahim et al. 2008). DESs have received considerable attention owing to their increased awareness of environmental issues and green technologies. DESs are highly adaptable green solvents that may be chemically modified to fulfil the requirements of a wide variety of applications. They are utilised in a wide range of industries and are very adaptable. This is accomplished by combining various HBAs and HBDs. DESs have several advantages, including high biodegradability, cheaper cost, low toxicity, and environmental friendliness. β–O–4 bonds are the primary linkages in the chemical structure

1 Carbon Fibre Precursor from Oil Palm Biomass Lignin

3

of lignin and are frequently targeted during lignin degradation and pretreatment. DESs are extremely effective in breaking β–O–4 bonds to obtain high purity lignin (Malaeke et al. 2018). The currently available precursors are heavily dependent on nonrenewable and nonsustainable fossil fuels. Due to the increased demand for carbon fibre, expensive precursors, and environmental concerns, research into developing a less expensive carbon fibre precursor has increased. Therefore, the viability of lignin as a potential precursor for carbon fibres should be explored. Using lignin as a precursor for carbon fibres is commercially feasible (Karunakaran et al. 2020). This review assesses the feasibility of extracting lignin from oil palm biomass using DESs as a precursor for carbon fibre production.

1.2 Oil Palm Biomass Biomass is defined as the organic matter that can be used as a renewable energy source. It includes plant and animal resources such as household waste, wood, manure, paper waste, and agricultural waste. Owing to its ease of access and abundance throughout the years, biomass has attracted significant interest in its use as a bioenergy and biomaterial product (McKendry 2002). Biomass is cellulose, hemicellulose, and lignin-based organic material. The relative composition of these components changes depending on the type of biomass and other factors such as weather, soil fertility, and fertiliser. Lignin is the most complex natural polymer among the three components of lignocellulosic biomass. The three-dimensional amorphous polymer is composed primarily of phenylpropane units. Common lignin building blocks are coniferyl alcohol, p-coumaryl alcohol, and sinapyl alcohol. However, the types of lignin building blocks vary according to whether the plant is hardwood or softwood. Softwood lignin contains more than 90% coniferyl alcohol, with the remainder being p-coumaryl alcohol (Lehto et al. 2018). In contrast, hardwood lignin has different percentages of coniferyl and sinapyl alcohols. Oil palm biomass is an agricultural residue from palm oil plantations that are either burned or left to decompose. Oil palm biomass is generated during the replanting, pruning, and milling processes and accounts for approximately 90% of the bulk oil palm tree. Due to biomass underutilisation for useful end-products, various studies have been conducted to convert this biomass into value-added products (Mohd-Yusof et al. 2019). Table 1.1 summarises the elemental analysis of oil palm biomass. It is desirable to have a high carbon content in biomass because one of the criteria for lignin as a carbon fibre precursor is that it contains at least 60% carbon (Rozhan et al. 2019). As shown in Table 1.2, oil palm biomass contains significant lignin, making it an ideal precursor for carbon fibre. Additionally, palm oil biomass contains very little ash or extractives. Low ash content is preferable because it inhibits the formation of char, which is detrimental at high temperatures (Omar et al. 2018). The high

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Table 1.1 Elemental analysis of oil palm biomass on a dry basis Oil Palm Biomass

Elemental percentages (wt%) C

EFB

H

N

S

Sources O

48.6

6.6

0.6

0.4

43.8

Karunakaran et al. (2020)

45.6

6.2

0.4

–

47.8

Rozhan et al. (2019)

Trunk

51.4

11.8

0.2

–

36.6

Tan et al. (2017)

Frond

43.6

4.8

0.6

0.5

50.5

Shahbaz et al. (2017)

Table 1.2 Chemical analysis of oil palm biomass Oil palm biomass

Content (wt%)

Sources

Cellulose

Hemicellulose

Lignin

Extractives

Ash

Empty fruit bunch

28.0

19.5

33.4

16.2

2.9

Medina et al. (2018)

Trunk

22.4

39.3

36.1

–

2.2

Mohtar et al. (2015)

Frond

50.1

17.5

22.2

6.6

3.6

Hussin et al. (2018)

extractives content is detrimental because it causes a mechanical flaw in the carbon fibre (Qu et al. 2017).

1.3 Lignin Lignin is the main structural component of lignocellulosic biomass, frequently underutilised because of the difficulties in obtaining pure lignin. Lignin is a complex, crosslinked polyphenol that contains several important functional groups. The polyphenolic structure of lignin increases its resistance to chemical and biological degradation and its strength and rigidity (Constant et al. 2016). The primary functions of lignin include cell wall strengthening, compressive strength in plant tissues, and resistance to insects and pathogens. However, the chemistry, molecular biology, and lignin structure remain poorly understood. β–O–4 linkages account for approximately half of all the linkages. Hardwood lignin constitutes about 60% of the total linkages. The β–O–4 linkages are particularly susceptible to degradation by pulping, bleaching, and biological processes. Thus, linkages are the primary degradation targets during lignin extraction (Brodin et al. 2010). The primary challenge in using lignin is developing a precursor with properties comparable to commercially available carbon fibre precursors. Therefore, the quality of lignin should be compared to industry standards to determine its suitability as a precursor for carbon fibres (Khalid et al. 2020). The Oak Ridge National Laboratory

1 Carbon Fibre Precursor from Oil Palm Biomass Lignin Table 1.3 Lignin specification as a precursor to carbon fibre (Baker and Rials 2013)

Properties

Value (wt%)

Ash content

< 0.1

Volatile matter

< 5.0

Particulate matter

100% removal for matter > 1 μm in diameter

Carbon content

60

Lignin purity

99

5

focused on lignin blends to produce carbon fibre, and the results were used to develop the parameters indicated in Table 1.3 (Baker and Rials 2013). These parameters assess if lignin is suitable for use as a carbon fibre precursor.

1.4 Conventional Lignin Refining Process It must first be physically or chemically separated from the lignocellulose to use lignin as raw material. The lignin source and isolation method strongly influenced the isolated lignin’s structure, purity, and properties. The most common lignin refining process is kraft pulping. It separates cellulose from hemicellulose and lignin to produce a pulp that may be used to produce paper and other paper-related products. The biomass was treated with aqueous sodium hydroxide and sodium sulphide solutions. This process was carried out at a high temperature to remove lignin from the fibres. Kraft pulping degrades the chemical bonds in lignin, resulting in lignin extraction. The ester and ether bonds in lignin are disrupted, resulting in a lignin suspension in the black liquid. The separation of lignin and a significant portion of hemicellulose derived from black liquor is required. Lignin can be degraded by reacting with sulphide ions. Nucleophiles such as hydrogen sulphide or hydroxide ions are frequently added (Mohtar et al. 2015). Extraction can be controlled by adjusting the reaction time, temperature, and alkalinity (Bengtsson et al. 2019). Sulphite pulping, which involves using an aqueous solution of sulphur dioxide at a range of pH values, is also widely used for lignin separation. Lignosulphonates are formed when the sulphonate groups react with the α-position of the propane side chain of lignin. In contrast, the addition of sulphonate groups results in water-soluble lignosulphonates. The isolated lignin exhibited distinct properties. Carbohydrates are present in lignosulphonate fragments. Carbohydrate impurities may need to be removed before obtaining pure lignin fractions via fermentation, chemical treatment, or selective precipitation (Gosselink et al. 2012). Orgonosolv pulping or fractionation is another conventional lignin refining process performed at high temperatures and pressures. This method enabled the production of high-quality cellulose and lignin. Furthermore, the isolated lignin was extremely pure and yielded a large amount of lignin. Organic acids such as acetic

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acid and ethanol were combined with water to isolate lignin-cellulose structures. Acid precipitation produces pure lignin. The organosolv process cannot generate sulphur as a by-product, which causes fewer structural changes to lignin because this method utilises sulphides and does not require extreme conditions (Mohamad Ibrahim et al. 2008; Khalid et al. 2020).

1.5 Carbon Fibre Carbon fibres are composed of carbon atoms bonded in a long chain, with each filament measuring approximately 5–10 mm in diameter. Carbon fibre has several advantages, including high stiffness, strength, lightweight properties, high chemical resistance, minimal thermal expansion, and high-temperature tolerance. The exceptional properties of carbon fibre have increased its use in industry, particularly in aerospace, automotive, civil engineering, and construction (Bhatt and Goel 2017). Carbon fibre precursors are the raw materials used to produce carbon fibre. Carbon fibre precursors are potential carbon substances that yield carbon residues but do not melt during pyrolysis. Additionally, carbon fibre precursors have low linear density, high strength and modulus, and fewer structural defects. Carbon fibre should also contain at least 90% carbon (Dumanli and Windle 2012). PAN accounts for 90% of carbon fibre manufacturing, whereas petroleum pitch accounts for 10% (Bhatt and Goel 2017). PAN is a nonrenewable and unsustainable source of carbon fibre because it is derived from petroleum. Potential industrial applications of carbon fibre have sparked interest in carbon fibre precursors. By 1980, the aerospace industry was driving the global demand for carbon fibre, with pitch serving as the primary precursor. However, PAN has rapidly become the most frequently used precursor, owing to the high processing costs associated with spinnable pitch production (Choi et al. 2019). As a carbon fibre precursor, PAN is known to have the highest theoretical carbon yield of roughly 67%, and it is also thought to have the highest ability to produce highquality carbon fibre. On the other hand, pitch materials derived from petroleum offer a potential yield of up to 80%. However, the key drawbacks of these precursors are their unsustainability and nonrenewability, which has been a significant incentive for the development of more affordable and sustainable carbon fibre precursor replacements (Nunna et al. 2019). Despite the increased demand for carbon fibre, its high cost precludes its use in industrial applications. The high price of this composite is due to the expensive precursor material used to manufacture carbon fibre. As illustrated in Fig. 1.1, the cost of precursors accounts for more than half of the total cost of manufacturing carbon fibre. Therefore, substantial research is being conducted to resolve this issue by substituting sustainable and renewable precursors for petroleum-based precursors. It is necessary to significantly produce low-cost, high-yielding precursors to reduce carbon fibre costs. Lignin research has revealed a promising approach for producing low-cost carbon fibre with properties comparable to PAN and pitch. The use of lignin-based precursors

1 Carbon Fibre Precursor from Oil Palm Biomass Lignin Fig. 1.1 Manufacturing cost of carbon fibre (Khalid et al. 2020)

7

Depreciation 12% Other fixed 9%

Precursor 51%

Labor 10%

Utilites 18% Precursor

Utilites

Labor

Other fixed

Depreciation

is expected to significantly reduce the cost of carbon fibres, making them economically viable for various applications. The environmental and sustainability concerns associated with petroleum-derived precursors can be systemically addressed (Fang et al. 2017).

1.6 Lignin as Carbon Fibre Precursor Due to the structural complexity of lignin and the technical obstacles involved in isolating it from lignocellulosic biomass, lignin is mostly underutilised. Using this feedstock as a carbon fibre precursor, on the other hand, will boost its economic value and stimulate future advances in lignin separation technology. Lignin is converted into carbon fibres via melt-spinning and dry-spinning processes. Consequently, the use of lignin as a carbon fibre precursor is intriguing. This is mostly due to its cheap cost and high carbon content, which may reach as high as 60% in certain cases. Table 1.4 summarises the cost of carbon fibre derived from various precursors. The overall cost of lignin as a carbon fibre precursor is the lowest of all precursors, at 1.1 USD/kg. Despite its low precursor cost, lignin has both advantages and disadvantages. One disadvantage is the difficulty of converting lignin to carbon fibre. Consequently, various lignin types require distinct manufacturing processes and parameters. The intricacy of lignin’s structure and impurities may result in deficient carbon fibre structures and low mechanical properties. From another perspective, having a range of lignin readily accessible for extraction may be advantageous because the lignin structure may be selectively altered depending on the isolation method. Lignin can be melt-spun and stabilised at a faster heating rate to increase its carbon content (Brodin et al. 2010). Although lignin has a low melting point, it also has a relatively high Tg value. As a result, fibre oxidation can be maintained at a reasonable rate. Solvents can be

8 Table 1.4 Carbon fibre cost derived from various precursors (Fang et al. 2017)

S. K. Amran et al. Material

Precursor price (USD/kg)

Production price (USD/kg)

Total price (USD/kg)

Melt-spun PAN

6.3

17.4

23.7

Textile-grade PAN

4.4–13.2

12.2–25.4

16.6–38.6

Conventional PAN

10.2

24.4

34.6

Lignin

1.1

5.2

6.3

removed during melt-spinning operations, resulting in cost savings associated with carbon fibre production. In addition, lignin may stabilise more quickly because of its high oxidation state, limiting oxygen diffusion into the fibre filament during the oxidation step (Souto et al. 2018).

1.7 Deep Eutectic Solvent DESs were discovered at the turn of the twentieth century and have since gained popularity as alternatives to conventional petroleum-based solvents. It is considered a green solvent because of its advantageous properties, including low toxicity, low cost, environmental friendliness, low volatility, ease of manufacture, and high biodegradability (Hou et al. 2018). Green solvents, also called bio-solvents, are derived from plants and are used in place of petroleum solvents. The first eutectic solvent was created by reacting quaternary ammonium ions with urea (Abbott et al. 2003). DESs were coined to designate solvents of Lewis or Brønsted acids and bases and include a broad range of anionic and cationic compounds. HBD and HBA are the primary components of the DESs at ambient temperature. In contrast to HBA and HBD, the mixture has a substantially lower melting point, which results in it being a liquid at room temperature (Abbott et al. 2003). DESs have low volatility due to the hydrogen bonding between HBA and HBD (Abbott et al. 2003). DESs have a broad variety of industrial uses with their distinct features, including biodiesel synthesis, reaction medium, extractive agents, and separation and purification processes. The physicochemical and thermal properties of DESs can be altered by changing the composition of HBAs and HBDs. As a result, DESs can be used in various applications because they can be tailored to have specific thermophysical characteristics (Peyrovedin et al. 2020). However, because various DESs can be synthesised depending on the HBAs and HBDs, more research is needed to understand this class of green solvents fully.

1 Carbon Fibre Precursor from Oil Palm Biomass Lignin

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1.8 Lignin Isolation from Biomass Using DES DESs have piqued the interest of scientists owing to their potential application in lignin extraction from biomass. The individual components of the DESs and their molar ratios significantly impact the degree of lignin extraction from biomass. Eutectic mixtures containing high concentrations of hydrogen have a high propensity to cleave ether bonds in lignin and increase the solubility of lignin in DESs (Li et al. 2021). Owing to the stronger hydrogen bonds found in acidic DESs, lignin solubility is greater in acidic DESs than in basic DESs. Acidic DESs are more effective at solubilising lignin and increasing hydrolysis yield (Skulcova et al. 2018). The rate of delignification, on the other hand, varies according to the type of biomass feedstock and pretreatment conditions used. Although it has been demonstrated that DESs can dissolve and extract high-quality lignin with greater than 90% purity, they have a much lower solubility for cellulose. Numerous studies have shown that DESs with high hydrogen bond accepting ability and polarity can aid in the breakdown of lignin. Choline chloride (ChCl) is a common HBA ingredient in DESs owing to its strong hydrogen bonding and chloride ions. Strong hydrogen bonding between the hydroxyl groups and chloride ions has been proposed to aid in the breakdown of lignin. ChCl was investigated for its effect on lignin solubility and its role in lignin extraction (Smink et al. 2019). Delignification was improved by increasing the breakdown of the lignin-carbohydrate complex. The lignin-carbohydrate complexes were dissolved by dissolving the hydrogen bonds between carbohydrates and lignin and forming new hydrogen bonds between the chloride ions in the DESs and lignin hydroxyl groups. Despite growing interest in DES-based solvents, research into how DES isolate lignin remains limited. Fractionation of lignin occurs because of the interaction of chloride ions in the DESs with polysaccharides in the biomass (Xia et al. 2018). Rapid delignification is enabled by forming strong hydrogen bonds between the chloride ions and hydroxyl groups of lignin. However, the precise mechanism by which lignin is cleaved remains unknown. Previously conducted research successfully demonstrated the intriguing properties of extracted lignin, implying that DES could be used to synthesise technical lignin. The extraction of high-purity lignin (94.46%) from willow using DES was achieved with a 1:10 molar ratio of ChCl to lactic acid (Li et al. 2017). Interestingly, the properties of the extracted lignin can be tailored by varying its composition and reaction conditions (Xia et al. 2018). In general, mild pretreatment conditions preserve a greater percentage of β–O–4 bonds in lignin, whereas severe pretreatment conditions completely cleave the ether bonds. The extraction temperature was determined by the type of HBA and HBD components present in the eutectic mixture. A study was conducted to assess the effect of DESs on lignin solubility (Malaeke et al. 2018). The researchers hypothesised that increasing the number of hydroxyl and phenyl groups in the DES mixture would increase lignin solubility. Additionally, the study recommended using freshly

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prepared DESs because moisture content has been shown to affect the dissolution of lignocellulosic components (Malaeke et al. 2018). In addition, the molar ratio of the DESs had a significant effect on the isolation of lignin from biomass. Additionally, DESs are recyclable and reusable. This can be accomplished with minimal loss of lignin (Kim et al. 2018). DESs have been used in various studies to pretreat palm oil biomass. However, these investigations focused on extracting lignin from cellulose and hemicellulose (Nor et al. 2016; Tajuddin et al. 2019; Zulkefli et al. 2017; Tan et al. 2019). The first work to focus only on DESs for lignin extraction used ChCl as the HBA and several HBDs with different functional groups as the HBD (Tan et al. 2019). Lignin extraction from oil palm biomass was improved by using HBD containing alphacarboxylic functional groups (lactic acid) and polyols (glycerol) (Tan et al. 2019). It should be highlighted that this study demonstrated that lignin could be extracted from lignin-carbohydrate complexes. Since lignin was not the primary focus of these investigations, the isolated lignin was not characterised to determine its fundamental properties, structural characteristics, and functional groups.

1.9 Conclusion Because of its capability to recover lignin in a simple, single-stage process while preserving high purity, DES have the potential to be employed in biomass processing, among other applications. It is also possible to utilise precise molar ratios of HBA and HBD to widen the use of DES while retaining high efficiency in simultaneous fractionation and lignin extraction, allowing for more widespread usage of DES. Finally, considering the significance of carbon fibre-based applications, notably in the polymer and composites sectors, research is being conducted to study the use of biomass lignin as a more viable and cheaper alternative carbon fibre precursor. Acknowledgements This work was supported by the Ministry of Education, Malaysia, under the Fundamental Research Grant Scheme (FRGS) (FRGS/1/2020/STG05/UNIKL/02/1).

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Qu W, Liu J, Xue Y et al (2017) Potential of producing carbon fiber from biorefinery corn stover lignin with high ash content. J Appl Polym Sci 135:1–11 Rozhan AN, Hairin ALN, Salleh HM et al (2019) Mechanism of carbon deposition within char derived from oil palm empty fruit bunch. AIP Conf Proc 2068:020009 Shahbaz M, Yusup S, Inayat A et al (2017) The influence of catalysts in biomass steam gasification and catalytic potential of coal bottom ash in biomass steam gasification: a review. Renewable Sustainable Energy Rev 73:468–476 Skulcova A, Russ A, Jablonsky M et al (2018) The pH behavior of seventeen deep eutectic solvents. BioResources 13:5042–5051 Smink D, Juan A, Schuur B et al (2019) Understanding the role of choline chloride in deep eutectic solvents used for biomass delignification. Ind Eng Chem Res 58:16348–16357 Souto F, Calado V, Pereira N (2018) Lignin-based carbon fiber: a current overview. Mater Res Express 5:072001 Tajuddin NA, Harun S, Sajab MS et al (2019) Influence of deep eutectic solvent (DES) pretreatment on various chemical composition of empty fruit bunch (EFB). Int J Eng Technol 8:266–274 Tan ST, Hashim H, Rashid AHA et al (2017) Economic and spatial planning for sustainable oil palm biomass resources to mitigate transboundary haze issue. Energy 146:169–178 Tan YT, Ngoh GC, Chua ASM (2019) Effect of functional groups in acid constituent of deep eutectic solvent for extraction of reactive lignin. Bioresour Technol 281:359–366 Xia Q, Liu Y, Meng J et al (2018) Multiple hydrogen bond coordination in three-constituent deep eutectic solvents enhances lignin fractionation from biomass. Green Chem 20:2711–2721 Zulkefli S, Abdulmalek E, Rahman MBA (2017) Pretreatment of oil palm trunk in deep eutectic solvent and optimisation of enzymatic hydrolysis of pretreated oil palm trunk. Renewable Energy 107:36–41

Chapter 2

Potential Use of Nanotechnology to Reduce Postharvest Spoilage of Fruits and Vegetables Abdallah Omar Hussein, Tong Woei Yenn, Leong Chean Ring, and Syarifah Ab Rashid Abstract Food spoilage is a major issue faced by people in various places globally regardless of the weather condition. Fruits have been the major victims of this spoilage. Sodium hypochlorite, iodine, hydrogen peroxide, and quaternary ammonium compounds are some of the commonly used chemical sanitizers. These sanitizers, however, have a range of negative side effects, including skin irritation, mucous membrane injury, and carcinogenic and mutagenic effects. Moreover, chemicalbased sanitizers are also known for degrading food by causing nutritional consistency, colour, and flavour loss. This has led to the demand of natural based alternatives which brings safe and good quality foods compared to the chemically based food sanitizers. Naturally based food sanitizers can be an ideal option as they may not form any health problems that may be related to the preservation of these foods. Nanotechnology has developed tremendously in recent decades, as shown by a 25-fold rise in the number of goods that contain or include nanoparticles in their manufacturing between 2005 and 2010. Nanotechnology provides a range of options to improve the food quality. This review describes the potential use of nanotechnology to reduce postharvest spoilage of fruits and vegetables. Keywords Food spoilage · Nanotechnology · Sanitizers

A. O. Hussein · T. W. Yenn (B) · L. C. Ring · S. A. Rashid Universiti Kuala Lumpur, Malaysian Institute of Chemical and Bioengineering Technology, Lot 1988 Kawasan Perindustrian Bandar Vendor, Taboh Naning, 78000 Alor Gajah, Melaka, Malaysia e-mail: [email protected] A. O. Hussein e-mail: [email protected] L. C. Ring e-mail: [email protected] S. A. Rashid e-mail: [email protected] T. W. Yenn Universiti Kuala Lumpur, Institute of Medical Science Technology, A1-1, Jalan TKS 1, Taman Kajang Sentral, 43000 Kajang, Selangor, Malaysia © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 A. Ismail et al. (eds.), Materials Innovations and Solutions in Science and Technology, Advanced Structured Materials 173, https://doi.org/10.1007/978-3-031-26636-2_2

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2.1 Food Spoilage Food spoilage is characterized as change in the quality of food making it unfit for human or animal utilization because of spoilage indicators like unpleasant odour and changes in texture and appearance. It is a complex process with the root cause being classified as microbiological, chemical, or physical in nature (Odeyemi et al. 2020). The spontaneous breakdown of complex organic molecules causes some spoilage. Other species, such as insects and rodents, can eat food as well. Microorganisms are responsible for most of the food spoilage intended for human consumption. Microbes colonise unprotected foodstuffs quickly because they are so tiny, have such large populations, and sometimes spread as resistant water, air, or soil borne spores. Colonization may be slowed by covering or isolating foods, but only with sealing sterile food in a jar that is not permeable, it can be avoided (Hammond et al. 2015).

2.1.1 Fruits Fruits are widely consumed globally and have been known to have abundance of benefits to the human body. But one of the main problems associated to the influence of fruits consumption is its short shelf life, that is for most fruits. Spoilage of these fruits is associated with physical and biological factors, and these changes are usually determined using the five sensory attributes of food. Following harvest, plants that offer fresh fruits are extremely susceptible to a variety of fungal infections (Arasu et al. 2019). Since fungus contains mycotoxins that can cause mycotoxicoses in humans after ingestion or inhalation, spoilage due to fungus of fruits is identified as a reason for potential health risk to animals and humans (Samuel 2015). The initial microbial load varies depending on horticultural activities, the hygiene and health of the employee, and environmental factors in the area and surrounding. Spoilage microorganisms can thrive in older fields and orchards, as well as places where dead and rotting plant material is not discarded on a regular. basis. Crop rotation, plant-based amendments, and traditional pesticides affect the initial microbial population before harvesting (Snyder and Worobo 2018). One of the most easily spoiled fruits is the table grape (Vitis vinifera), with problems like browning of the stem (rachis), weight loss, berry drop, and fungal deterioration are all typical during postharvest (Shen and Yang 2017). This fruit is one of many fruits that show the effects of postharvest spoilage. To assess the shelf life in Qatar, the percentage of various fruits with undiscovered, low, moderate, heavy, and swab identified contamination levels were evaluated (Saleh and Al-Thani 2019). The highest numbers of fungi per fruit were found in strawberries, which may be due to the skin’s characteristics. Besides, 56.25% of cucumber samples displayed no growth of hyphae at the end of the 10-day period, while 13.3% of orange samples had a high degree of contamination. Finally, although 60% of the tomato samples

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were infected, majority of them (53.3%) had a low distribution of contaminations in each fruit, which is due to the smooth, hard nature of the tomato skin (Saleh and Al-Thani 2019).

2.1.2 Vegetables The high-water activity of vegetables, along with their near-neutral pH, makes them an excellent resource for spoilage organisms looking for food nutrients. Although vegetables are exposed to a diverse range of soil microorganisms, not all of them can cause damage to plants, and some rotting species, such as lactic acid bacteria, are rare in soil. Rather than microorganisms that cause plant illnesses, bacteria and moulds that take advantage of mechanical and freezing damage to plant surfaces account for the majority of spoilage losses in agriculture (Rawat 2015). During all stages of the development process, including intake, ready-to eat (RTE) vegetables may be contaminated with foodborne microorganisms. Recent foodborne outbreaks suggest the importance of ready-to-eat fresh-cut items as potential fuel for foodborne pathogens (Iseppi et al. 2019). Their study paper went on to define the minimally processed vegetables, also known RTE vegetables, as primarily fresh vegetables that have been washed, peeled, sliced, sanitized, rinsed, dried, and packaged to prolong its shelf life and not needing further market manipulation (Iseppi et al. 2019). Despite the health benefits of taking raw fruits and vegetables, consistency and safety remain concerns, due to these foods being the means of transport for infectious disease transmission (Qadri et al. 2015). In terms of safety, fresh vegetables are no longer considered a low-risk product. Pathogens can infect fruits and vegetables at any point of their life cycle, from growth to consumption. Soil, waste (from some animals and humans), water, postharvest handling, cutting, and transportation are all sources of pollution (Medeiros et al. 2016). Aeromonas species were found to be present in 34% of the vegetables tested, including leafy greens (Iseppi et al. 2019). It also suggests that food degradation is primarily caused by the spread of microorganisms that can be transported from the field, water, mishandling of plants, parasites, rodents, and other sources (Iseppi et al. 2019). Changes in temperature, moisture, air, and light are all factors that were mentioned to be considered (Iseppi et al. 2019).

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2.2 Food Spoilage Caused by Microorganisms Plants contain defence mechanisms against microbial spoilage; however, these defences are impaired after harvest and senescence, exposing the fruit or vegetable to secondary plant pathogen colonization. The amount of agricultural water available, the use of specific growing substrates and insulating materials, and whether the processing environment is sealed, enclosed, or open all impact contamination risk (Snyder and Worobo 2018). Microbial degradation contributes to food waste and loss, albeit more study is required on the effect of microbial decomposition at the point of manufacturing in shelf life (Snyder and Worobo 2018). Despite the fact that there has been little study on the prevalence and influence of microbial food degradation on component loss and final product spoilage since then, there has been a significant growth in food safety research since then (Rawat 2015). The term “food protection” has gained awareness following the 1985 Listeriosis outbreak in California, which was linked to Mexican-style cheese (Snyder and Worobo 2018). As a result, the 2100 abstracts on food safety were published in 1988; this reflects the initial reference publication number based on the term’s use. In 2015, over 12,000 abstracts on food safety were published. In comparison, the number of abstracts containing the word “food spoilage” has remained relatively stable, averaging less than 500 per year from 1967 to 2012, with minor increase in the number of publications in recent years (Snyder and Worobo 2018; Contigiani et al. 2018). The primary cause of strawberry spoilage is fungal growth. Grey mould, Botrytis cinerea, is the most common pre and postharvest pathogen of strawberry crops, but postharvest rot can also be caused by Mucor, Rhizopus, Collectotrichum, and Phythophora fungi (Contigiani et al. 2018). Moulds, in general, and mycotoxin producers in particular, are the primary cause of spoilage, especially in open-box refrigerated products (Saleh and Al-Thani 2019).

2.3 Food Sanitizers One of the most significant strategies to increase the shelf life of a food product and prevent microbial contamination in the production line is to reduce microbial contamination in the manufacturing environment. Hygienic-sanitary methods, such as the use of an effective cleaning system followed by a sanitization process employing suitable sanitizing agents at appropriate doses, are recommended to accomplish the objectives (Bernardi et al. 2018). Sanitation following harvest is critical for all fresh foods, since it may reduce spoilage losses by 50% or more (Feliziani et al. 2016). Sanitization is essential for minimizing the prevalence of microbiological risks in minimally processed vegetables (MPV) since minimal processing is not an end-point preservation approach.

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Fungi on fruits and vegetables are well-known to be regulated by synthetic antifungal agents. Furthermore, because of the potential for antifungal resistance strains to emerge, the use of these synthetic drugs is restricted, and their use is also prohibited (Arasu et al. 2019). Chlorine (Cl2 ), commonly known as hypochlorite (OCl-) in solution, is the most utilized aqueous sanitizer. It is widely utilized in the food sector as well as in the decontamination of drinking water. Pathogen propagules die fast, which is important for preventing their spread during processing from tainted, rotting produce to healthy items (Feliziani et al. 2016). To generate aqueous hypochlorite solutions of specific concentrations for commercial disinfection, chlorine gas, sodium hypochorite (NaOCl) solutions, or calcium hypochlorite (CaCl2 O2 ) are utilized (Feliziani et al. 2016). The antifungal efficacy of sanitizing agents used in the food industries on different species of microorganisms common for food spoilage, according to the permissible amounts, was analysed. Sanitizers show different levels of antifungal efficiency according to results observed. Both sanitizer concentrations and fungal species treated with the same sanitizer concentration showed variances. It is possible that the differences are related to different mechanisms of action (Bernardi et al. 2018). Certain sanitizers, such as quaternary ammonium compounds, modify cell membrane permeability and deplete cells by stimulating glycolysis; others, such as peracetic acid, oxidize microbe biological components, causing injury to the enzymatic system. Apart from organic waste, sodium hypochlorite was determined to be the most efficient sanitizer against the fungal species studied (Feliziani et al. 2016). Organic matter, on the other hand, may reduce the antibacterial efficiency of sodium hypochlorite because it stabilizes the cytoplasmic membrane, enabling wounded bacterial cells to recover (Bernardi et al. 2018). While the use of synthetic antimicrobials is permitted in many countries, natural foods that do not contain synthetic or chemical preservatives are becoming increasingly popular. Fresh-like, delicious, natural, organic, nutritious, and practical food products are becoming increasingly popular among consumers (Odeyemi et al. 2020). Table grapes have been treated for storage by combining low temperature and sulphur dioxide fumigation. However, due to the chemical preservative’s phytotoxicity, the development of antimicrobial resistance, and food safety concerns about the effects of chemical residues on human health and the environment, this approach has been gradually questioned (Shen and Yang 2017). In the pepper fruits that were sampled in research of the effects of different sanitizers, no Escherichia coli colonies were found (Mani-López et al. 2016). Low inactivation values were achieved by using a low sanitizer concentration and short exposure times. Despite the fact that the most effective medication, ethanol (120 min of exposure time), essentially removed the initial microbial load, it may not be economically feasible owing to its high cost and lengthy treatment duration (Mani-López et al. 2016). A broad variety of concentrations of sanitizers were used to investigate microbial reductions and their impact on the physicochemical attributes of pepper fruits.

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Long-term exposure treatments are inevitably unrealistic in the food industry, but they do give useful information on the effects of duration and sanitizer concentration (Mani-López et al. 2016). Traditionally, fruits have been washed with a variety of chemical sanitizers to ensure microbial food protection by inhibiting microorganism growth and activity. These sanitizers have been extensively applied for food safety because of their ability to effectively inactivate microbial growth. Promising outcomes have been documented using sanitizers and ultrasonication. Salmonella could be eliminated from cherry tomato surfaces using either a single ultrasound treatment or a combination of ultrasound and peracetic acid (Mustapha et al. 2020). Furthermore, the study claimed that using organic acids in conjunction with ultrasound was efficient in eliminating harmful microorganisms while keeping the colour and texture of lettuce throughout storage (Mustapha et al. 2020). Because of their ease of application, low cost, strong antibacterial action, and full breakdown in water, chlorinated agents are tempting for routine consumption in the fruit and vegetable sectors. Chlorine-based chemicals must be handled with attention since they are dangerous and may cause skin and respiratory system irritation (de São José and Vanetti 2015). In the electronics sector, ultrasound has been used to disinfect surfaces, and it has recently been proposed as a sanitization alternative in the food business. Processors may employ ultrasound to process minimally processed fruits and vegetables, enabling them to adjust to shifting market trends (Santos et al. 2020).

2.4 Nanoparticles Nanotechnology has developed tremendously in recent decades, as shown by a 25fold rise in the number of goods that contain or include nanoparticles (NP) in their manufacturing between 2005 and 2010. Their general characteristics are distinct (in terms of particle size, surface reactivity, surface charge, and particle shape) in comparison to their volume or dissolved counterparts are likely to have aided this growth. This opens a wide variety of potential uses in cosmetic, pharmaceutical, and medical applications (Bundschuh et al. 2018). It is critical to characterize the physical, chemical, and biological properties of the developed nanoparticles, to suit their applications. It is critical to characterize nanoparticles for biomedical applications, particularly in vivo delivery. While a variety of characterization techniques have been accepted, obtaining a comprehensive characterization profile of nanoparticles remains a difficult task. The time-dependent variations of their chemical and physical properties are a major cause of a defective or under-characterized nanoparticle formulation (Bundschuh et al. 2018). While fertilizers are critical for plant growth, due to a variety of causes, including leaching, photolysis, hydrolysis, and degradation, many fertilizers are unavailable to plants. As a consequence, it is vital to use novel applications made feasible by nanotechnology and nanomaterials to decrease nutrient losses during fertilization and

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enhance agricultural yields (Siddiqui et al. 2015). The capacity to release nutrients on demand, the ability to monitor the release of chemical fertilizers that govern plant development, and improved target activity are all qualities that nanofertilizers or nanoencapsulated nutrients may have (Siddiqui et al. 2015). Most antibiotic resistance mechanisms are irrelevant for nanoparticles since their effect is direct contact with the bacterial cell wall rather than penetration. This gives reason to believe that nanoparticles are less likely than antibiotics to cause bacterial resistance. As a result, fresh and exciting nanoparticle-based materials with antibacterial activity have gotten a lot of coverage (Wang et al. 2017). In certain cases, nanoparticles can effectively avoid microbial drug resistance, which is why they are being considered as an alternative to antibiotics. Antibiotic overuse has caused in the proliferation of several public-health threats, including superbugs that are resistant to all currently available drugs and epidemics against which medication has no protection (Wang et al. 2017). Nanoparticles have multifunctional properties and can be applied to a wide range of fields, that includes medicine, nutrition, and electricity. In biomaterial science, the synthesis of monodispersed nanoparticles that have complex sizes and shapes have been a challenge. It provides significant benefits in the pharmaceutical industry, allowing for the treatment of a variety of bacterial and viral diseases. For the synthesis of nanomaterials, because of the abundant richness and accessibility of plant entities have been extensively investigated (Kuppusamy et al. 2016). When exposed to oxygen, light, moisture, and heat, natural bioactive chemicals are chemically unstable and prone to oxidative destruction (Shishir et al. 2018). While nanoparticles have existed in the environment for millennia (e.g. as rocks, clays, and bacteria products), they are being used for centuries. Engineered nanoparticles are nanoscale materials that have been developed in a methodical manner (Gupta and Xie 2018). Drugs entrapped in nanoparticles have improved and extended delivery to target cells, as well as reduced toxicity, when compared to their corresponding free drug. This term can also be applied to agriculture. Furthermore, nanoparticles have a highly reactive surface and are thus biologically active. A few nanoparticle-containing agricultural products are available in the market (Pestovsky and Martínez-Antonio 2017). Many researchers are interested in using lipid nanoparticles for drug delivery because of the encapsulated drug’s long-term release and the raw materials’ safety. Solid lipid nanoparticles were succeeded by nanostructured lipid carriers, which were designed to improve encapsulation efficiency and resolve drug expulsion over time, which was common with solid lipid nanoparticles (Pivetta et al. 2018). On the skin, natural nanostructured lipid nanoparticles containing thymol are effective delivery systems. The nanoparticles have a negative zeta potential and a high thymol entrapment efficiency, and their size has remained stable over time (Pestovsky and Martínez-Antonio 2017).

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2.4.1 Nanotechnology for Food Application Nanotechnology has a wide range of applications in biomedical, engineering, food, and agriculture (Santos et al. 2020). In the food industry, food processing is an important field for modern nanotechnology applications. The novel nanoparticle-polymer composites could have several mechanical and functional advantages, including antimicrobial activity to protect packed foods, biosensors to detect the presence of microbes, gas and vapour barriers, and biocompatible materials (Iseppi et al. 2019). The agri-food sector increasingly relying on nanotechnology to boost shelf life, food quality and protection, monitor distribution, storage, and packaging, and to create nanosensors for contaminated food detection (Ball et al. 2019). Nanoparticles can be used in food and eaten in a normal way. Casein micelles in milk, for example, are complexes of three subgroups of casein molecules (s-casein, -casein, and -casein) that are between 50 and 400 nm in size. Nanoparticles have been used to solve problems with food quality, shelf life, safety, protection, and nutritional value (Liu et al. 2019). Chitosan is a polycationic biopolymer produced from chitin that is naturally produced, which can be found in crustacean exoskeletons, arthropod exoskeletons, and fungi cell walls and are biocompatible, biodegradable, and safe for humans. It is capable of being processed into gels, capsules, micro- and nanoparticles, and used as an additive in the pharmaceutical, dairy, agricultural, clothing, and cosmetic industries (Paomephan et al. 2018). Due to its high surface area and charge density, chitosan in the form of nanoparticles has gained popularity as a novel antibacterial agent (Liu et al. 2019). Metallic nanoparticles have gotten a lot of research attention because they can be utilized to make antimicrobial products that can help increase the shelf life of food by inhibiting bacteria growth. They can interact with a variety of microbial cells, kill them, and inhibit biofilm formation (Pestovsky and Martínez-Antonio 2017). Nanotechnology has long been recognized as having an important function in the food business, particularly in the processing and packaging of food and food products (Santos et al. 2020). Many natural antimicrobials are sensitive to severe environmental conditions such as high temperature or strain, are hydrophobic, and/or have distinct odours, making their use in the food industry difficult (Cacciatore et al. 2021). Nanotechnology has been proposed as a strategy for using natural substances in foods to address these limitations, as nanoparticle systems can protect sensitive compounds from premature inactivation and allow for the controlled release of antimicrobials from nanostructures, thereby extending their applications (Liu et al. 2019).

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2.5 Nanoencapsulation Encapsulation of active compounds is a relatively new technology, but its rapid and it may now be found in a wide range of industries thanks to significant improvements, primarily the pharmaceutical, cosmetic, and food industries. Encapsulation is a process in which one substance (active agent) is encased in another substance, resulting in nanometre (nanoencapsulation), micrometre (microencapsulation), or millimetre scale particles (Zanetti et al. 2018). There are several encapsulation techniques that have been suggested, but none of them can be considered universally applicable. The entrapped substance is frequently a liquid, but it can also be a gas or a solid. Capsule, wall material, membrane, or carrier are all terms used to describe the covering substance. The surface-to-volume ratio increases when the particle size is reduced to the nanoscale through nanoencapsulation. As a result, the reactions are accelerated by a factor of ten; however, the product’s mechanical, optical, and electrical properties are altered (Katouzian and Jafari 2016). The study then goes on to suggest that the vitamin physicochemical properties are highly influenced by the nanoencapsulation method and delivery system used. As a result, while choosing a nanoencapsulation technology, the required size, physicochemical qualities, type of the encapsulated vitamin, and wall material must all be considered (Zanetti et al. 2018). Nanoencapsulation technology may be used to address food industry concerns such as the effective delivery of functional ingredients and the controlled release of flavour compounds (Bratovcic and Suljagic 2019). Through nanoencapsulation, the active component is delivered to the targeted site of action. They secure the functional ingredient from chemical or biological degradation throughout manufacture, storage, and application (Bratovcic and Suljagic 2019; Assadpour and Mahdi Jafari 2019). In contrast to microcapsules, nanocapsules have a larger surface area, which increases the solubility. Nanocapsules contribute more to bioavailability and long-term drug release, allowing for more precise active compounds (Shishir et al. 2018). Nanoencapsulation methods have been developed as a consequence of nanotechnology’s rise in a variety of sectors, notably the food industry, for the preservation and controlled/targeted release of a variety of bioactive compounds, including medicines and food bioactive components (nutraceuticals). They are safe to use in formulations and provide maximum bioavailability (Assadpour and Mahdi Jafari 2019). Nanoemulsion is one of the nanoencapsulation methods for antimicrobial agents that is especially well suited for food applications due to the variety of food-compatible emulsion components and scalable manufacturing techniques such as high-pressure homogenization (Assadpour and Mahdi Jafari 2019). When free and encapsulated antimicrobials are compared for bactericidal activity, it is obvious that encapsulated antimicrobials are less active against bacteria initially, but their effect lasts longer than free antimicrobials (Cacciatore et al. 2021). Encapsulation performance is influenced by the nature of the active molecule, the physical–chemical features of the encapsulating material, and the interactions that occur

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between them. Nanoliposomes and polymeric nanocapsules were used to encapsulate carvacrol. Both formulations had a good size, a low polydispersity index, and a good encapsulation performance, suggesting that the encapsulation technique has no great effect on the compound. In conclusion, nanotechnology can be used to reduce postharvest spoilage of fruits and vegetables. Acknowledgements Authors would like to thank Universiti Kuala Lumpur for supporting this project.

References Arasu MV, Viayaraghavan P, Ilavenil S et al (2019) Essential oil of four medicinal plants and protective properties in plum fruits against the spoilage bacteria and fungi. Ind Crops Prod 133:54– 62 Assadpour E, Mahdi Jafari S (2019) A systematic review on nanoencapsulation of food bioactive ingredients and nutraceuticals by various nanocarriers. Crit Rev Food Sci Nutr 59(19):3129–3151 Ball AS, Patil S, Soni S (2019) Introduction into nanotechnology and microbiology. Methods Microbiol 46:1–18 Bernardi AO, Stefanello A, Garcia MV et al (2018) Efficacy of commercial sanitizers against fungi of concern in the food industry. LWT- Food Sci Technol 97:25–30 Bratovcic A, Suljagic J (2019) Micro- and nano-encapsulation in food industry. Croat J Food Sci Technol 11(1):113–121 Bundschuh M, Filser J, Lüderwald S et al (2018) Nanoparticles in the environment: where do we come from, where do we go to? Environ Sci Eur 30(1):6 Cacciatore FA, Brandelli A, Malheiros PS (2021) Combining natural antimicrobials and nanotechnology for disinfecting food surfaces and control microbial biofilm formation. Crit Rev Food Sci Nutr 61(22):9 Contigiani EV, Jaramillo-Sánchez G, Castro MA et al (2018) Postharvest quality of strawberry fruit (Fragaria x Ananassa Duch cv. Albion) as affected by ozone washing: fungal spoilage, mechanical properties, and structure. Food Bioproc Technol 11(9):1639–1650 de São José JFB, Vanetti MCD (2015) Application of ultrasound and chemical sanitizers to watercress, parsley and strawberry: microbiological and physicochemical quality. LWT-Food Sci Technol 63(2):946–952 De Medeiros I, da Costa MJA, de Oliveira KÁR et al (2016) Efficacy of the combined application of oregano and rosemary essential oils for the control of Escherichia coli, Listeria monocytogenes and Salmonella enteritidis in leafy vegetables. Food Control 59:468–477 Dos Santos CA, Ingle AP, Rai M (2020) The emerging role of metallic nanoparticles in food. Appl Microbiol Biotechnol 104(6):373–2383 Feliziani E, Lichter A, Smilanick JL et al (2016) Disinfecting agents for controlling fruit and vegetable diseases after harvest. Postharvest Biol Technol 122:53–69 Gupta R, Xie H (2018) Nanoparticles in daily life: applications, toxicity and regulations. J Environ Pathol Toxicol Oncol 37(3):209–230 Hammond ST, Brown JH, Burger JR et al (2015) Food spoilage, storage, and transport: implications for a sustainable future. BioSci 65(8):758–768 Iseppi R, Sabia C, de Niederhäusern S et al (2019) Antibacterial activity of Rosmarinus officinalis L. and Thymus vulgaris L. essential oils and their combination against food-borne pathogens and spoilage bacteria in ready-to-eat vegetables. Nat Prod Res 33(24):3568–3572 Katouzian I, Jafari SM (2016) Nano-encapsulation as a promising approach for targeted delivery and controlled release of vitamins. Trends Food Sci Technol 53:34–48

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Kuppusamy P, Yusoff MM, Maniam GP et al (2016) Biosynthesis of metallic nanoparticles using plant derivatives and their new avenues in pharmacological applications—an updated report. Saudi Pharm J 24(4):473–484 Liu X, Zhang B, Sohal IS et al (2019) Is “nano safe to eat or not”? A review of the state-of-the art in soft engineered nanoparticle (sENP) formulation and delivery in foods. Adv Food Nutr Res 88:299–335 Mani-López E, Palou E, López-Malo A (2016) Effect of different sanitizers on the microbial load and selected quality parameters of “chile de árbol” pepper (Capsicum frutescens L.) fruit. Postharvest Biol Technol 119:94–100 Mustapha AT, Zhou C, Amanor-Atiemoh R et al (2020) Efficacy of dual-frequency ultrasound and sanitizers washing treatments on quality retention of cherry tomato. Innov Food Sci Emerg Technol 62:44 Odeyemi OA, Alegbeleye OO, Strateva M et al (2020) Understanding spoilage microbial community and spoilage mechanisms in foods of animal origin. Compr Rev Food Sci Food Saf 19(2):311–331 Paomephan P, Assavanig A, Chaturongakul S et al (2018) Insight into the antibacterial property of chitosan nanoparticles against Escherichia coli and Salmonella typhimurium and their application as vegetable wash disinfectant. Food Control 86:294–301 Pestovsky YS, Martínez-Antonio A (2017) The use of nanoparticles and nanoformulations in agriculture. J Nanosci Nanotechnol 17(12):8699–8730 Pivetta TP, Simões S, Araújo MM et al (2018) Development of nanoparticles from natural lipids for topical delivery of thymol: investigation of its anti-inflammatory properties. Colloids Surf B 164:281–290 Qadri OS, Yousuf B, Srivastava AK (2015) Fresh-cut fruits and vegetables: critical factors influencing microbiology and novel approaches to prevent microbial risks—a review. Cogent Food Agric 1(1):1121606 Rawat S (2015) Food Spoilage: microorganisms and their prevention. Asian J Plant Sci Res 5(4):47– 56 Saleh I, Al-Thani R (2019) Fungal food spoilage of supermarkets’ displayed fruits. Vet World 12(11):1877–1883 Samuel O (2015) Fungi associated with the spoilage of post-harvest tomato fruits sold in major markets in Awka Nigeria. Univers J Microbiol Res 3(2):11–16 Shen Y, Yang H (2017) Effect of preharvest chitosan-g-salicylic acid treatment on postharvest table grape quality, shelf life, and resistance to Botrytis cinerea induced spoilage. Sci Hortic 224:367–373 Shishir MRI, Xie L, Sun C et al (2018) Advances in micro and nano-encapsulation of bioactive compounds using biopolymer and lipid based transporters. Trends Food Sci Technol 78:34–60 Siddiqui MH, Al-Whaibi MH, Firoz M et al (2015) Role of nanoparticles in plants. In: Siddiqui MH (ed) Nanotechnology and plant sciences: nanoparticles and their impact on plants, 1st edn. Springer, New York Snyder AB, Worobo RW (2018) The incidence and impact of microbial spoilage in the production of fruit and vegetable juices as reported by juice manufacturers. Food Control 85:144–150 Wang L, Hu C, Shao L (2017) The antimicrobial activity of nanoparticles: present situation and prospects for the future. Int J Nanomed 12:1227–1249 Zanetti M, Carniel TK, Dalcanton F et al (2018) Use of encapsulated natural compounds as antimicrobial additives in food packaging: a brief review. Trends Food Sci Technol 81:51–60

Chapter 3

Integrating a Hydrogen Fuel Cell in a Vehicle as a Hybrid for a Sustainable Energy Application Muhammad Amer Zahin Ahmad Dzaki, Ernie Mazuin Mohd Yusof, Siti Nor Zawani Ahmmad, Norziana Yahya, and Muhammad Remanul Islam Abstract The current energy source for a typical transportation vehicle is mainly non-renewable energy such as fossil fuel. The combustion of fossil fuel in the engine will produce carbon emissions into the air. This is called greenhouse gas (GHG) emission. High amount of GHG in the atmosphere will result in advanced greenhouse effect that will result in higher global temperature every oncoming year. The solution to reduce GHG released into the atmosphere is by reducing the usage of combustion engine vehicles on the road. Therefore, an electric vehicle (EV) is the ideal type of transportation as it emits zero-carbon emission. However, a typical EV is too expensive, takes too long to recharge and relies on lithium ion for the battery structure where lithium is a non-renewable source and can deplete in the future. Hence, a hydrogen fuel cell is a device that exploits the energy transfused between oxygen and hydrogen molecules into water and electrochemical energy that could directly be connected to a load for power consumption. Since oxygen and hydrogen are renewable and abundant resource on earth, this project focuses on the study of utilizing a hydrogen fuel cell as an energy source for a clean and hybrid transportation vehicle. Furthermore, this project aims to develop a remote control (RC) car that uses the hydrogen fuel cell technology as a hybrid to drive the motor of the car by supplying hydrogen and oxygen to the fuel cell. By accomplishing the M. A. Z. A. Dzaki · E. M. M. Yusof (B) · S. N. Z. Ahmmad · M. R. Islam Universiti Kuala Lumpur, Malaysian Institute of Industrial Technology, Persiaran Sinaran Ilmu, Bandar Seri Alam, 81750 Johor Bahru, Johor, Malaysia e-mail: [email protected] M. A. Z. A. Dzaki e-mail: [email protected] S. N. Z. Ahmmad e-mail: [email protected] M. R. Islam e-mail: [email protected] N. Yahya Universiti Teknologi MARA, Cawangan Perlis, Kampus Arau, 02600 Arau, Perlis, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 A. Ismail et al. (eds.), Materials Innovations and Solutions in Science and Technology, Advanced Structured Materials 173, https://doi.org/10.1007/978-3-031-26636-2_3

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development of this prototype, it would simulate the possibility of using hydrogen fuel cell technology to power a real hybrid passenger vehicle achievable in real-life applications. Keywords Renewable energy · Automation · Hydrogen fuel cell · Remote control car

3.1 Introduction The initial championship for discovering vigorous energy consumption during the beginning of the Industrial Revolution was later demobilized gradually into a new excavation for much greener, environment-friendly, abundant and more sustainable energy resources during the mid-nineteenth century (Britannica 2020). This was notably during the first discovery of the greenhouse effect that took place and was first theorized by Foote in 1856 (Foote 1856) and worriedly the depletion of coal and fossil fuel mining in the near future. The global issue that humans now face is responsibly by their own activities. Particularly, the burning of fossil fuels (coal, oil and natural gas), agriculture and land clearings (Britannica 2020). These activities increase the concentrations of greenhouse gaseous. This is the enhanced greenhouse effect, which is contributing to warming of the earth for the last 150 years which disturbingly has undone 6500 years of natural global cooling (Global Climate Change Vital Signs of the Planet 2020). According to the United States Environmental Protection Agency (EPA.GOV, 2018), until the year 2018, the largest source of greenhouse gas emissions from human activities in the USA are from burning fossil fuels for electricity, heat and transportation with a percentage of 28% for transportation sector and 27% for electricity production of total greenhouse effect contributions. Disturbingly, the total emissions in 2018 amounts to 6677 million metric tons of CO2 equivalent (Climate Change Division 2018). Malaysia’s CO2 emissions amounted to 250.3 million tons in 2018, up from 241.6 million tons in 2017. The main sources of the emissions were electricity consumption, mobility (vehicles) and waste (municipal solid waste that ends up in landfills) (U.S Energy Information Administration 2020). At this rate, the total amount of global carbon emission will only increase each year and will inevitably create major issues to the world we live in. The main contributor to carbon emission worldwide is the transportation sector due to the fuel combustion that is used to power the vehicle’s engines. This sector has proven to be the highest contributor to the greenhouse effect in scales of metric tons globally and this reading will only increase annually (U.S. Energy Information Administration 2020). In addition, the vigorous demand for natural energy source such as fossil fuel to power everyday transportation vehicle will result in various issues for short-term and long-term period such as sea pollution from oil rig leakages and the depletion of the natural energy source mentioned (Levi 2013).

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A solution to this issue is to use a plug-in electric vehicle (EV) that emits minimal or non-carbon footprint value such as the vehicles manufactured by Tesla Inc. Since December 2019, Tesla Inc. have manufactured approximately 365,300 units of EVs (Harrison 2020). However, several problems have surfaced since the manufacturing of this EV. For instance, due to logistical issues and taxes, Tesla cars will remain too expensive for commercial and mass use. Not only the vehicles are too expensive for consumers to purchase, but it is also costly for Tesla Inc. to manufacture thus effecting the company’s capital expenditure and limit the number of consumers to own an EV. Charging an EV takes too long and another major problem with Tesla EV is that the vehicle operates on lithium ion battery structure in which this reactive alkali metal is a non-renewable resource (Russell 2006). Therefore, this resource will deplete in the near future due to mass demand and exploitation of this element for its rechargeable characteristics in modern technologies. Not to mention, the excavation for this element and building lithium mines will distort the local ecosystem such as currently happening in Ganzizhou Rongda and Congo (Katwala 2018). Given these points based on the problems and research stated in this section, this particular project is to introduce an alternative sustainable power source for a vehicle which is the hydrogen fuel cell hybrid technology which eliminates the need of using harmful energy source such as fossil fuel and toxic materials like battery acid in a vehicle.

3.2 Methodology There are several steps in designing this project that are shown using flowcharts and block diagrams. In general, this prototype is divided into three main segments which are: (1) Moving driver system (2) Communication driver system (3) Fueling system version 1.0.

3.2.1 Fuel Cell Process Flow Figure 3.1 shows the general process of the fuel cell. The first process is the electron exchange process where the hydrogen ions’ electrons are transferred to the cathode that creates a potential difference between the anode and cathode. This potential difference creates an electrical energy. When connected to a load, the electrical energy generated is used to power the load (Soto 2004).

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Fig. 3.1 Working process of fuel cell

3.2.2 Moving Driver Process Flow Based on Fig. 3.2, the system starts when the power switch of the prototype is turned on. Accordingly, the moving driver system controller is turned on. The servo will rotate and stays at 90° which is its initial position. Next, the system awaits the radio-frequency (RF) signal from the transmitter (TX) from the remote control. If it detects no signal, the system will remain idle. When it does detect any signal from the transmitter, the system will hold for 6 s to allow the hydrogen fuel cell to be fully powered. Concurrently, the system will then detect which number of channels is the signal transmitting to. Since channel ‘64’ is set to go forward, the brushless DC motor will rotate clockwise to drive the car forward. Laterally, the system will follow the same proceedings with channel ‘68’ as to drive the motor anticlockwise for reverse. Hence, if the IR receiver detects that the transmitter is transmitting the signal to channel ‘64,’ the system will immediately turn on relays 1 and 3. This will allow current to pass through the relays and power the front and rear DC motors to rotate

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Fig. 3.2 Moving driver system flowchart

clockwise which is the forward movement of the prototype. Vice versa, if the receiver detects channel ‘68,’ relays 2 and 4 will turn on and the DC motors will rotate anticlockwise which is reverse. Channels ‘7,’ ‘21’ and ‘9’ are for rotating the front wheels of the tires to maneuver the car left right or straight. For instance, if the receiver detects channel ‘7’ from the transmitter signal, the servo motor will rotate 35° anticlockwise to turn the tires to the left direction and vice-versa for channel ‘21’ which is 110° clockwise for the right

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direction. Channel ‘9’ will rotate the servo to 90° which is forward. The receiver will then wait for the signal from the transmitter to change or else it will continue to run the specific program in a loop. If the signal from the transmitter changes, it will return to identify which channel is currently being transmitted to. The system will end when the power switch is manually turned off or the PEM fuel cell runs out of fuel either hydrogen gas or oxygen gas which the latter fuel is hypothetically difficult to deplete.

3.2.3 Communication Driver Process Flow Figure 3.3 displays the process flowchart for the communication driver system. When the prototype is turned on, the communication driver microcontroller will be powered on. The system will proceed to command the high-toque servo motor to rotate to 0° which is the initial state of the servo. The HC05 Bluetooth module will turn on as well to connect to the remote XY apps from the user’s mobile device. When there is a secured connection, the microcontroller will display the interface programmed on the apps. The interface consists of the pressure value from the pressure sensor, voltage value from the voltage sensor and several options for the user to interact. If the user selected the ‘refuel?’ option, this indicates that the user is trying to refuel the hydrogen into the prototype. Therefore, the 3/2 way solenoid valve will turn off and cut the supply of hydrogen to fuel cell. The high-torque servo will hold its initial position to avoid pressure interruptions. The fuel port is now open, and the user will insert hydrogen into it via a syringe. The remote XY apps will continuously display the internal fuel pressure of the hydrogen on the mobile device. When the user has finished refueling and turned off the ‘refuel?’ option, the system will continue to turn on the solenoid valve and allow the supply flow to the fuel cell again. The high-torque servo will proceed to rotate according to the internal pressure value and control the supply to the fuel cell. The power mode option is for the user to select between the hybrid and batterypowered mode to drive the prototype. If the user selected the hybrid mode, the hybrid relay switch will turn on and allow the current from the fuel to connect to the battery and charge it while running. Vice versa, if the user selected the battery-powered mode, the hybrid relay switch will turn off and the prototype will only run on battery power. The voltage value of the prototype will continuously be displayed on the remote XY apps. The system will end when the user has disconnected the connection from the apps and turn off the prototype. Otherwise, the system will continue to run in a continuous loop.

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Fig. 3.3 Communication driver system flowchart

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3.3 Results and Discussion 3.3.1 The Prototype Figure 3.4 boasts the dignified prototype of this project entitled Pandai Besi Hydrogen Hybrid RC Car. Other than the prototype, Fig. 3.5 shows the equipment needed for outdoor operations. The remote control is for transmitting the direction signals to the prototype. The syringe is used for collecting the hydrogen gas from the depository and refuel the hydrogen into the prototype. The mobile device is used for IoT controlling and monitoring the status of the prototype. Figures 3.6 and 3.7 show the screenshots of the layout of the monitoring system on the apps transmitted by the prototype.

Fig. 3.4 Pandai Besi hydrogen hybrid RC car

Fig. 3.5 External apparatus

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Fig. 3.6 Pandai Besi hydrogen hybrid RC car (landscape mode)

Fig. 3.7 Pandai Besi hydrogen hybrid RC car (portrait mode)

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3.3.2 System Condition Status This section explains the status of several system conditions of the program which are hydrogen pressure, voltage value, mode selection and refueling option. Blynk and PAX DAQ software are used to record the status of the parameter value. Table 3.1 displays the prototype system condition status. The measurement unit for the hydrogen pressure in this project is in hectopascal. This is because the sensor detects in terms of force per unit area which is also Pascal’s law.

3.3.3 Analysis of Hydrogen Fuel Cell Reaction Time This section discusses the reaction time of the hydrogen fuel cell in the presence of hydrogen and oxygen. The transition, rising and decreasing time of the fuel cell voltage production are also presented in this subsection. The data displayed are in voltage unit against time. The fuel cell used in this experiment is the 5 W hydrogen fuel cell. Figure 3.8 displays the whole run of the hydrogen fuel cell reaction time. The y-axis is the voltage value in mV unit, and the x-axis is the time in seconds unit. The highest voltage recorded in the graph is 4700 mV. The setup of the run is by supplying hydrogen using the direct fueling method. The oxygen is supplied from the surrounding air by using the DC axial fan. The volume of H2 O used is a constant of 25 ml supplied to the hydrogen fuel station. The time for this experiment is 11 min or 680 s. The pressure value is discarded due to the targeted analysis of the fuel cell reaction time. This experiment starts by supplying constant 5 V DC to the hydrogen fuel station. Then the hydrogen produced is directly connected to the 5 W fuel cell. The voltage output is connected to the voltage sensor. The timer is then set for 2 phase which are 5 min to the see the increasing time and another 5 min to observe the decreasing time of the fuel cell. The data are then collected using the PLX-DAQ software tool and analyzed. Figure 3.9 is the first 60 s of the whole graph shown in Fig. 3.8. This is because it is much clearer to observe the transition of the fuel cell reaction and observing the rise time of the fuel cell. The apparent shaded region below the graph is actually individual lines for each data. It is observed that the rise time occurs at approximately the 13th second after the experiment started. The graph continues to gradually rise to an initial peak of 4000 mV at the 26th second. Then the graph falls to 3000 mV range before rising up to a steady level between 5000 and 4000 mV. Figure 3.10 displays the fuel cell increasing rate against time at approximately 12–26th s of the experiment. This simplified graph from the experiment is to observe the time taken for the fuel cell to produce from the initial value to the initial peak which is 4000 mV. The red line indicates the 3rd order polynomial line applied to

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Table 3.1 System condition status for the prototype Description of condition

App status

Condition 1 When the hydrogen pressure is below 1260 hPa, the indicator will turn on LED Red indicating low fuel. It will also turn on the warning alarm if the user selects the turn on sound

Condition 2 When the pressure is more than 1260 hPa and below 1500 hPa, indicator will turn blue for medium fuel

Condition 3 When the pressure is more than 1500 hPa, the indicator will turn green meaning the fuel is full

Condition 4 At the start of the program, the hybrid mode will always turn on. This is relative to the objective. However, when the user selects the battery mode, it will turn off the relay switch and change to battery powered only. The app will also display the current mode based on the user’s selections

(continued)

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Table 3.1 (continued) Description of condition

App status

Condition 5 The refuel option is always off. If the user wants to refuel and select the ‘YES’ option, the refuel relay switch will turn off to cut off the hydrogen from entering the fuel cell and open the fueling port gate. The high-torque servo motor will also turn to its original state which is 0°. When the user selected ‘No’ again, the relay will turn on and the servo will control the internal pressure as coded

Condition 6 This feature enables the user to turn on or off the warning alarm sound. The sound icon will start blinking upon selecting on. The specific sound ID from the app library for Condition 1–3 are as follows: I. Sound ID: 1023 (FLUORINE) II. Sound ID: 1031 (MEROPE) III. Sound ID: 1034 (MOONBEAM)

Fig. 3.8 Fuel cell voltage production (mV) against time (s)

this data. It could be observed that the rate of increment is a steady incline rate with the R2 value of 0.96. Note that the data line below the graph is much more visible than in Fig. 3.9. By applying the trend line in the graph, we are able to calculate the rate of increment by integration method. The upper limit is the peak value which is 4030 mV, and the lower limit value is 430 mV.

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Fig. 3.9 Fuel cell voltage (mV) transition

Fig. 3.10 Fuel cell increasing rate of change

y = −0.0302x 2 + 33.753x + 36.54

(3.1)

430 0.0302x 2 + 33.753x + 36.542dx

(3.2)

4030

Area under graph = 386731.59923969 The rate of increment calculated for the fuel cell was 386.73 mV/s. This value could be supported by a simple calculation from Fig. 3.11. Figure 3.11 displays the filtered graph from this experiment. The graph represents several data between the 12th and 26th s. This period is when the voltage rises from low to the initial peak is observed in this run. At the 13th–14th second of the run, the graph remains constant. At 15th second, the voltage started to rise to a total of 220 mV increment. At 16th second, the voltage rises 290 mv of increment. At 17th, the voltage rises to 1400 mV

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Fig. 3.11 Time taken to reach peak voltage

which is 440 mV of increment. At the 26th second, the voltage rises to its initial peak value of 4030 mV. From the graph, it is observed that the time taken for the fuel cell to reach its peak value is approximately 12.34 s. To support the calculation by Eq. (3.2), the three data presented are the 14–17th s of this experiment are selected. The difference between these data values are added and divided by 3 for an average rate. The value obtained is 316.67 mV/s. Another calculation involves the peak value to the low value and divide it by 12.34 s which is the time taken for the fuel cell to reach its peak. The value obtained was 297.53 mV/s. Hence, the rate of increment from the integration method from Eq. (3.2) is acceptable since the R2 value of the trendline does not equal to 1. Therefore, the increment rate of the 5 W hydrogen fuel cell is 386.73 mV/s, or 0.4 V/s, and the time taken to reach its peak is 12.34 s.

3.4 Conclusion The method of storing hydrogen is to store pure hydrogen on board the vehicle and the method of supplying hydrogen to the HFC is by using the FuS01 method. The developed prototype is entitled Pandai Besi Hydrogen Hybrid RC Car. The results for the hybrid runtime for the prototype show an astounding of 100% runtime with 96.94% battery power remaining for hybrid mode compared to 55.48% of runtime and with only 9% remaining power compared to the battery-powered mode. Therefore, the hybrid mode boasts an increment of 44.52% of runtime and 87.94% battery power remaining compared to the battery-powered mode. Hence, by addressing these data, the main objective for this project is proven achieved.

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In conclusion, the development of this project in its entirety is to introduce an alternative sustainable power source for a hybrid electric vehicle which is the hydrogen fuel cell technology which eliminates the need of using harmful and non-renewable energy source such as fossil fuel in a vehicle. By accomplishing the development of this prototype, the possibility of using hydrogen fuel cell technology to power a real hybrid passenger vehicle is proven achievable in real-life applications. Acknowledgements The authors would like to thank Universiti Kuala Lumpur, Malaysian Institute of Industrial Technology (UniKL MITEC), for providing conducive environment and technical support for this project.

References Britannica (2020) Industrial revolution. Encyclopedia Britannica. https://www.britannica.com/ event/Industrial-Revolution. Accessed 10 Sept 2020 Climate Change Division (2018) Sources of greenhouse gas emissions. https://www.epa.gov/ghg emissions/sources-greenhouse-gas-emissions#overview. Accessed 28 June 2022 Foote E (1856) Circumstances affecting the heat of the sun’s rays. Am J Sci Arts 22:382–383 Global Climate Change Vital Signs of the Planet (2020) Is it too late to prevent climate change? https://climate.nasa.gov/faq/16/is-it-too-late-to-prevent-climate-change/. Accessed 28 June 2022 Harrison R (2020) How Tesla went from the verge of bankruptcy to the most valuable automaker in the world. https://inewsnetwork.net/8005/science-technology/how-tesla-went-from-the-vergeof-bankruptcy-to-the-most-valuable-automaker-in-the-world/. Accessed 28 June 2022 Katwala A (2018) The spiralling environmental cost of our lithium battery addiction. https://www. wired.co.uk/article/lithium-batteries-environment-impact. Accessed 28 June 2022 Levi M (2013) Climate consequences of natural gas as a bridge fuel. Climatic Change 118(3):609– 623 Russell R (2006) Nitrogen oxides—nitric oxide (NO) & nitrogen dioxide (NO2 ). Windows to the Universe. https://windows2universe.org/physical_science/chemistry/nitrogen_oxides.html. Accessed 28 June 2022 Soto J (2004) How a fuel cell works. Popular Science. https://www.popsci.com/scitech/article/ 2004-01/how-fuel-cell-works/#:~:text=It%20permits%20the%20positively%20charged,with% 20oxygen%20to%20form%20water. Accessed 28 June 2022 US Energy Information Administration (2020) How much carbon dioxide is produced when different fuels are burned? https://www.eia.gov/tools/faqs/faq.php?id=73&t=11. Accessed 17 June 2020

Chapter 4

Bio-Based Adhesive from Extracted Durian Seed Powder Noor Faizah Che Harun, Muhamad Mohd Rosli, Mohd Aizuddin Shahmi A’zim, Haniza Kahar, and Mizah Ramli

Abstract In this project, bio-based adhesives were produced from extracted durian seeds powder by two methods: non-heating and heating raw materials methods. Biobased adhesives in this project were prepared by extracting the starch powder from durian seeds. The obtained durian seeds starch was to be then grinded and sieved to make it uniform in size. Subsequently, the durian seed starch powders were roasted and mixed with borax and sodium hydroxide at certain amount for cleaning and hardening. The resultant bio-adhesives were characterized its physical and mechanical testing such as FTIR analysis, tensile strength test and shear strength test. The resultant adhesives in this project were expected to be compatible with current commercial synthetic adhesives. Moreover, bio-based adhesives in this project will be benefited for alternating material replacement of synthetic adhesives, sustainability as well as availability at the lowest price. This bio-based adhesives are expected to have a high potential to be applied and marketed in various industries such as in the wood bonding technology in furniture industries and as surgical tape for medical applications. Keywords Adhesive · Bio-based · Extracted durian seed powder · Heating · Non-heating

N. F. C. Harun (B) · M. M. Rosli · M. A. S. A’zim · H. Kahar Malaysian Institute Chemical and Bioengineering Technology, Universiti Kuala Lumpur, Lot 1988, Bandar Vendor, Taboh Naning, 78000 Alor Gajah, Melaka, Malaysia e-mail: [email protected] M. M. Rosli e-mail: [email protected] M. A. S. A’zim e-mail: [email protected] H. Kahar e-mail: [email protected] M. Ramli Centre for Advanced Research on Energy, Universiti Teknikal Malaysia Melaka, Hang Tuah Jaya, 78000 Durian Tunggal, Melaka, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 A. Ismail et al. (eds.), Materials Innovations and Solutions in Science and Technology, Advanced Structured Materials 173, https://doi.org/10.1007/978-3-031-26636-2_4

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4.1 Introduction Even though synthetic adhesives such as formaldehyde-based adhesive, urea formaldehyde, melamine–formaldehyde and phenol formaldehyde are still dominants due to several advantages, including their easy regulation of viscosity or thickness for optimal final application. However, formaldehyde-based synthetic adhesives are continuously releasing formaldehyde emissions during the production of the adhesive. The released formaldehyde will give a bad effect to the human and the environment (Mantanis et al. 2017). Moreover, synthetic adhesives are costly and the depletion of the petrochemical feedstock increased the trend to develop bio-based adhesive. The development of bio-based adhesive also can be used to overcome the excessive agriculture by product. The production of bio-based adhesive could overcome the non-renewability problem of synthetic adhesives (Frihart and Hunt 2010; Liu et al. 2012; Mathias et al. 2016). Starch is one of the most important carbohydrates in human diets. Starch-derived adhesives have tremendously been studied for uses in several applications such as manufacturing wood composite, paper and textile industries as binders and sizing materials (Liu et al. 2011; Alamsyah et al. 2020). Several fruits that been developed as a bio-based adhesive such as jackfruits-based adhesives (Madruga et al. 2014; Shetty et al. 2016). Fresh durian seed consists largely of starch and thus, it can be considered as such a suitable raw material for producing bio-based adhesives. Durian fruits can easily be found in tropical countries especially in South East Asia; in Malaysia, in Thailand, in Philippine and in Indonesia hence the feedstock of durian is sustainable (Nuryawan et al. 2020). The main objective of this project is to develop a bio-based adhesive through nonheating or heating raw materials. These methodologies were developed in attempting to produce eco-friendly adhesives with desirable viscosity, shear strength and tensile strength suitable for the related industrial application and market.

4.2 Methodology 4.2.1 Preparation of Durian Seed Powder A certain amount of durians seeds were washed using water and dried in a hot air oven for 12 h to remove moisture content. Dried durian seeds were grounded into a fine powder using mixer-grinder. Then, the grinded powders were sieved using a 80-mesh sieve to remove big chunks. It was stored in a plastic container and kept in the freezer to prevent from the microbial attack till further use.

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Fig. 4.1 The construction for preparing bio-based adhesive through non-heating method

4.2.2 Preparation of Bio-adhesive Without Roasting Raw Materials (Method A) Durian seed powders (33.3 g) and 0.66 g of sodium tetraborate were mixed together in a 500 mL of beaker. Then, 200 mL of distilled water was added into the mixture. After stirring the mixture for 5 min, 3.33 g of NaOH was then added into the mixture solution and subsequently, continue stirred for 15 min until the mixture solution became viscous. Figure 4.1 shows the construction for preparing bio-based adhesive by non-heating method.

4.2.3 Preparation of Bio-adhesive by Roasting Raw Materials (Method B) Sodium tetraborate weighing of 0.66 g was mixed together with 33.3 g of durian seed powder in a 500 mL of beaker. Then, the mixture compound was directly roasted on a magnetic heater. The mixture was roasted were roasted for 5 min and followed by adding 200 mL of distilled water into the mixture and continued stirring. After 5 min, 3.33 g of NaOH was added into the mixture solution and continued stirring with a magnetic stirrer. After 15 min of stirring, viscous gum solution was obtained.

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4.2.4 Preparation of Bio-adhesive by Roasting Raw Materials with HCl (Method C) 1 mL of 0.01 N HCl was added onto durian seed powder weighing of 33.3 g in a 500 mL of beaker. The mixture was roasted at 70 °C for 5 min, and then, 0.66 g of sodium tertraborate was added into the roasted mixture. Next, 200 mL of distilled water was added, and followed by stirring the mixture. After 5 min of stirring, 3.33 g of NaOH prills was added into the mixture, and continue stirred for 20 min. Viscous gum solution was obtained after continue stirred.

4.2.5 Preparation of Bio-adhesive by Roasting Raw Materials with HCl and H2 SO4 (Method D) Durian seed powder weighing of 30 g was mixed with 0.3 mL of 0.01 N HCl and 0.1 mL in a 500 mL of beaker. Then, the mixture was roasted at 70 °C on a magnetic heater. After 5 min of roasting, 0.2 g of NaOH and 180 mL of distilled water were added into the mixture and stirred the solution until the solution become more viscous. Figure 4.2 shows the construction for preparing bio-based adhesive with heating method for Method B, Method C and Method D.

4.3 Results and Discussion Chemical compound of starch that extracted from durian seeds in this study was confirmed through FTIR analysis as shown Fig. 4.3. The appeared peaks at 3369, 2928, 1634, 1413, 1154, 1018, 857 and 575 cm−1 were showed as FTIR peaks for carbohydrate chemical compound. The appeared FTIR peaks for carbohydrates in the extracted powder from durian seeds proved that there were no any contamination compounds in extracted powder used for the later adhesive preparation. Moreover, the innovation of bio-based adhesive utilizing starch extracted from durian seeds in this project was developed through several methodologies; heating or non-heating the raw materials. In heating method system, samples with concentrators, which are hydrochloric acid and sulfuric acid and sample without concentrator were prepared. As the results, the obtained bio-based adhesive through with non-heating method (Method A) was less viscous than the obtained bio-based adhesive with heating method (Method B) as shown in Fig. 4.4. Through this observation, it can be expected that, by inserting the step of roasting of raw material could produce a better bio-based adhesive than without roasting step. Furthermore, for heating method systems, bio-based adhesive prepared together with concentrators showed more viscous than that bio-based adhesive without concentrators. Samples prepared with stronger acid exhibited more viscous and

4 Bio-Based Adhesive from Extracted Durian Seed Powder

Fig. 4.2 The construction for preparing bio-based adhesive through heating method

Fig. 4.3 FTIR spectrum of extracted powder from durian seeds

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Fig. 4.4 Bio-based adhesive prepared through (left) Method A and (right) Method B

Fig. 4.5 Bio-based adhesive prepared through Method C

thicker compared to that adhesive prepared with less acid. The obtained bio-based adhesives from Method C and Method D were shown in Figs. 4.5 and 4.6, respectively. The presence of concentrators aided to produce the best bio-based adhesives.

4.4 Conclusion From four methods that been developed in this project, roasting raw materials and utilizing a concentrator show desirable viscous bio-based adhesives from durian seeds powder. Further analysis and application studies of obtained bio-based adhesive from durian seeds powder are now under progress. The formulation and methodology developed in this project is expected to be a fundamental study in the related field as

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Fig. 4.6 Bio-based adhesive prepared through Method D

well as could be applied and/or commercialized such as wood bonding technology in furniture industries, can be used in surgical tape for medical industries and various application in other related industries. Acknowledgements The authors thank Universiti Kuala Lumpur Malaysian Institute of Chemical and Bioengineering Technology, Melaka, Malaysia for providing resources and necessary facilities for producing the bio-based adhesive and analyses.

References Alamsyah EM, Sutrisno NA, Widyorini R (2020) Identifying best parameters of particleboard bonded with dextrin-based adhesives. Agriculture 5:345–351 Frihart CR, Hunt CG (2010) Adhesive with wood materials. In: Bond formation and performance, General Technical Report FPL-GTR-190, (Chap. 10). Wood Handbook, Madison, USDA 10: 1–24 Liu X, Wang Y, Cao Y, Yadama V, Xian M, Zhang J (2011) Study on dextrin-derived curing agent for waterbone epoxy adhesive. J Carbohydr Polym 83:1180–1184 Liu J, He C, Yu M, Zhang H, Hou R (2012) Decorative materials from rice straw and cornstarch adhesives. For Product J 62(2):150–156 Madruga MS, Albuquerque FS, Silva IR, Amaral DS, Magnani M, Neto VQ (2014) Chemical, morphological and functional properties of Brazilian jackfruit (Artocarpusheterophyllus L.) seeds starch. Food Chem 143:440–445 Mantanis GI, Athanassiadou ET, Barbu MC, Wijnendaele K (2017) Adhesive system used in the European particleboard, MDF and OSB industries. Wood Mat Sci Eng 13:104–116 Mathias JD, Grediac M, Michaud P (2016) Bio-based adhesives. In: Biopolymers and biotech admixtures for eco-efficient construction materials (Chap. 16), France, pp 369–385 Nuryawan A, Ridwansyah AAM, Widyorini R (2020) Starch based adhesives made from Durian Seed through dextrinization. J Phy: Confer Series 1542:1–7 Shetty M, Fernandes CM, Suraksha P, Karkera N, Hedge K, Shet VB, Rao V (2016) Production of eco-friendly adhesive from jackfruit seed. Research J Chem Env Sci 4(4S):102–106

Chapter 5

Review of the Development of Palm Broom in Producing Food Packaging Mohamad Sazali Said, Jum’azulhisham Abdul Shukor, Mohamad Firdauz Mohamad Ridzuan, Muhammad Aman Azizi Saiful Azahar, and Muhammad Zikry Zamzuri Abstract Citizens nowadays are environmentally conscious; thus, they look for environmentally friendly things to use on a regular basis. They want items that are made in a way that is not harmful to the environment. This initiative will use oil palm fronds to manufacture biodegradable paper, which will then be used to make food packaging. Oil palm is a well-known and widely farmed plant family, especially in Indonesia and Malaysia. Oil palm is one of the most economically important plants since it is utilized in a wide range of products and foods. This has resulted in an overabundance of oil palm waste, which is causing environmental issues. This initiative will use oil palm fronds to develop biodegradable paper, which will then be used to construct food packaging. This project was undertaken because the decomposition of oil palm waste has resulted in environmental contamination such as air pollution and soil pollution. This product will avoid the accumulation of oil palm waste, reducing the environmental impact immediately. Initially, studies were conducted to investigate the environmental impact of oil palm trash. According to the reasoning, this product was created by turning oil palm brooms into paper. The brooms will be mashed into pulp after being blended with water. After that, the pulp will be placed into a mold and shaped into a paper. After that, the pulp will be dried at room temperature to form paper that will be used for food packaging. The product’s paper is used to make biodegradable and environmentally friendly food packaging. The finished result has a positive impact on the environment and the end M. S. Said (B) · J. A. Shukor · M. F. M. Ridzuan · M. A. A. S. Azahar · M. Z. Zamzuri Manufacturing Section, Universiti Kuala Lumpur Malaysian Spanish Institute, Kulim Hi-Tech Park, 09000 Kulim, Kedah, Malaysia e-mail: [email protected] J. A. Shukor e-mail: [email protected] M. F. M. Ridzuan e-mail: [email protected] M. A. A. S. Azahar e-mail: [email protected] M. Z. Zamzuri e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 A. Ismail et al. (eds.), Materials Innovations and Solutions in Science and Technology, Advanced Structured Materials 173, https://doi.org/10.1007/978-3-031-26636-2_5

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user in a variety of ways. To summarize, the accumulation of oil palm waste can be solved via innovative food packaging, hence minimizing the environmental impact of inadequate oil palm waste treatment. This project also resulted in a product that is both environmentally friendly and safe to use. Keywords Oil palm waste · Food packaging · Biodegradable paper · Environmentally friendly

5.1 Introduction Packaging materials allow foods to be preserved, protected, merchandized, marketed, and distributed. They play an important role in ensuring that these foods reach customers in a safe and healthy manner without sacrificing quality. The interaction between the food and contact with the packing material is ongoing and adds to the changes that might occur in these foods over time. As a result, while selecting the proper package for a certain food product, various aspects must be addressed. In general, packing materials can be stiff or flexible. Plastic films, papers, foil, various types of vegetable fibers, and clothing are all examples of flexible packaging materials that may be used to produce wrappings, sacks, and sealed or unsealed bags (Raheem 2013). Paper and paperboards account for 31% of the worldwide packaging market and are the most used in food packaging for product containment and protection, ease during storage or consumption, and conveyance of vital information to customers, including marketing elements (Deshwal et al. 2019). In the year 2000, packaging accounted for around 47% of total paper and paperboard production. Paper carries an environmentally favorable label, making it the preferred option for food businesses, and is widely used in elementary and secondary schools (Khwaldia et al. 2010). Paper and paperboard are commonly used for ice cream cups, microwave popcorn bags, baking paper, milk cartons, fast-food containers such as pizza, beverage cups, and so on. Paper may be made from any raw material that can be shaped into a continuous sheet. The characteristics of paper pulp and the papers that follow are directly affected by the fiber quality. The most typical reasons for selecting one fiber over another are the length, diameter, and thickness of its wall. For papermaking, pulp made from oil palm fronds has been proven. As a result, in order to maximize the use of the vast biomass created by Malaysia’s palm oil industry, this study was carried out with the goal of investigating the papermaking potential of this industrial by-product (Ghazali et al. 2009). Oil palm fronds were employed in this investigation because they are regarded as a viable non-wood lignocellulosic compound for paper manufacture due to their 43.8% cellulose content, which falls within the acceptable range of wood fiber (40–45%). Meanwhile, the lignin concentration of oil palm leaves has been observed to be approximately 19%, which is in the low range of those found in wood resources (18–25%). As a result, the compositions found in oil palm leaves are thought to be ideal for use in paper production (Singh et al. 2013).

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The present project’s goal is to create biodegradable paper from oil palm fronds. Based on confirmation study, the oil palm fronds were selected for use in the papermaking process. This will help preserve the environment from deforestation and poor oil palm trash handling.

5.2 Methodology Oil palm fronds (OPF) were chosen as raw material. Only petioles of the OPF were needed for this paper-making project and were bought from vendor in 10 kg. The first step was to cut all the OPF petiole into 1 cm to ease the grinding process afterward. After cutting it, the petiole will be mixed with water and baking soda and let it sit for 10 min to let it soak into the petiole. To maintain the alkalinity of the water, baking soda is one of the materials that are excellent and easy to procure. After that, boiling process was applied to the soaked petiole and boiled for 2 h to make it smooth and fine pulp. Furthermore, dyeing process is used rather than bleaching in this project. Thus, the residuals are dyed to turn the paper into any desired color. Other than that, the binder is also important as residual sources and is prepared simultaneously to keep the fiber together and strengthen the paper. Aloe vera pulp and corn flour were used to prepare it. The skin of the aloe vera leaf was removed, and the transparent part will be blend together with corn flour. The reason why aloe vera was chosen as a binder was because it presents good anti-microbial activity. It is also produced long life to paper and avoided fungal and bacterial broadening in paper. On the other hand, corn flour acts as a starch and produces the stickiness to paper and it is also an excellent natural binder. After that, blending process was applied by mixing the dyed materials with the self-made binder and warm water by following a predefined percentage. Next, to obtain uniformity and consistency in the pulp, the pulp will undergo process of beating. Consequently, all the water in the pulp was transferred to muslin cloth to remove the excess water. To detach the paper after drying, flat plastic material was applied and acts as an excellent substitute-laminated material. Moreover, the drying process only allowed the pulp to semi-dry naturally under the sun. Therefore, pressing was applied before paper dries completely by using a small roller and then again allowed to dry naturally under the sun completely to make the paper flat and straight. Lastly, to estimate the paper quality, the paper must dry completely. The bursting strength, moisture content, and bursting factor of the paper were measured and calculated by a formula (Patel 2016).

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5.3 Results and Discussion Drawing paper for artists, permanent document paper, dark-colored card sheets, deckle-edged stationery, exclusive greetings, and a variety of fancy decorative wraps, unique paper for carry bags, water mark paper certificates, filter papers and pads, as well as other cultural grades such as covers, duplicating paper, and tissue paper are all produced by the handmade paper industry. These items are in high demand in the home market and are used in the stationery, greeting card, and packaging industries. They also offer a lot of untapped export potential. Handmade variety of superior quality bond paper, decorative paper, drawing paper, card sheets, mottled paper, moon rock paper, banana paper, and other types of paper can all be manufactured. Handmade paper comes in a variety of styles that can be utilized for interior design, corporate presents, and office purposes. New appealing forms of ecofriendly handmade paper are in high demand. A unique quality handmade paper can be created in small quantities and converted into value-added items to earn a fair profit. One of the aims in this project is to reduce plastic bags. A significant environmental impact is caused by the fact that plastic bags take a long time to disintegrate. A harmful material is emitted into the air when plastic bags are burnt, and hazardous compounds are released into the soil when the bags degrade in sunlight. Toxic pollution from plastic bag trash endangers the health of wildlife and people alike. By causing litter and backing up storm drains, improperly disposed plastic bags hurt the environment. In comparison with plastic bags, paper bags are more environmentally friendly. To begin with, unlike plastic bags, paper bag waste will not remain on the planet’s surface for the next 1000 years like it would be with plastic bags. Biodegradable paper packaging could save marine species from extinction in the upcoming years. Plastic in topsoil is also reducing the fertility of the land; therefore, a switch to biodegradable paper packaging is a better option for the environment. In fact, most paper bag waste dissolves in less than six months and, in most cases, serves as a source of food for flora. The second advantage that paper bags have over plastic bags is the majority of paper bags are 100% recyclable. Unlike plastic, which releases highly harmful and dangerous gases into the atmosphere during the recycling process, paper does not pose such a threat. The most important reason to use paper bags is to reduce waste. Reusable paper bags do not pollute the environment. Therefore, as a business owner and a client, you should encourage your customers to utilize it. Aside from the numerous advantages of utilizing paper bags, one of the reasons why they are so environmentally friendly is that they help save a significant amount of electricity. It is typically manufactured with locally available materials, which helps to save transportation costs and, in turn, save energy. The fact that paper bags are made from unbleached, recycled brown kraft paper makes them an excellent way to conserve natural resources, save energy, and reduce greenhouse gas emissions. To sum up, there is no doubt that more environmentally friendly options must be adopted in order to rescue the globe. Making use of paper bags is one excellent technique to do

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Fig. 5.1 Illustration of OPBF a oil palm leaf, b magnified image of oil palm leaf, c OPBF tied into broom units

so. The use of OPBF, as illustrated in Fig. 5.1 may be made to produce eco-friendly paper bags. As a result, it maximises the usage of palm tree products. Finally, oil palm is also Malaysia’s most valuable crop, changing its agricultural and economic scenario. While the oil palm mill appears to benefit the environment, both its input and output contribute to environmental destruction. On the input side, crude palm oil mills use a lot of water and energy. Outputs include large amounts of solid waste, water waste, and air pollution (Abdullah and Sulaiman 2013). This project was made with oil palm broom, which can help prevent the accumulation of oil palm waste and thereby protect the environment. The completed prototype is seen in Fig. 5.2.

5.4 Conclusion The study concentrated on the use of oil palm broom to create handmade paper. It was discovered that when combined with starch, palm broom can be used to make handmade papers. The end result is paper bags for food packaging. These materials are safe for the environment and pose no health risks when handled. Furthermore, it has the potential to reduce the environmental impact of palm oil waste accumulation and the use of plastic bags.

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Fig. 5.2 Food packaging made from oil palm broom

Acknowledgements The work is ostensibly supported by the Dana Penyelidikan & Inovasi MARA (DPIM) 2021, MARA 600-6/4/3 project.

References Abdullah N, Sulaiman F (2013) The oil palm wastes in Malaysia. In: Biomass now—sustainable growth and use. United Kingdom, London Deshwal GK, Panjagari NR, Alam T (2019) An overview of paper and paper based food packaging materials: health safety and environmental concerns. J Food Sci Technol 56(10):4391–4403 Ghazali A, Wan Rosli WD, Law KN (2009) Pre-treatment of oil palm biomass for alkaline peroxide pulping. Cellul Chem Technol 43(7–8):331–338 Khwaldia K, Arab-Tehrany E, Desobry S (2010) Biopolymer coatings on paper packaging materials. Compr Rev Food Sci Food Saf 9(1):82–91 Patel B (2016) Manufacturing of environmental friendly paper from domestic residuals of fruits and vegetables. Int J Eng Res Technol 5(10):1–10 Raheem D (2013) Application of plastics and paper as food packaging materials. Emir J Food Agric 25(3):177–188 Singh P, Sulaiman O, Hashim R, Peng LC, Singh RP (2013) Using biomass residues from oil palm industry as a raw material for pulp and paper industry: potential benefits and threat to the environment. Environ Dev Sustain 15(2):367–383

Chapter 6

Formulation of Emulsion Containing Chloramphenicol and Cinnamon Essential Oil for Topical Use Siti Hajar Musa, Nurhanis Fasihah Muhamad, Fatin Fathia Mohd Ali, and Nur’Aisyah Rifhan Mohammad Shuhaimi Abstract Methicillin-resistance staphylococcus aureus (MRSA) is a fatal pathogen that causes infections in various parts of the body due to high resistance toward wide antibiotics alternatives. The return of chloramphenicol is believed to overcome antibiotic-resistance issues of MRSA. In this study, chloramphenicol was cooperated with cinnamon essential oil in which the combination has been reported to be synergistically effective against MRSA. The emulsion carrier was formulated using both a high-shear homogenizer and an overhead stirrer homogenizer. Three emulsions were prepared at different compositions of cinnamon essential oil, water and surfactant based on the constructed ternary phase diagram. Samples with different formulation (F 1 , F 2 and F 3 ) were subjected to several tests including the stability, rheological, colony and invitro release analysis. F 1 , F 2 and F 3 possessed good stability against phase separation for 1 month storage at temperature 4 and 25 °C. All the formulations were having pH values within the range of 3–5 as well as showing no mold and microbial growth after been incubated on nutrient agar plates at controlled conditions. From the rheological aspect, non-Newtonian and pseudoplastic flow behavior well-suited an emulsion for the topical used. A Franz diffusion cell was used in the permeation study where F 1 resulted in up to 60.83% of chloramphenicol permeation through the cellulose acetate membrane. This corresponded to controlled release mechanism and best-fitted to zero-order kinetic behavior (R2 = 0.9937). Preliminary studies have proven that the formulated emulsion has a promising potential as topical medicament and could open up new possibilities for the production of pharmaceutical products. The increase in demand of topical skin treatment is predicted in this country S. H. Musa (B) · N. F. Muhamad · F. F. M. Ali · N. R. M. Shuhaimi Faculty of Pharmacy and Health Sciences, Royal College of Medicine Perak, Universiti Kuala Lumpur, 30450 Ipoh, Perak, Malaysia e-mail: [email protected] N. F. Muhamad e-mail: [email protected] F. F. M. Ali e-mail: [email protected] N. R. M. Shuhaimi e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 A. Ismail et al. (eds.), Materials Innovations and Solutions in Science and Technology, Advanced Structured Materials 173, https://doi.org/10.1007/978-3-031-26636-2_6

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together with other neighboring countries. The closely sharing genetic pool and environmental climate result in skyrocketing skin problems. Thus, the formulation could generate a great potential for a better future. Keywords Formulation · Topical · Emulsion · Chloramphenicol · Cinnamon essential oil

6.1 Introduction An emulsion is a mixture of two immiscible liquid phases that are able to form a stable homogeneous mixture by dispersing one into another. An emulsion system consists of two main phases: the continuous phase that is also known as the external phase and the dispersed phase or known as internal phase (Chrisman et al. 2012). Disapproving contact between water and oil phases has led to an unstable system of emulsion (Akbari and Nour 2018). However, it can be stabilized through the modification and formation of small droplet sizes and the presence of an interfacial film that is able to repel the small droplets (Chrisman et al. 2012). A mechanical energy is required to disperse one phase into another phase to form an emulsion. The help of a surface-active agent (surfactant) is necessary to form a stable emulsion and avoiding the phases from separation to different layers according to their density contradiction. Thus, incorporation of a surfactant into an emulsion is important to achieve a well-formulated emulsion with longer shelf-life. Staphylococcus aureus (S. aureus) is one of the prevalent bacteria causing infections in human with the ability to resist numerous current antibiotics’ action. S. aureus had undergone a transformation to evolve becoming a new bacteria strain by altering itself. Most of the common infections are skin and soft tissue infections that may cause complications such as endocarditis, osteomyelitis, foreign-body infections, sepsis, endovascular infections septic arthritis and pneumonia (Knox et al. 2015). Methicillin-resistant S. aureus (MRSA) strain is when the bacteria survived perseverantly within the hospital surrounding due to its concurrently resistance to various groups of traditional antibiotics. This includes aminoglycosides, beta-lactam antibiotics, tetracyclines, lincosamides, rifampin and quinolones (Uzair et al. 2017). Compared to the current drug, chloramphenicol is considered as an old antibiotic, but it is stated to have a good susceptibility in treating the MRSA infection (Fayyaz et al. 2013). Besides, chloramphenicol and cinnamon essential oil are proven to possess antibacterial activity (Green et al. 2012) that would be beneficial in treating MRSA. Cinnamon essential oil is reported to be a great combination to chloramphenicol because of its strong broad-spectrum that exhibits as synergistic enhancers. The combination of cinnamon essential oil and chloramphenicol is believed to reduce the minimum effective dose and reduce the adverse effect of the drugs (Kalita et al. 2015). Currently, the common treatment for the MRSA infection is by the intravenous or oral route. Both routes need frequent dosing (Hassoun et al. 2017). Frequent dosing

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by the intravenous route or injection is non-patient compliance and painful for the patients to endure. Thus, they are less favored among the patient as compared to the topical treatment. Topical administration is defined as a treatment to the skin and mucous membranes for localized effects. It can be classified as creams, gels, lotions and ointments. By choosing topical administration, it is believed to improve the patient compliance by reducing the irritation effect during the injection process and it is easy for self-treatment (Singla et al. 2012). This application technique is suitable for the patient even though the drug needs frequent dosing as it is an invasive and non-irritating method. The advantages of topical administration are avoidance of the first pass metabolism which is the liver, and it prevents the fluctuation in drug level and toxicity (Sharadha et al. 2020). Combining cinnamon essential oil with chloramphenicol in one emulsion formulation is an act to provide an alternative treatment to replace the current therapeutic approach. Theoretically, as the antibiotic is directly applied on the site of action, this would reduce the effective dose per treatment. As the effective dose can be lessen, the possible unwanted effects can be avoided, hence becoming more cost-effective (Atki et al. 2019). Highly hydrophobic chloramphenicol with large molecular size has raised an issue in the carrier development for topical treatment. The emulsion system that is thermodynamically unstable faced a major challenge in order to form a stable emulsion.

6.2 Methodology 6.2.1 Construction of the Calibration Curve The chloramphenicol standard stock solution was diluted with acetonitrile and prepared at concentrations of 0.2, 0.1, 0.05, 0.025 and 0.0125 mg/mL through the serial dilution technique. Standard absorbance was analyzed using an ultraviolet– visible (UV–Vis) spectrophotometer at 278 nm wavelength. The absorbance data was plotted to the graph against the concentration of the chloramphenicol prepared.

6.2.2 Construction of the Ternary Phase Diagram Cinnamon essential oil, Tween80 and distilled water were weighted at various proportions ranging from 0.100 to 100.0. A 0.5 g total weight of mixture was placed into 10 mL centrifuged tubes. Then, the mixture was vortexed for 5 min before proceeding to the centrifugation process. The appearance of the mixture was observed and recorded. Steps were furthered by repeating the addition of water according to different percentages from 0 to 100%. The observation was reported by plotting

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the ternary phase diagram using the Chemix software and the optimum and stable compositions of emulsion were selected.

6.2.3 Chloramphenicol Solubility Study Chloramphenicol (1%, w/w) was added into two different concentrations of cinnamon essential oil (5 and 10%, w/w) and dissolved at temperature 30 °C with continued stirring. After the chloramphenicol was dissolved and cinnamon essential oil was observed as translucent, additional chloramphenicol was added into the same oil–chloramphenicol mixture until a non-transparent and saturated cinnamon essential oil-chloramphenicol mixture was observed. The cumulative percentage of chloramphenicol which was dissolved effectively in the clear transparent cinnamon essential oil with no precipitation sign after heating and mixing was recorded as the highest amount of chloramphenicol that can solubilized in the oil.

6.2.4 Formulation of an Emulsion Containing Chloramphenicol and Cinnamon Essential Oil Cinnamon essential oil (5.0–10.0%, w/w), beeswax (0.2%, w/w) and chloramphenicol (0.3%, w/w) were prepared and labeled as the oil phase. Distilled water (63.2 to 78.2%, w/w), Tween80 (15–25%, w/w) and xanthan gum (0.6%, w/w) were prepared and labeled as the aqueous phase. Both phases were stirred and heated at a temperature of 45 °C. It was then homogenized using a high-shear homogenizer at 13,000 rpm for 30 min. The formulated emulsion was further proceeded to a highspeed digital overhead stirrer for an hour. Phenonip was added into the mixture as preservative.

6.2.5 Over-Time Stability Study The formulated emulsions were stored at different storage conditions: 4, 25 and 40 °C for 1 month. The physical appearances of emulsions were observed, and their individual pH value was recorded, weekly.

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6.2.6 Freeze–Thaw Cycle Stability Study The formulated emulsions were stored in two storage conditions for 24 h each. Sets of temperature setting used were: (i) 4 and 25 °C (C-RT), (ii) 25 and 40 °C (RTMW) and (iii) 4 and 40 °C (C-MW). This cycle of storage was repeated twice for each emulsion. Stability analyses were carried out in triplicate with respect to the individual physical observation and pH reading.

6.2.7 Colony Count Study Three sets of seven microcentrifuge tubes were filled with 900 μL of sterile saline; each set was numbered 10–1 till 10–7 . The formulated emulsions with 100 μL volume were appended into the first corresponding tube (10–1 dilution), and serial dilution was carried out by transferring 100 μL of the suspension to the following micro centrifuge tubes until 10–7 . A 100 μL from each tube was drawn out and was spread using the spreading technique onto the nutrient agar plate. The plate was further incubated at a storage temperature of 37 °C for 16–18 h. The appearances of colonies were observed and counted (if any).

6.2.8 Rheology Study A modular compact rheometer was used to determine the rheological behavior of the formulated emulsions. The shear rate ranged from 0.01 to 50.00 s−1 at a controlled temperature (25 °C). After the sample was placed on the plate, it took 5 min for the instrument to equilibrate the measurement beforehand. From the 100 data points generated, average viscosity results were recorded in Pascal second (Pa s). The formulated emulsion was analyzed with respect to its behavior which fitted the power law model, see Eq. (6.1): η = k y n−1

(6.1)

where η is the viscosity (Pa s−1 ), y is the shear rate, k is the consistency index of the emulsion of the nanoemulsion and n is the power (shear thinning) index (n < 1); the lower the n-value, the more shear thinning the emulsion is (Han et al. 2011).

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6.2.9 In Vitro Release Study The formulated emulsions were characterized with respect to their release potential using a Franz diffusion cell. An emulsion sample was placed on the synthetic cellulose acetate membrane at the top of the chamber. At time intervals of 0.5, 1, 2, 3, 4, 5 and 6 h, 1 mL of the sample was taken from the bottom chamber to analyze its release potential. Then, 1 mL of equal amount of fresh receptor phosphate buffer medium was replaced into the receptor chamber. The collected 1 mL sample was mixed with acetonitrile and was measured on their absorbance using an UV-spectrophotometer against the blank solution of mixture containing new phosphate buffer solution and acetonitrile.

6.2.10 Kinetic Release Study The kinetic release study was carried out with respect to five kinetic models, which are zero-order, first-order, Higuchi, Korsmeyer–Peppas and Hixson–Crowell. The construction of the graph was prepared using the respective theoretical equation model. The zero-order rate [see Eq. (6.2)] describes situations in which the rate of drug release is independent of the concentration of the drug. The first-order rate [see Eq. (6.3)] explained the rate of drug release from the system, which is concentrationdependent. Higuchi [see Eq. (6.4)] defined drug release from the insoluble matrix as a time-dependent square root mechanism based on Fickian diffusion. Korsmeyer– Peppas model [see Eq. (6.5)] devised a straightforward mathematical formula for describing drug release from a polymeric system. Q 0 − Q t = k0 t

(6.2)

ln(Q 0 /Q t ) = −k 1 t

(6.3)

Q t = kt 1/2

(6.4)

Q 1 /Q ∞ = kt n

(6.5)

1/3

1/3

Q0 − Qt

= kHC t

(6.6)

where Q 0 is the initial amount of chloramphenicol, Q t is the amount of chloramphenicol permeated, k0 is the zero-order rate constant, k1 is the first-order constant, k is the constant reflecting the design variables of the system, Q 1 /Q ∞ is the fraction of drug released over time, n is the release exponent, k H C is the Hixson–Crowell rate constant, and t is the time.

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6.2.11 Statistical Analysis All analyses were carried out in triplicate, and all data are shown as mean ± standard deviation (n = 3).

6.3 Results and Discussion 6.3.1 Ternary Phase Diagram Analysis Figure 6.1 shows the constructed ternary phase diagram that consists of three main components of emulsion that are oil, water and Tween80 as the surfactant. Only regions with blue and light blue colors possessed a stable system with one phase emulsion after the centrifugation process. The best emulsion was observed to be at a high content of water (more than 60%), with oil and Tween80 content not greater than 20 and 30%, respectively. Based on this diagram, three readings (F 1 , F 2 and F 3 ) were selected with specific O/W emulsion compositions as per tabulated in Table 6.1. Meanwhile, the other region is neglected because the rest of the area reflects the conventional and turbid emulsions on the phase diagram (Azeem et al. 2009). The content of each composition will read off from the intersection of line either Tween80-water or Tween80-oil that followed the stable system for emulsion.

Fig. 6.1 Constructed ternary phase diagram with three main components; water, cinnamon essential oil and Tween80

62 Table 6.1 Composition of F 1 , F 2 and F 3

S. H. Musa et al. Formulation components

Formulation compositions (%)

Oil

F1

F2

F3

5

5

10

Water

80

75

65

Tween80

15

20

25

With the help of the ternary phase diagram, the presence of the emulsion formation zone can be demonstrated. The ternary phase diagram is crucial to produce a good and stable emulsion because of their equilibrium conferring to the composition of those three components at persistent pressure and temperature, therefore allows to select the desired points with respect to the physiochemical properties (such as appearance, flowability and concentration of excipients). Past research has reported the value from the phase diagram was significant in designing, defining and characterizing the drug delivery systems (Syed and Peh 2014). By mixing oil, water and surfactants in various proportions, a wide variety of structures and phases can be produced.

6.3.2 Chloramphenicol Solubility Analysis The 5% of cinnamon essential oil was observed to be successfully solubilized the chloramphenicol up to 0.3% while the 10% oil was able to solubilize the chloramphenicol up to 0.5% (Table 6.2). The solubility test was repeated until 0.7% to make a comparative assessment. The physical evaluation through visual checking indicates precipitation formation on the surface of cinnamon essential oil, and the color changed during the stability analysis after the addition of 0.4 and 0.6% of chloramphenicol. One of the essential criteria for achieving the desired concentration of the drug for pharmacological response is solubility in which the mechanism of dissolution of the solvent to give a homogeneous system. It was also reported that the degree of solubility of a product in a particular solvent is assessed as the concentration of saturation which does not increase its concentration in the solution by adding more solvent (Savjani et al. 2012). Table 6.2 Limit of chloramphenicol solubility in cinnamon essential oil Cinnamon essential oil (%)

Chloramphenicol content (%) 0.1

0.2

0.3

0.4

0.5

0.6

0.7

5

/

/

/

×

×

×

×

10

/

/

/

/

/

×

×

/ = Chloramphenicol solubilized; × = Insolubilized chloramphenicol

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6.3.3 Over-Time Stability Analysis Physical observation The results of this current study showed that all formulation samples were stable in different storage conditions, 4, 25 and 40 °C except for F 1 and F 3 at 40 °C at the end of the experimental period (Table 6.3). These results have related with higher temperature that was kept for such a long period of time (week 4); thus, the oil from the emulsion starts to show the separation. The heights of cream layers were observed after 4 weeks in different storage conditions. Smaoui et al. (2017) and Goodarzi and Zendehboudi (2018) stated that creaming results in phase separation and under the influence of gravity is often related to density difference between these two phases. Furthermore, Goodarzi and Zendehboudi (2018), Smaoui et al. (2017) stressed that the former emulsion starts to be altered after the first drop formation due to various time-dependent methods, which are Ostwald ripening, coalescence, flocculation, sedimentation and creaming. pH of emulsion All formulations were observed to endure an incessant escalate up to one month of observation, and for almost all conditions tested, emulsions had stable pH values (Fig. 6.2). However, a significant increase in pH was observed at 40 °C storage. High temperatures lead to hydrolysis emulsion destabilization, but it did not impact the entire emulsion efficiency because the pH values stayed about pH 3–5, which is an appropriate and non-skin-irritating pH value (Smaoui et al. 2017). Table 6.3 Phase separations and percentage of cream layer for F 1 , F 2 and F 3 at 4, 25 and 40 °C after 4 weeks storage Emulsion storage

1st week

2nd week

3rd week

4th week

F1

4 °C 25 °C 40 °C

– – –

– – –

– – –

– – +

F2

4 °C 25 °C 40 °C

– – –

– – –

– – –

– – –

F3

4 °C 25 °C 40 °C

– – –

– – –

– – –

– – +

– = No change; + = Slight change

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Fig. 6.2 The average of pH values of F 1 , F 2 and F 3 at a 4 °C, b 25 °C and c 40 °C

6.3.4 Freeze–Thaw Stability Analysis Physical observation The actual color of freshly prepared F 1 , F 2 and F 3 is pale yellow. The color of the emulsion formulation samples possessed no significant changes after the free-thaw analysis. In addition, no phase separation and creaming were revealed after the end of the freeze–thaw process. In freeze–thaw experiments, temperature cycling affects parameters apart from those specifically related to creaming, which is the real factor of emulsion instability (Matousek et al. 2003). Solid proof for the stability of the

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emulsions under investigation was provided by the absence of changes in the physical appearance of the formulations. Rapid and extreme changes of temperature mimic the potential conditions of outdoor storage. Lopez-Montilla et al. (2002) reported that a simple temperature shift causes an emulsion transition thus might alter the emulsion stability. Thus, results proved that F 1 , F 2 and F 2 were all stable against system’s deterioration. pH of Emulsion Average pH comparison during the first and second cycles of the freeze and thaw process for (a) F 1 , (b) F 2 and (c) F 3 in triplicate along with the standard deviation is shown in Fig. 6.3. The changes of pH from one cycle to another were proven to be insignificant (P < 0.005) which represent a good stability of the formulated emulsion system. Daaou and Bendedouch (2012) reported that the ionization of polar groups of film active components that cause sufficient electrostatic repulsive interactions to unravel interfacial film cohesion is typically due to the pH effect on the emulsion stability. Fig. 6.3 The average of pH comparison during freeze–thaw analysis for a F 1 , b F 2 and c F 3

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Fig. 6.4 Results on agar plate with no microbial growth for a F 1 , b F 2 and c F 3 after stored in an incubator (37 °C) for 18 h

6.3.5 Colony Count Analysis Based on the observation, there is no microbial growth present on the agar plate (Fig. 6.4). Zhang et al. (2017) claimed that the presence of microbes or total plate count is crucial to determine whether the preservative and oil (cinnamon essential oil) used in this study is effective in inhibit the growth of microorganisms from spreading. Significantly, determination of quantitative study related to bacteria growth that is associated to animal and human is depending on the types of agars medium and incubation parameters used in the analysis. According to Allen et al. (2004), nutrient agar medium with short incubation time and high incubation temperature (35–37 °C) were preferred for the growth of bacteria from animals and humans.

6.3.6 Rheology Analysis All the plotted graphs (Fig. 6.5) show a similar pattern in which the shear stress increases gradually with shear rate. Therefore, the emulsions are said to be nonNewtonian (Abd et al. 2014). On the other hand, the viscosity declined as the shear rate increased thereby the samples followed shear thinning and pseudoplastic behavior (Hojjat et al. 2011). Rheological analysis was used to evaluate the stability of the emulsion. Rheology is the technique that explains a material’s response to a superimposed stress. In this test, xanthan gum plays the main role to enhance the emulsion stability by aiding the emulsion to increase the viscosity and lessening their mobility (Tekin et al. 2020).

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Fig. 6.5 Rheological behavior of F 1 , F 2 and F 3

6.3.7 In Vitro Permeation Analysis The most efficient permeation was showed by F 1 with 60.83% chloramphenicol permeation, followed by F 2 and F 3 with cumulative permeation rate at 46.61 and 45.91%, respectively (Fig. 6.6). Each sample showed a nearly similar release for the first 3 h but F 1 showed a rapid release after the third hour. Both F 2 and F 3 showed a slow release until the end of the experiment. Drug release from a waterin-oil emulsion is mainly driven by the diffusion capacity of active agent which is chloramphenicol through the composition with slightly different amount. The release from the F 1 showed a higher released active agent amount after 6 h due to its composition of the highest amount of water and lowest amount of Tween80. According to Mandal et al. (2009), the release rate was affected by the drug– polymer ratio. The formulation with a 1:10 drug–polymer ratio exhibited the slowest release rate, whereas the formulation with a 3:10 drug–polymer ratio exhibited the

S. H. Musa et al.

Percentage of cumulative cyclosporine in total solution (%)

68 70

F1

60

F2

F3

50 40 30 20 10 0

0

1

2

3 4 Time (hours)

5

6

7

Fig. 6.6 Permeation profile of the formulated chloramphenicol-loaded emulsion

fastest release rate. This indicated that the polymer concentration reduced the release rate of chloramphenicol. The polymer is one of important ingredients for the formulation of an emulsion as it acts as an emulsifying agent that stabilizes the emulsion. With low Tween80 concentration, it increased the droplet size of the emulsion and thus increased the interfacial tension between the liquid. The permeation of chloramphenicol through the membrane is easier. This explained that the highest release is exhibited by F 1 compared to F 2 and F 3 . Based on the graph, all the formulated emulsions showed almost a linear graph which indicates the release pattern of the emulsion is nearer to the controlled release rather than sustained release. The controlled release is defined as the drug level that is maintained and remained constant for an extended period of time in blood or tissue. The in vitro release study using the Franz cell is an analogy of the release of drug when applied to the skin. The synthetic cellulose acetate membrane with a pore size of 0.2 μm mimics the skin. The fresh receptor phosphate buffer medium with a pH of 7.4 used in the chamber mimics the pH of the circulatory system of the body. It is a significant analytical technique for determining the drug behavior through the different phases of development.

6.3.8 Kinetic Release Analysis All graphs (not shown) for the kinetic model showed a linear relationship to different degrees of the model. When respective correlation coefficients were compared, F 1 , F 2 and F 3 found to show its highest linearity to the zero-order model. According to Kalita et al. (2015) and Khan et al. (2013), the indication of which model bestfitted the formulation is by comparing the regression coefficient (R2 ) to determine the mechanism of chloramphenicol release. This indicated that the best-fitted model was the zero-order model for each F 1 , F 2 and F 3 with R2 value of 0.9762, 0.9937 and

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Table 6.4 Correlation coefficients determined by plotted graph corresponding to kinetic release models Emulsion

Kinetic model First-order

Zero-order

Higuchi model

Korsmeyer–Peppas

Hixson–Crowell

F1

0.9239

0.9762

0.8390

0.8899

0.9730

F2

0.9732

0.9937

0.8917

0.9266

0.9398

F3

0.9618

0.9878

0.8701

0.8995

0.9556

0.9878, respectively (Table 6.4). This zero-order kinetic model indicates the process of constant drug release with time, and it is independent of concentrations. At each hour of experiment, the same amount of active ingredient was released throughout the chamber. It was the simplest type of kinetic order. The F 1 result was slightly differed from F 2 and F 3 due to its composition with the lowest amount of Tween80 and highest amount of water content.

6.4 Conclusion The results provided in the present study indicated that three different chloramphenicol-loaded emulsions (F 1 , F 2 and F 3 ) comprising cinnamon essential oil were selected at the most stable point (water: > 60%; oil and surfactant < 20 and 30%) based on the constructed ternary phase diagram. The solubility of the formulated emulsions showed that 10% of cinnamon essential oil has successfully solubilized more chloramphenicol than the 5% of cinnamon essential oil. Formulation and further evaluation of the emulsion showed all the formulated emulsions were stable at different storage conditions throughout the 4 weeks period except for formulation F 1 and F 3 at 40 °C. Acceleration and freeze–thaw stability test also gave positive results with no significant changes on its physical appearance and pH analysis which successfully maintained in their optimum pH value range in between 3 and 4 for a topical emulsion. A good stability system is also proven by the positive result (no microbial growth) on the agar plate after been stored in an optimum condition for colony growth. The rheological analysis has proven that the emulsions possessed non-Newtonian and pseudoplastic behavior. Through the comparative study of the release study of three different compositions of formulation, it can be concluded that F 1 demonstrated to be the most efficient release of chloramphenicol with 60.83%, followed by F 2 and F 3 with 46.61% and 45.91% release within 6 h of analysis, respectively. It was found that the composition of formulation of the emulsion does give effect to the release potential of the emulsion, especially the oil, water and surfactant concentration. On the other hand, all the formulated emulsions appeared to best-fit the kinetic release of zero-order model with controlled release behavior.

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Acknowledgements The authors were grateful to the Ministry of Higher Education (MOHE), Malaysia, for funding this study under the Fundamental Research Grant Scheme (FRGS/1/2020/STG04/UNIKL/03/1).

References Abd RM, Nour AH, Sulaiman AZ (2014) Kinetic stability and rheology of water-in-crude oil emulsion stabilized by cocamide at different water volume fractions. Int J Chem Eng 5:204–209 Akbari S, Nour AH (2018) Emulsion types, stability mechanisms and rheology: a review. Int J Innov Res Sci Stu 1:14–21 Allen MJ, Edberg SC, Reasoner DJ (2004) Heterotrophic plate count bacteria—what is their significance in drinking water? Int J Food Microbiol 92:265–274 Azeem A, Rizwan M, Ahmad FJ et al (2009) Nanoemulsion components screening and selection: a technical note. AAPS PharmSciTech 10:69–76 Chrisman E, Lima V, Menechini P (2012) Crude oil emulsion-composition stability and characterization. InTech 9:1–240 Daaou M, Bendedouch D (2012) Water pH and surfactant addition effects on the stability of an Algerian crude oil emulsion. J Saudi Chem Soc 16(3):333–337 El Atki Y, Aouam I, El Kamari F et al (2019) Antibacterial activity of cinnamon essential oils and their synergistic potential with antibiotics. J Adv Pharm Technol Res 10:63–67 Fayyaz M, Mirza IA, Ahmed Z et al (2013) In vitro susceptibility of chloramphenicol against methicillin-resistant Staphylococcus aureus. J Coll Physicians Surg Pak 23:637–640 Goodarzi F, Zendehboudi S (2018) A comprehensive review on emulsions and emulsion stability in chemical and energy industries. Can J Chem Eng 97:281–309 Green BN, Johnson CD, Egan JT et al (2012) Methicillin-resistant Staphylococcus aureus: an overview for manual therapists. J Chiropr Med 11:64–76 Han NS, Basri M, Abd. Rahman MB, Raja Abd. Rahman RNZ, Salleh AB, Ismail Z (2011) Phase behavior and formulation of palm oil esters O/W nanoemulsions stabilized by hydrocolloid gums for cosmeceuticals application. J Dispers Sci Technol 32:1428–1433 Hassoun A, Linden PK, Friedman B (2017) Incidence, prevalence, and management of MRSA bacteremia across patient populations—a review of recent developments in MRSA management and treatment. Crit Care 21:211 Hojjat M, Etemad SG, Bagheri R, Thibault J (2011) Rheological characteristics of non-Newtonian nanofluids: experimental investigation. Int Commun Heat Mass Transf 38:144–148 Kalita S, Devi B, Kandimalla R et al (2015) Chloramphenicol encapsulated in poly-ε-caprolactone– pluronic composite: nanoparticles for treatment of MRSA-infected burn wounds. Int J Nanomed 10:2971 Khan S, Batchelor H, Hanson P et al (2013) Dissolution rate enhancement, in vitro evaluation and investigation of drug release kinetics of chloramphenicol and sulphamethoxazole solid dispersions. Drug Dev Ind Pharm 39:704–715 Knox J, Uhlemann AC, Lowy FD (2015) Staphylococcus aureus infections: transmission households and the community. Trends Microbiol 7:437–444 López-Montilla JC, Herrera-Morales PE, Pandey S et al (2002) Spontaneous emulsification: mechanisms, physicochemical aspects, modeling, and applications. J Dispers Sci Technol 23:219–268 Mandal B, Halder KK, Dey SK, Bhoumik M, Debnath MC, Ghosh LK (2009) Development and physical characterization of chloramphenicol loaded biodegradable nanoparticles for prolonged release. Pharmazie 64:445–449 Matousek JL, Campbell KL, Kakoma I et al (2003) Evaluation of the effect of pH on in vitro growth of Malassezia pachydermatis. Can J Vet Res 67:56–59

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Savjani KT, Gajjar AK, Savjani JK (2012) Drug solubility: importance and enhancement techniques. ISRN Pharm 2012:1–10 Sharadha M, Gowda DV, Vishal GN et al (2020) An overview on topical drug delivery system— updated review. Int J Pharm Sci Res 1:368–385 Singla V, Saini S, Joshi B et al (2012) Emulgel: a new platform for topical drug delivery. Int J Pharma and Bio Sciences 3:485–498 Smaoui S, Hlima HB, Chobba IB et al (2017) Development and stability studies of sunscreen cream formulations containing three photo-protective filters. Arab J Chem 10:S1216–S1222 Syed HK, Peh KK (2014) Identification of phases of various oil, surfactant/co-surfactants and water system by ternary phase diagram. Acta Pol Pharm 71:301–309 Tekin ZH, Avci E, Karasu S et al (2020) Rapid determination of emulsion stability by rheology-based thermal loop test. Lwt 122:109037 Uzair B, Niaz N, Bano A et al (2017) Essential oils showing in vitro anti MRSA and synergistic activity with penicillin group of antibiotics. Pak J Pharm Sci 30:1997–2002 Zhang Y, Wang Y, Zhu X et al (2017) Antibacterial and antibiofilm activities of eugenol from essential oil of Syzygium aromaticum (L.) Merr. and L. M. Perry (clove) leaf against periodontal pathogen Porphyromonas gingivalis. Microb Pathog 113:396–402

Chapter 7

Water Pollution Detection System for Illegal Toxic Waste Dumps Zuhanis Mansor and Nurul Nur Sabrina Abdul Latiff

Abstract Nowadays, there is an increment of the contaminated rivers in Malaysia due to illegal toxic waste dumping. They increased water pollution cases from a river in Malaysia, such as Johor and Selangor. This paper aims to detect real-time pollution to make the authorities take fast action to prevent widespread pollution and contamination. This work’s significance stems from its ability to wirelessly monitor real-time data, detect early pollution sources, and detect criminal activity. The system detects illegal toxic waste dumping via a wireless sensor network in every polluted river. It consists of the Arduino UNO as the microcontroller, a 9 V lithium-ion rechargeable battery as the power supply, a pH metre sensor, a DS18B20 temperature sensor, and a turbidity sensor, a SX1278 LoRa, a GPS Neo 6 m, and a SIM800C GSM. The WSN system is used to track freshwater quality measurements and is implemented at a distributed location. Each node can communicate with a range of water quality sensors. The signals from a GPS can give accurate and concise information used to estimate the exact location of the contaminated water. The collected data from each sensor will go to the sub-base station as the device network coordinator and alert the dedicated people of the activities via the GSM network. The accuracy shows that both classifications to distinguish clear freshwater and polluted water using ten different situations prove that this project has great potential for real-time detection of illegal toxic waste dumping in the target area. Keywords Water quality detection system · Wireless sensor network · Polluted water · LoRa

Z. Mansor (B) Advanced Telecommunication Technology Research Cluster, Communication Technology Section, British Malaysian Institute, Universiti Kuala Lumpur, 53100 Gombak, Selangor, Malaysia e-mail: [email protected] N. N. S. Abdul Latiff Medical Technology Section, British Malaysian Institute, Universiti Kuala Lumpur, 53100 Gombak, Selangor, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 A. Ismail et al. (eds.), Materials Innovations and Solutions in Science and Technology, Advanced Structured Materials 173, https://doi.org/10.1007/978-3-031-26636-2_7

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7.1 Introduction Nowadays, there is an increment of the polluted rivers in Malaysia due to illegal toxic waste dumping. The illegal disposal of harmful waste negatively influences human and environmental health, and waste management has become one of the critical problems for humankind (Yap et al. 2019). Some of the rivers in our country are classified in Class III, which means, according to the Water Quality Index stated, the rivers are slightly polluted because of social activities. In contrast, some rivers are classified in Class V, which means very polluted and dangerous to society because of the industrial and illegal toxic dump activities (Adilah and Nadia 2020). This initiative is a new approach for detecting environmental freshwater quality and providing authorities with further notice and alarms for potential ecotoxicity and societal health hazards (Wee et al. 2016). Any link between the criminal act of dumping hazardous waste and harmful consequences on human health should be viewed with scepticism. It is critical to safeguard the environment by identifying pollution on time and pinpointing the source of the contamination. Previous work in Ibrahim et al. (2021) examines an incident of illegal chemical dumping in Pasir Gudang, Malaysia and its potential health impacts on children. Several Pasir Putih primary school students and Pasir Putih high school students had difficulties breathing, coughing, nausea, vomiting, and disturbances of the eye and throat after they breathed an unpleasant odour at their school (Ifwan 2020). In the early morning, several of the residents of Pasir Putih also noticed a heavy, foggy smell. Two hundred forty-three tonnes had been dumped into the river Kim Kim as hazardous waste. A lorry from an unidentified location transported the chemical waste into Pasir Gudang and tossed it into the river on the night of 6 March 2019. The dumping site lies 500 m from the primary school of Taman Pasir Putih and the secondary school of Pasir Putih. Thus, this chemical reaction has indicated the possibility of respiratory issues for children being exposed in the Kim Kim river incident to high levels of toxic substances from the illegal dumping site. The pollution in Pasir Gudang is an example of a failure to learn from previous incidents in Johor in particular and other parts of the country in general (Mohd 2021). According to a previous study, exposure to the chemical can increase the risk of people developing respiratory symptoms such as wheezing and shortness of breath (D’Andrea and Reddy 2018). However, acrolein and acrylamide exposure caused oxidative stress and inflammation in animal and in vitro human airway tissue models, resulting in increased mucus discharges, bronchial wall oedema, bronchoconstriction, and tissue damage (Pan et al. 2018; Yilmaz et al. 2017; Snow et al. 2017; Xiong et al. 2018). As a result, the chemical reaction shows the possibility of people and habitat can suffering from respiratory symptoms because of the exposure to the high concentrations of toxic chemicals due to the illegal waste dumping at the incident site, the Kim Kim river. Other side effects from exposure to this traumatic incident might threaten an individual or population’s mental health, which can also develop post-traumatic stress disorder (PTSD) (Charnsil et al. 2020).

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This project aims to detect real-time pollution to make the authorities take fast action to prevent widespread pollution and contamination. The objectives that this project seeks to attain are: . To detect the appearance of the poisonous chemical by using a wireless sensor network (WSN) sensor. . To detect the location of the illegal activities by using GPS. . To alert the dedicated people nearby using GSM to take further action.

7.2 Methodology 7.2.1 Overall Systems Block Diagram This system uses seven components which for the water quality parameter will use a pH metre sensor, temperature sensor and turbidity sensor, microcontroller, LoRa, GPS, and GPRS, as shown in Fig. 7.1. This project is powered up by the Li-ion rechargeable 9 V battery in each node circuit. As an input, the water quality sensors and LoRa are embedded in each WSN. The data is continuously analysed to determine whether the quality of water is polluted or not. Due to the processing of so much information for classification, a practical, accurate detection principle to judge the presence of poisonous gas or polluted water in real time is the core element of this system detection. When pollution in real-time occurs, the microcontroller in WSN will trigger the LoRa to transmit data to the receiver LoRa in the substation centre communication node. The centre communication node will track the location of the polluted area, and the alert system is working to send the notification to the authorities through text or call which may need satellite access. By providing a rapid system detection for emergency or immediate action, it can avoid widespread pollution and criminal activity from being overlooked. This prevents pollution widespread and avoids a threat to an individual or population’s mental health.

Fig. 7.1 Overall system block diagram

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Fig. 7.2 Project flowchart

The pH metre sensors, temperature sensors, and turbidity sensors detect the water quality in real time, as shown in the flowchart in Fig. 7.2. The system keeps on running and noticing any changes in the freshwater quality. If there are changes in the water quality index during the toxic waste dumping activity detected and the index is showing as the polluted index Class V, the data will be transmitted to the substation centre communication node immediately. The substation centre communication node will receive the data of contaminated water during toxic waste dumping activity from the WSN. The GPRS will send an SMS to the authorities with the location of the movement. The GPS in the substation centre will keep running. Thus, there will be no delay in tracking the location when GPRS need to send an SMS to the authorities.

7.2.2 Project Hardware and Software Figures 7.3 and 7.4 show the connection between the circuit diagram and its installation. A 9 V rechargeable battery powers up the circuit. The pH metre, temperature sensor, and turbidity sensor are connected to the 5 V of Arduino as input to pull up the sensor module and A0, A1, and A2 as the analogue output from the sensor

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module. The sensors will keep on measuring the changes in the freshwater indexes in real time. Since this LoRa module works at 3.3 V, the 3.3 V pin on the LoRa module is linked to the 3.3 V pin on the Arduino UNO board. The communication system circuit automatically powers up when connected to the battery. GPS will detect the position and continue to track it. Until the LoRa receives data from the WSN circuit, the GSM will remain in standby mode. The GSM will then quickly send an SMS to the authorities to take swift action against the unlawful trash disposal operations. The software used in this project is the Arduino IDE. Arduino’s integrated development environment (IDE) is a cross-platform Windows framework written in the Java language. It is widely accessible for operating systems. Each of them includes a programmed microcontroller on the board and accepts the information in code form.

Fig. 7.3 WSN circuit diagram and installation

Fig. 7.4 Communication circuit diagram and installation

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7.3 Results and Discussion The pH metres sensor functions well by sensing the concentration of hydrogen ions in water and transferring it to the Arduino UNO for processing. Positive charges of hydrogen ions will be found in freshwater when it is acidic. This condition can potentially destroy all freshwater ecosystems while also emitting poisonous gases, while under alkaline circumstances, negative hydrogen ions can influence ammonia in humans. The high-precision pH sensor may assist in detecting the freshwater condition. Table 7.1 displays the accuracy of the pH sensor from the solution substance. The temperature sensor has been tested in three different water temperatures. The outcome is depicted in the graph in Fig. 7.5a. Here, we can observe the sensitivity of the DS18B20 temperature sensor. Temperature is also significant due to its impact on water chemistry. The pace of chemical reactions typically increases as the temperature rises. The turbidity programme was designed so that the lowest NTU represents the most turbid water and the highest NTU means pure water. The result for the turbidity sensor is shown in Fig. 7.5b. Turbidity causes a drop in water clarity, which is visually unattractive, as well as a decrease in photosynthetic rate and an increase in water temperature. Table 7.1 pH sensor result

Solution

pH value

Measured

Accuracy %

Tap water

7

Taking reading from pH sensor pH: 7.00 pH value: 7.00 Water is neutral (safe)

100

Potassium hydrogen phthalate

4.00

Taking reading 97 from pH sensor pH: 3.88 pH value: 3.88 Water acidity high

Mixed phosphate

6.85

Taking reading from pH sensor pH: 6.61 pH value: 6.61 Water is neutral (safe)

96.5

Sodium tetraborate

9.18

Taking reading from pH sensor pH: 9.17 pH value: 9.17 Water alkalinity high

99.8

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Fig. 7.5 a Temperature sensor and b turbidity sensor result

Real-time GPS recorders can give precise and timely information on the existence and location of illegal toxic waste dump activity sites. It takes 1 min for the GPS tracker to deliver the accurate longitude and latitude of the position. Figure 7.6 depicts the GPS coding only, wherein the GPS will continue to function when other components in communication nodes are in standby mode. This will allow the GSM to send an SMS as soon as the LoRa gets pollution data. It will shorten the time it takes for authorities to take action.

Fig. 7.6 GPS tracker and coding

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Fig. 7.7 SMS received

Figure 7.7 demonstrates an example of an SMS sent via GSM/GPRS to alert authorities. The alert warning for unlawful toxic waste disposal will be delivered as soon as the LoRa gets data from the WSN. The GSM has been programmed to remain in standby mode at all times and only to operate once. For the next operation, the system must be restarted. The data sent through SMS will include the temperature, pH value, and turbidity of the water. The SMS alarm also consists of the activity site latitude and longitude coordinates.

7.4 Conclusion In this work, the WSN system is used to track freshwater quality measures, with each node being capable of communicating with various water quality sensors. The data obtained from each sensor will be sent to the sub-base station, which serves as the device network coordinator and is installed in a dispersed location. The GPS signals can provide precise and concise information that can be utilised to determine the exact location of contaminated water and warn devoted individuals of illegal actions via the GSM network. The appropriate technique, hardware, and software for building the prototype have been used, including the use of an Arduino UNO as the microcontroller, a 9 V lithium-ion rechargeable battery as the power supply, a pH

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metre sensor, a DS18B20 temperature sensor, a turbidity sensor, an SX1278 LoRa, a GPS Neo 6 m, and a SIM800C GSM. Using a wireless sensor network (WSN) in each polluted river, this system will identify unlawful hazardous waste disposal. In the future, this system should be required to maintain the environment and play a significant part in ensuring human health. It can save lives by identifying early pollution caused by illegal toxic waste dumps. With this prototype, the user and the Ministry of Health (MOH) will have a better mechanism for detecting harmful illicit waste dump operations. Acknowledgements The authors would like to thank the Universiti Kuala Lumpur British Malaysian Institute for the provision of the Advanced Telecommunication Technology (ATT) research cluster laboratory.

References Adilah A, Nadia H (2020) Water quality status and heavy metal contains in selected rivers at Tasik Chini due to increasing land use activities. IOP Proc: Mater Sci and Eng 712(1):012022 Charnsil C, Narkpongphun A, Chailangkarn K (2020) Post-traumatic stress disorder and related factors in students whose school burned down: cohort study. Asian J Psychiatr 51:102004 D’Andrea MA, Reddy GK (2018) Health risks associated with benzene exposure in children: a systematic review. Global Pediatric Health 5:1–10 Ibrahim MF, Hod R, Toha HR et al (2021) The impacts of illegal toxic waste dumping on children’s health: a review and case study from Pasir Gudang, Malaysia. Int J Environ Res Public Health 18(5):2221 Ifwan TT (2020) SK Pasir Putih, SMK Pasir Putih Dibuka Esok. BH Online. https://www.bharian. com.my/berita/wilayah/2019/03/539387/sk-pasir-putih-smk-pasir-putih-dibuka-esok. Accessed 11 Nov 2020 Mohd FI (2021) Illegal toxic waste dumping. Encyclopedia Online. https://encyclopedia.pub/8978. Accessed 15 Mar 2021 Pan X, Wu X, Yan D et al (2018) Acrylamide-induced oxidative stress and inflammatory response are alleviated by N-acetylcysteine in PC12 cells: Involvement of the crosstalk between Nrf2 and NF-κB pathways regulated by MAPKs. Toxicol Lett 288:55–64 Snow SJ, Mcgee MA, Henriquez A et al (2017) Respiratory effects and systemic stress response following acute acrolein inhalation in rats. Toxicol Sci 158(2):454–464 Wee SY, Omar T, Aris A et al (2016) Surface water organophosphorus pesticides concentration and distribution in the Langat River, Selangor, Malaysia. Expo Health 8:497–511 Xiong R, Wu Q, Muskhelishvili L et al (2018) Evaluating mode of action of acrolein toxicity in an in vitro human airway tissue model. Toxicol Sci 166(2):451–464 Yap C, Peng S, Chee S et al (2019) Contamination in Pasir Gudang Area, Peninsular Malaysia: what can we learn from Kim Kim River chemical waste pollution? J Humanities and Edu Development 1:82–87 Yilmaz BO, Yildizbayrak N, Aydin Y et al (2017) Evidence of acrylamide- and glycidamide-induced oxidative stress and apoptosis in Leydig and Sertoli cells. Hum Exp Toxicol 36(12):1225–1235

Chapter 8

Alternative Processes for the Production of Bioactive Peptides Norfahana Abd-Talib, Alia Shahiza Shaharuddin, Emmy Liza Anak Yaji, Nur Suraya Abd Wahab, Nadia Razali, Kelly Yong Tau Len, Jumardi Roslan, Fadzlie Wong Faizal Wong, Nazamid Saari, and Khairul Faizal Paée Abstract Bioactive peptides are molecules of paramount importance with significant health benefits. These bioactive peptides extracted from various food sources demonstrated significant bioactivity and potency, including antimicrobials, angiotensin-converting enzyme (ACE) inhibitors, antioxidants, opioids, and antimicrobials. However, various challenges hindered the industrial-scale production of peptides, such as the sensory performance of peptides due to bitterness, low peptides bioavailability and yield, minimal human tests, unconfirmed molecular mechanisms, N. Abd-Talib · K. F. Paée (B) New Product Development, OHR Marketing Sdn Bhd. No. 421, Jalan Perusahaan 6, Taman Bandar Baru Mergong, Lebuhraya Sultanah Bahiyah, 05150 Alor Setar, Kedah, Malaysia e-mail: [email protected] N. Abd-Talib e-mail: [email protected] A. S. Shaharuddin · E. L. A. Yaji · N. S. A. Wahab · N. Razali · K. Y. T. Len Biomaterials Cluster, Food Technology Section, Universiti Kuala Lumpur Malaysian Institute of Chemical and Bioengineering Technology, Taboh Naning, 78000 Alor Gajah, Melaka, Malaysia e-mail: [email protected] E. L. A. Yaji e-mail: [email protected] N. S. A. Wahab e-mail: [email protected] N. Razali e-mail: [email protected] K. Y. T. Len e-mail: [email protected] J. Roslan School of Food Science and Nutrition, Universiti Malaysia Sabah, Jalan UMS, 88400 Kota Kinabalu, Sabah, Malaysia e-mail: [email protected] F. W. F. Wong Faculty of Biotechnology and Biomolecular Sciences, Universiti Putra Malaysia, 43400 Serdang, Selangor, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 83 A. Ismail et al. (eds.), Materials Innovations and Solutions in Science and Technology, Advanced Structured Materials 173, https://doi.org/10.1007/978-3-031-26636-2_8

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and the sustainability of the resources for mass production. The emerging alternative processes such as high hydrostatic pressure, microwave, ultrasound, sub- and supercritical fluids are selectively beneficial, albeit time-consuming and expensive. The diversity of the properties of bioactive peptides complicates the design of the appropriate purification steps, particularly for novel peptides. The integrative process by coupling the production and purification of bioactive peptides to a single integrative system can be a way forward for bioactive peptides production with high purity, potency, and cost-effectiveness. Thus, the review provides a comprehensive insight into the current status, trends, and challenges of bioactive peptide production through conventional and emerging processes. Meanwhile, the potential technological leap through integrative processes is also featured as the sustainability of the process must be assured. Keywords Bioactive Peptides · Functional Food · Bioprocessing Technology · Integrative process

8.1 Introduction Bioactive peptides are unique protein fragments that improve human and animal physiological functioning (Sánchez and Vázquez 2017). Antimicrobials, ACE inhibitors, antioxidants, endogenous opioids, and other bioactivities have been discovered in them (Mann et al. 2019; Toldrá et al. 2020). Bioactive peptides are favourable compared to traditional medications since they have minimal toxicity and few side effects in humans. Bioactive peptides from dairy, animal, and vegetable sources have been reported, and they comprise protein precursors with unique biological activity components (Mohanty et al. 2016). The production of bioactive peptides requires various steps due to the diverse functionalities of bioactive peptides. The batch technique is the most common way to create bioactive peptides. The batch hydrolysate, on the other hand, is often a complicated mixture of peptides. The efficacy of the bioactivity was lowered as a result. As a result, a high-efficiency separation method involving purification is necessary. A membrane-based and chromatographic method is commonly used for downstream processing, such as separating and purifying bioactive peptides from protein hydrolysates. Immobilized enzyme reactors, membrane reactors, enzyme membrane reactors, ultrafiltration electrolysis, and ion-exchange chromatography are among the purification technologies employed (Marciniak et al. 2018). To create peptides with the desired purity and activity, these procedures are used in tandem. It is, however, time-consuming and costly. As a result, low-cost, easy isolation with a small number of unit operations is required. Due to a lack of prior N. Saari Faculty of Food Science and Technology, Universiti Putra Malaysia, 43400 Serdang, Selangor, Malaysia e-mail: [email protected]

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information on the properties of bioactive peptides, it is difficult to develop good purification techniques, particularly in finding new peptides (Marciniak et al. 2018). Bitterness, limited peptide bioavailability, food-matrix peptide interactions, unconfirmed molecular mechanisms, and the sustainability of resources for mass manufacturing are some of the problems that must be overcome during the creation of the bioactive peptide. Therefore, this review gives an in-depth look at the potential technological leap via alternative processes, which is also important for long-term development sustainability.

8.2 Conventional Process and Its Drawbacks The transformation of bioactive peptide discoveries made in the laboratory into commercially available functional meals has proven challenging. Peptide bitterness, food-peptide interactions, poor peptide absorption and production, limited human research, a lack of understanding of molecular mechanisms, and protein supply sustainability are all factors that contribute to these difficulties (Li-Chan 2015). Considering this, commercially accessible bioactive peptides have demonstrated their viability and marketability. Pretreatment, hydrolysis, and then separation and purification are normally the three stages of the traditional method. A variety of upstream and downstream approaches must be explored to develop highly potent bioactive peptides. Chemical hydrolysis, enzymatic hydrolysis by proteolytic enzymes, or microbial fermentation by proteolytic bacteria can all be used to provide bioactive protein hydrolysates at first. Following that, bioactive peptides are purified, fractionated, and enriched using methods such as selective precipitation, ion-exchange, liquid chromatography, membrane filtration, gel filtration, ultrafiltration, or a combination of these methods (Agyei and Danquah 2011). The most common way of producing bioactive peptides is enzymatic hydrolysis, which is a batch process (Fig. 8.1). Any bioprocessing facility can use the batch method because it is straightforward to implement. To ensure optimum temperature control and heat distribution, most batch reactors are double jacketed and fitted with a stirrer. However, because consecutive peptide hydrolysis of the parent protein molecule can occur, protease-hydrolyzed protein is generally a complex mixture. Sequential hydrolysis can continue until the bio-specificity of the enzymes, species with resistant peptide bonds, or the loss of enzyme activity causes the synthesis of peptides with their primary sequence varying from the bio-specificity of the enzymes. As a result, adopting a simple kinetic model to simulate protein hydrolysis of several sequential reactions is challenging.

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Fig. 8.1 Main barriers to the conventional processes of bioactive peptides production

8.3 Alternatives Process Emerging process technology can be defined as a comprehensive approach to enhancing process design and optimization while reducing costs. The most promising emerging technologies in the production process of bioactive peptides have been identified as high hydrostatic pressure (HHP), microwave, ultrasonic, sub- and supercritical fluids, and other technologies that aid in enzymatic hydrolysis.

8.3.1 High Hydrostatic Pressure HHP, also known as Pascalization or cold pasteurization, is based on Chatelier’s principle, which states that any phenomenon resulting in a reduction in volume is enhanced by pressure. The pressure transmission fluid is usually water, and the process can be used with or without heat. It is essentially a non-thermal technology and is often perceived as a cost-effective technology. Various studies addressed the significance of HHP technologies in protein denaturation and aggregation. HHP has been shown in some studies to improve the enzymatic hydrolysis of different protein resources such as plants, dairy, and meat. It can also boost the production of bioactive peptides from a variety of enzymes (Boukil et al. 2018; Guan et al. 2018; Homma et al. 1994). HHP treatment causes protein unfolding or denaturation by disrupting hydrophobic and electrostatic bonding of peptides but has no effect on covalent bonds (Rivalain et al. 2010; Mozhaev et al. 1994, 1996). Enzymatic hydrolysis of casein protein with HHP at 100 MPa increased

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the degree of hydrolysis and antioxidant characteristics compared to 200 MPa and atmospheric pressure, according to Bamdad et al. (2017). Several parameters, including pressure, holding period, protein supplies, and enzyme, influence the effectiveness of enzymatic hydrolysis and the bioactivity of antioxidant peptides. HHP’s operational parameters are determined by the availability of proteins, their nature, and the substrate and enzyme employed qualities. Because of the complexity of the reactions involved in pressurization and decompression, protein aggregation can arise, inhibiting hydrolysis. HHP’s energy usage is a significant consideration, especially given the financial consequences. The energy consumption is primarily determined by the compressibility of the pressure medium, the holding pressure, the filling efficiency of the vessel, and the scale of the apparatus. The optimization of HHP settings is crucial for reducing energy consumption and expenses. As a result, initiatives to cut operational expenses and energy usage are being developed, notably during the pressurization phase.

8.3.2 Microwave-Assisted Processing The movement and collision of charged ions through inter- and intra-molecular friction is responsible for extracting peptides utilizing microwave-assisted processing (Wang and Zhang 2017). Rapid heating and the disintegration of membranes and protein cell walls resulted as a result of this (Jin et al. 2019; Nguyen et al. 2016; Zhou et al. 2018). Microwave heating improves enzymatic proteolysis and improves hydrolysate characteristics while lowering hydrolysis time. Protein conformation is altered by microwave-assisted processing, which improves enzyme bond accessibility and susceptibility (Ketnawa and Liceaga 2017; Zhang et al. 2019). Several researchers have recognized microwave-assisted processing as a promising strategy for generating bioactive peptides (Zhang et al. 2019; Gohi et al. 2019). It has outstanding qualities (protein solubility, oil and water absorption capacity) and improved the enzymatic digestion of Australian rock lobster shells (Nguyen et al. 2016). Ketnawa and Liceaga (Ketnawa and Liceaga 2017) demonstrated the utilization of microwave-assisted processing of fish frame protein feed for 5 min at 800 W and 90 °C, followed by 2–10 min of enzymatic hydrolysis with Alcalase. The approach improves the degree of hydrolysis, protein solubility, and free radical scavenging activity of hydrolysate as compared to untreated hydrolysate.

8.3.3 Ultrasound Ultrasound processing is another emerging technology in producing bioactive peptides (Zou et al. 2016; Dong et al. 2017; Wen et al. 2019; Wu et al. 2018). High intensity (16–100 kHz, power 10–1000 W/cm2 ) and low intensity (100 kHz–1 MHz,

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power < 1 W/cm2 ) ultrasound technologies are typically used in the food industry (Wang and Zhang 2017). Yu et al. (2014) found that though the pepsin activity was increased, a-amylase and papain activity was suppressed under the same sonification conditions. According to the researchers, this was due to changes in the protein’s secondary and tertiary structures after hydrolysis. Ultrasound has been demonstrated to promote peptide release by increasing surface hydrophobicity, which increases ACE-inhibitory peptide synthesis (Huang et al. 2014). It also boosted enzyme activity by improving enzyme dispersion and reducing aggregation (Kadam et al. 2015). Ultrasound pretreatment of porcine cerebral protein followed by Alcalase digestion resulted in a greater quantity of peptides, according to Zou et al. (2016). Furthermore, pretreatment with porcine cerebral ultrasonography provided protein hydrolysate with a stronger scavenging effect on DPPH radicals (72%), ABTS radicals (73%), and hydroxyl radicals (73%). Several factors must be evaluated and addressed, even though the potential for ultrasound processing has been shown. Its efficacy may be influenced by protein availability, unit operations, enzyme types, and process circumstances. As Ozuna et al. (2015) pointed out, it is also critical to accurately characterize the ultrasound system’s acoustic field to quantify acoustic energy during hydrolysis.

8.3.4 Sub- and Supercritical Fluids For the production of bioactive peptides, sub- and supercritical fluids are alternative methods. Under subcritical and supercritical levels, the physical and chemical properties of water change with temperature and pressure. For example, in sub- and supercritical circumstances, water’s dielectric constant lowers, allowing it to interact with non-polar substances and lowering the binding force, allowing it to dissolve more easily (Ahmed and Chun 2018). Water or another solvent has good transport capabilities in a sub- and supercritical state and has thus proven to be a simple, cost-effective, and highly efficient approach (Ahmed and Chun 2018). It is also considered a green technique because it uses only water rather than toxic chemicals. To make adequate functional peptides, one needs the right circumstances, especially the right temperatures. The optimal conditions are typically different depending on the protein source. Animal resources, for example, require greater temperatures and longer reaction times than plants. Bioactive peptides have recently been produced using supercritical carbon dioxide (CO2 ). Several factors influenced the process since protein, peptides, and amino acids are extremely temperature-dependent. The extracted protein rose with temperature while the amino acids decreased, according to Lamoolphak et al. (2006). Protein can suffer some degradation when exposed to high temperatures. Denaturation, the formation of a disulphide bond between amino acids, the liberation of polypeptides and free amino acids, the Maillard browning reaction between amino acids and carbohydrates, and the direct destruction of amino acids by oxidation are all responsible for this.

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Overall, while new techniques have demonstrated their ability to produce bioactive peptides, there are still several challenges to overcome. Protein unfolding and oligomer dissociation, for example, were produced by high hydrostatic pressure (Garcia-Mora et al. 2015; Hoppe et al. 2013). Furthermore, the complicated denaturation of peptides produced by sub- and supercritical fluids rendered them inactive and useless (Chao et al. 2013; Leeb et al. 2011). Finally, hydration effects and the exposure of hydrophobic groups caused protein structures to be disturbed by ultrasonic (Uluko et al. 2014; Kangsanant et al. 2015).

8.3.5 Integrative Process The integrative process is a simultaneous and continuous process that combines the upstream and downstream processing to produce peptides with different bioactive properties. The use of the ion-exchange principle has gained much interest in peptides purification. Separation of highly valuable protein precursors through ion-exchange methods has replaced traditional approaches, i.e. acid precipitation, which causes denaturation and low purity (Konrad et al. 2000; Rojas et al. 2006). The mild nature of the ion-exchange process to the protein and peptides had laid the foundation for developing the process. The simplistic approach and its versatility would allow the integration of the ion-exchange in the upstream process. The approach by Paée et al. (2015) is based on the integration of the ionexchange process for the adsorption of specific protein precursors for ACE-inhibitory peptides. The adsorbed protein precursor to the ion-exchanger is hydrolyzed in situ, releasing the peptides. The approach has significant advantages such as high potency hydrolysate with no subsequent purification, protease stability during hydrolysis and cost-effectiveness since the process occurs within a single vessel. Furthermore, the hydrolysate produced less complex peptides, contributing to the higher potency than conventional methods, requiring subsequent purification steps. Welderufael and Jauregi (Welderufael and Jauregi 2010; Welderufael et al. 2012a) observed the specific hydrolysis towards caseinomacropeptide in the early hydrolysis period, suggesting caseinomacropeptide (CMP) adsorption along with βlactoglobulin. Removing the CMP fraction and the recommencement of the in situ hydrolysis allows the release of peptides derived from β-lactoglobulin. As a result, three potent ACE-inhibitory peptides were identified: Ile-Pro-Pro (IPP) and GlnAsp-Lys-Thr-Glu-Ile-Pro-Thr (QDKTEIPT) derived from CMP and Ile-Ile-Ala-Glu (IIAE) derived from β-lactoglobulin. The study was successful in obtaining less complex peptides due to simultaneous purification during the process. Furthermore, enzyme-product inhibition was reduced, resulting in significantly increased enzyme stability. Paée et al. (2015) observed some disadvantages of the integrative process when acid whey was used as feedstock. The authors reported that only 62% β-lactoglobulin adsorbed using acid whey compared to 90% β-lactoglobulin yield from sweet whey.

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The low adsorption of β-lactoglobulin was caused by the high ionic calcium concentration in acid whey versus sweet whey. This is quite common for the ion-exchange process when an attracting ion from the solution (continuous phase) could interfere with the protein adsorption to the resin. Instead, some of the proteins form complexes with ionic calcium leading to low adsorption of β-lactoglobulin. The β-lactoglobulin conversion was also affected by the ionic calcium of which the conversion was only 38%. ACE-inhibitory activity remained high, however, due to the release of similar ACE-inhibitory peptides from sweet whey (Welderufael and Jauregi 2010). Furthermore, Ozorio et al. (2019) deduced that several steps, including whey reception, membrane separation, hydrolysis, drying, and packing, must be considered to develop an economically feasible integrative process for whey protein-based products. The selectivity of the β-lactoglobulin obtained in this study matched that of pure β-lactoglobulin (Welderufael and Jauregi 2010). Similarly, Zhao et al. (2013) devised an integrative process for obtaining casein phosphopeptides (CPPs) from Alcalase casein hydrolysates that included continuous hydrolysis, separation by enzymatic membrane reactor (EMR) and enrichment by anion-exchange chromatography. The integrative process facilitated separating CPPs and non-phosphorylated peptides (CNPPs) due to the difference in charge, allowing these compounds to bind with the ion-exchange resin. The process aided in the conventional process that required different preparation and separation processes (types of enzymes, resin, and membrane) due to the diversity of the targeted peptides (different structures, molecular sizes, bioactivities). Furthermore, they concluded that the integrative process produced high yield and purity, but it is also easily scaled up.

8.4 Conclusion The establishment of a productive and cost-effective process must be emphasized in every process development. The development of alternative processes such as the integrative process allows specific protein precursor isolation for specific bioactive peptides of high potency. Most importantly, the process, i.e. adsorption, in situ hydrolysis, and peptides purification, occurs within a single reaction vessel. Following this advancement, the innovation opens the opportunity for more studies, especially to explore the application of different nature of protein feedstock, i.e. processing byproducts from the food industry. Furthermore, the idea can be adapted to currently available bioprocess technology of which it could be translated into various technological approaches. Still, it must be based on the fundamental understanding of the process. Then, each approach suggested can undergo feasibility studies, including its bioactivities and peptides sequence and the scalability of setup for large-scale production.

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Acknowledgements The Universiti Kuala Lumpur is thankful for the grant given to Dr. Khairul Faizal Paée by the Ministry of Education (MOE) under the Fundamental Research Grant Scheme (FRGS), FRGS/1/2018/STG05/UNIKL/02/8 and Short-Term Research Grant (STR17031) awarded by Universiti Kuala Lumpur, part of which enabled this review article to be prepared. We are grateful for the contribution of all researchers involved in this paper preparation

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Chapter 9

Mode II Debonding Characterization of Adhesively Bonded Aluminum Joints Muhammad Noor Hazwan, Siti Faizah Mad Asasaari, Wong King Jye, Mohd Nasir Tamin, Mohd Shahrom Ismail, Mohamad Shahrul Effendy Kosnan, Mohd Al Fatihhi Mohd Szali Januddi, Mohd Anuar Ismail, and Mahzan Johar Abstract Adhesive joints as versatile methods offer several advantages, including eliminating galvanic corrosion for metallic adherents and overall weight saving. This work’s goal is to establish a systematic methodology for determining the strain rate-dependent interface properties of adhesively bonded joints loaded in mode II. Double lap joints consisting of aluminum Al 6061-T6 bonded with polymer adhesive M. N. Hazwan Faculty of Engineering Science, Department of Civil and Construction Engineering, Curtin University Malaysia, 98009 Miri, Sarawak, Malaysia e-mail: [email protected] S. F. M. Asasaari · W. K. Jye · M. N. Tamin Faculty of Engineering, Department of Applied Mechanics and Design, School of Mechanical Engineering, Universiti Teknologi Malaysia, Skudai, Johor, Malaysia e-mail: [email protected] W. K. Jye e-mail: [email protected] M. N. Tamin e-mail: [email protected] M. S. Ismail Politeknik Sultan Salahuddin Abdul Aziz Shah, Persiaran Usahawan, 40150 Shah Alam, Selangor, Malaysia e-mail: [email protected] M. S. E. Kosnan · M. A. F. M. S. Januddi · M. A. Ismail · M. Johar (B) Advanced Facilities Engineering Technology Research Cluster (AFET), Plant Engineering Technology (PETech) Section, Malaysian Institute of Industrial Technology, Universiti Kuala Lumpur, 81750 Masai, Johor, Malaysia e-mail: [email protected] M. S. E. Kosnan e-mail: [email protected] M. A. F. M. S. Januddi e-mail: [email protected] M. A. Ismail e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 A. Ismail et al. (eds.), Materials Innovations and Solutions in Science and Technology, Advanced Structured Materials 173, https://doi.org/10.1007/978-3-031-26636-2_9

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were used to investigate the delamination failure process. The strain rate-dependent interface properties were determined based on hybrid experimental and computational approaches. Both experiments and finite element simulations were conducted at displacement rates of 5, 50, and 500 mm/min using an end-notch flexure specimen. The strain rate-dependent interface strength properties were verified based on the finite element simulation results. The experimental and simulated mode II load– displacement curves showed promising findings and correlation. Hence, establishing a validated methodology fulfills the industrial requirement of an accurate predictive model with a minimum number of testing and material property data. Keywords Adhesively bonded joints · Mode II fracture toughness · Cohesive zone model · Finite element simulation

9.1 Introduction The application of adhesively bonded joints has contributed significantly to joining components from simple to complex engineering constructions in many engineering applications. These include assembling small products and structural components such as composite laminates and honeycomb structures used in aircraft, and repairing damaged ones (Annamalai et al. 2020; Lai et al. 2017, 2020, 2021; Rahman et al. 2019). Adhesive technology will continue to expand due to its adaptability in different applications. During service, the adhesive joint will experience a complex loading resulting in a complex stress pattern consisting of tensile, shear, and mixed-mode stresses. Additionally, the loading rate and the deformation mechanism affect the mechanical properties of adhesive materials (Johar et al. 2020). As seen in Fig. 9.1a, the failure modes of adhesive joints vary from establishing the surface fracture of cohesive failure and end-up with adhesive failure. The mechanics of cohesive failure can be understood when the adhesive’s bond with the adherent is stronger than the adhesive cohesive force. When the adhesive and adherents separate, this is referred to as adhesive failure. The failure is caused by local variation in stiffness and strength generated by the adhesive and adherents differing material qualities and surface preparation. The behavior of adhesive joints under varying loads has been studied using numerical modeling. The multi-geometry component was used to study the nonlinearity behavior that necessitates three-dimensional analysis using a numerical model (da Silva et al. 2009a, b). Finite element modeling is widely used for solving geometries and nonlinear material behavior. Modeling adhesive joint failure is difficult due to the complex interaction of various parameters (He 2011). The critical modeling concerns accurately represent various influences in the model and fracture initiation and propagation behavior in adhesively bonded double lap joints. The model should account to capture the effect of the strain rate and how it influences the damage

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(a)

(b) Fig. 9.1 End-notch flexure (ENF) specimen a An example of an adhesive joint failure. b An adhesive fracture surface illustrates the failure process

behavior until a catastrophic failure occurs (Khosravani et al. 2019). Because it may be employed in complex geometries, cohesive zone modeling (CZM) is versatile in capturing the damage process or fracture behavior in adhesive joints (Katsivalis et al. 2020). Numerous researchers have used the CZM technique to simulate debonding due to initiation of damage followed by the propagation of interface cracking and catastrophic failure in adhesive joints (Delbariani-Nejad et al. 2019; Sadeghi et al. 2020; Tserpes et al. 2021). However, the CZM technique is used to assess interface damage solely. If the cohesive failure occurs, the CZM model with finite thickness may be utilized instead. This paper focuses on adhesive joint deformation and failure mechanisms at its interface plane, where the crack initiates and propagates. Figure 9.1b illustrates the adhesive joint specimens that failed under the mode II loading fracture approach. From the illustration depicted, the adhesive failure always occurs when it satisfies the following condition: The interface cracking is located somewhere between the adherent materials and the bulk of the adhesive layer. The failure processes will be simulated using the CZM with zero-thickness adhesive. Section 9.2 discusses the cohesive zone model formulation in simulating the fracture behavior of adhesively bound joints.

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9.2 Cohesive Zone Model The interface’s cohesive behavior can be explained by interface degradation in adhesive joints. The CZM model depicts the separation of the interface as a progressive damage initiation and propagation process (Dugdale 1960; Barenblatt 1962). Cohesive traction resists the separation of the mating surfaces before a crack front, which occurs across a prolonged crack tip region or cohesive zone. The model was developed in 1959 when Barenblatt (1962) used the term “CZM,” referring to the brittle interface fracture and separation.

9.2.1 Cohesive Zone Model Formulation In Fig. 9.2, the CZM formulation begins by describing the interface damage initiation when subjected to the combined loading consisting of tensile and shear monotonic loading. Each material point describes a bilinear softening law. The interface stresses increase linearly as loading satisfies the input stress value. The contact’s penalty stiffness represents the linear rate of stress evolution (k n , k s ). The following equation is the quadratic stress damage initiation criterion (Davila and Camanho 2001).  σ 2 33

N

+

 τ 2 13

S

+

 τ 2 23

S

≥1

(9.1)

The assigned Macaulay’s bracket symbol indicates no value in normal stress (in compression). They are in the position of orthogonal components to be intact with the adhesive interface plane. The letters N and S denote the component of tensile and shear strengths of the interface located at the adhesive joint structure. The debonding occurs at stress levels below the interface tensile or shear strength of the interface

Fig. 9.2 Mixed-mode loading traction-displacement fundamental law

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material. Subsequently, the amount of critical energy release rate will energize the following damage initiation, allowing damage propagation. As anticipated by Eq. 9.2, the critical contact material point is separated (Benzeggagh and Kenane 1996). 

G II + G III G T = G IC + (G IIC − G IC ) GT

η (9.2)

The amount of energy release rate was significant (GIC and GIIC ) and is calculated separately based on the experimental result of opening and shearing mode (mode I and mode II). Therefore, the exponent symbols indicate the presence of a mixedmode ratio averaging, which is obtained from plotting an exponential trend between modes I and II.

9.3 Materials and Methods 9.3.1 Three-Point Bending End-Notched Fracture Test (a) The Specimen Preparations The three-point bending end-notched fracture (ENF) test was used to assess the critical energy release rate of an adhesively bonded aluminum joint subjected to mode II debonding loading. The Al6061-T6 double lap joint aluminum specimen was fabricated using Araldite 2015 adhesive. First, the specimen is created by cutting aluminum plates of 3 mm into 25 × 200 mm dimensions. As shown in Fig. 9.3, the specimen’s half-span length, L, is 70 mm. Then, aluminum adherents were sandblasted with 100 µm abrasive silica particles. Next, the surface roughness was measured using a surface roughness surface measuring machine, MarSurf CD 140 series, yielding 5.26 µm of average roughness. Next, the aluminum adherents’ surface was cleaned with acetone before bonding. Next, a thin Teflon film 16 µm thick was inserted in the middle of the adhesive joints. Next, in the top half of the adhesive joints, a thin Teflon film 16 m thick was inserted with a0 = 50 mm long to create the initial crack inside the adhesive bonded joints. The bonded specimens were then subjected to a constant pressure of 2 MPa for 15 s. Then, the specimen was left to dry for two hours at 50 °C. Before the tests, the specimens were kept at room temperature for 24 h. (b) Three-Point Bending ENF Test A universal testing machine (Instron 5982) with a 5 kN load cell was used to perform the ENF test. The 10 mm diameter for loading and both supported rollers were used to avoid localized damage on the specimens’ tops. Under ambient conditions, tests were carried out at different crosshead speeds (5, 50, and 500 mm/min). The load–displacement response was measured and recorded continuously until the specimen failed in each test. At least three times, the test was conducted to ensure that it was repeatable and to obtain an average value.

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Fig. 9.3 Setup configuration of the test specimen

(c) Critical Energy Release Rate The load–displacement response curve was utilized to measure the mode II critical energy release rate, GIIC , for varied displacement rates. Equation (9.3) represents the formulation to calculate the critical energy release rate using the simple beam theory. G IIC =

9Pi a 2 δ   2b 1 4 L 3 + 3a 3

(9.3)

where Pi is the load initiation (N), δ is the load’s corresponding displacement (mm), b is the adherent aluminum width (mm), L is the span length of the respective adherent aluminum (mm), and a0 is the initial crack created by thin Teflon film (mm).

9.3.2 Finite Element Simulation The CZM approach describes the fracture characteristics of mode II debonding by incorporating strain rate responses into the model. The results of the simulation are presented in this paper. The developed geometry is depicted in Fig. 9.4. The adherents and bulk adhesive layer have been discretized into solid elements with 20 nodes. Next, the pre-crack section is discretized into a cohesive interface element with matching nodes with eight nodes and zero thickness. It is necessary to study the sensitivity of the mesh to ensure that the mesh size does not influence the calculated stresses. The rollers (loading and both supporting) are considered rigid in this scenario. Both support rollers rotate according to their respective axes (U RX = U RZ = 0) clockwise. The load was applied by setting the loading roller’s vertical (z-direction) displacement at a specific loading rate (ranging from 5 to 500 mm per minute). The properties of the adhesives and adherents used in the FE simulation are summarized in Table 9.1.

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Fig. 9.4 Discretized FE model of the ENF specimen

Table 9.1 Mechanical properties of adhesive (Campilho et al. 2012) and aluminum (Jogi et al. 2008)

Property

Araldite 2015 Al 6061T6

Young’s modulus, E (GPa)

1.85

69

Poisson’s ratio, υ

0.33

0.33

Yield strength, σ Y (MPa)

12.63

289

Tensile strength, σ f (MPa)

21.63

328

Curing temperature/ time (°C/min) 60/35 Glass transition temperature (°C)

67

– –

9.4 Results and Discussion 9.4.1 Interfacial Fracture Adhesive Joints Under Mode II Debonding Loading A rate-dependent force is applied to an adhesive joint, causing the distribution of loads and displacements near the tip of an interface edge fracture to become unstable, as shown in Fig. 9.5. The application of the highest or critical load and the displacement of the load signify the start of continuous fracture propagation. The crosshead is moving at 5 to 500 mm/min, and the maximum peak loads are around 1061.1, 1223.9, and 1288.6 N, respectively. As the crosshead speed rates applied increase, the load– displacement response curve shifts upward, indicating an increase in displacement. The decreasing load-bearing value also revealed that the interface adhesive started to crack propagating. Finally, it is worth noting that the displacement at rupture appears to decrease slightly as the loading rate increases. This indicates that adhesive joints are well adapted to sustain large loads and stiffen and toughen over various loading rates.

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Fig. 9.5 Load–displacement curves for ENF

Fig. 9.6 Effect of loading rate (mode II)

9.4.2 Loading Rate Effect on Adhesive Joint Strain Energy Release Rate Figure 9.6 illustrates mode II fracture toughness variation for adhesive joints when rates range from 5 to 500 mm/min. In the case of fracture energy (GIIC ), it is observed that the fracture energy decreases as the rate increases from 5 to 500 mm/min. Numerous publications have been written about the effect of strain rate. Machado et al., for example, examined the strain rate effect on the fracture toughness of modes I and II (Campilho et al. 2012; Jogi et al. 2008). The results reveal that when strain rates increase, mode fracture energy reduces. A similar pattern of specimen interlaminar fracture of composite materials was found (Machado et al. 2017a, b).

9.4.3 Extraction of CZM Parameters Through an Experimental-FE Approach It was discussed in depth in the section CZM’s main equation on calculating the required CZM parameters. Figure 9.6 depicts a representative load–displacement response for the mode II test performed on the ENF specimen. At first, it appears that

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Fig. 9.7 Identifying the interface damage load level

there is a linear reaction. Specifically, the point designated A represents a departure from linearity with a 5-percent slope reduction. Assuming this load level is reached, it is hypothesized that interface damage will begin to manifest itself when the interface is opened. Additionally, FE simulations of the test were performed assuming no damage condition. As a result of the simulations, the predicted load–displacement response is depicted in Fig. 9.7. At point A, the progressing shear stress anticipated by FE at the critical material point would have achieved the interface’s shear strength, S. As illustrated in Fig. 9.8, more significant shear stress is predictable in the specimen’s center (a). As a result, interface damage is projected to occur at these critical points when the shear stress approaches the interface shear strength of S = 29.45 MPa. The accompanying shear traction-relative displacement curve slope denotes the interface’s penalty stiffness, k s , as illustrated in Fig. 9.8b. As shown in Fig. 9.9, the strain rate for subsequent model parameter values is retrieved accordingly. The penalty stiffness, k s , and shear strength, S, increase with strain rate, while the strain energy release rate, GIIC , decreases. Table 9.2 summarizes the retrieved features of the mode II interface.

Fig. 9.8 Stress prediction b slope of shear traction relative to shear displacement

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Fig. 9.9 Derived parameters reveal the effect of strain rate on the bilinear shear tractiondisplacement softening law

Table 9.2 Summary of extracted CZM properties ks

(N/mm3 )

5 mm/min

50 mm/min

500 mm/min

7.0 ×

8.5 ×

1.0 × 106

105

105

S (MPa)

29.450

37.890

49.190

GIIC (N/mm2 )

2.587

1.952

1.690

9.4.4 FE Model Verification for CZM The same FE model discussed for ENF is used to verify interface properties’ data. Cohesive interfaces respond according to a bilinear traction–separation law. Figure 9.10 compares the mode II test case (5 and 500 mm/min). The high degree of agreement demonstrates the validity of the combined experimental-FE technique.

Fig. 9.10 Comparison of the adhesive joint specimen’s measured and anticipated load–displacement response under mode II loading a 5 mm/min b 500 mm/min

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Fig. 9.11 Internal state variable distributions for a 5 mm/min b 500 mm/min

In comparison, Fig. 9.11 depicts the internal state variation of damage characteristics for the adhesively bonded joint located at the critical material point on the interface plane. The load applied satisfied the stress value via Eq. (9.1) and trigged the damage initiation represented by damage index one, and the damage evolution process begins. In this case, the damage evolution process was energized by the critical energy release rate via Eq. (9.2). As represented by Fig. 9.11, it can be observed the response time is slower for the 5 mm/min than for the 500 mm/min displacement rate, respectively. According to the graph, damage initiation takes approximately 14.3 s to reach a damage index of 1, compared to 0.24 s for damage initiation at 500 mm/min. The shear stress versus time graph is also shown for the 5 mm/min and 500 mm/min shear rates. The corresponding shear stress (S 13 ) achieves its highest value in 14.3 s and then gradually drops to 46 s for 5 mm/min loading displacement. However, the maximum shear point approaches 0.24 s for a 500 mm/min displacement rate. These results indicate that the 500 mm/min rate is faster when computing the separation of a single material point in a shorter amount of time. These differences suggest that the simulation correctly predicted a case for a different loading rate when the rate effect of the interface attributes was included. Additionally, traction-free crack faces can imply a decrease in shear stress components, resulting in the stable interface crack propagation under the mode II loading scenario examined.

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(a) Normal stress

(b) Shear stress

Fig. 9.12 On the interface plane, the distribution of normal and shear stress components corresponding to 3.7 mm; 5 mm/min roller displacement

A shear stress component denotes the loading on the interface caused by mode II. As seen in Fig. 9.12, the applied loading roller displacement causes a significant stress distribution in the adhesive interface plane. A high shear stress gradient with a denoted value of −29.42 MPa to zero defines the stress at the crack tip.

9.5 Conclusion The failure mechanics of an adhesively bonded aluminum joint subjected to mode II loading were investigated experimentally and numerically. Results show that the significant effect of adhesive failure was dominant in the failure mode, governs the interphase fracture process, and occurs in stable crack propagation. In addition, the developed methodology successfully determined a set of data for strain rate-dependent properties. The interface fracture occurs due to continuous crack propagation in the direction of the loading displacement. A verified finite element simulation method based on the CZM was developed to evaluate an adhesive joint’s strain rate effect. Acknowledgements This research is part of an inter-university collaborative research program.

References Annamalai VE, Vijayan S, Saeedipour H, Goh KL (2020) The rise of short fibre reinforced plastics. Reinf Plast 64(2):97–102 Barenblatt GI (1962) The mathematical theory of equilibrium cracks in brittle fracture. Adv Appl Mech 7:55–129 Benzeggagh ML, Kenane MJ (1996) Measurement of mixed-mode delamination fracture toughness of unidirectional glass/epoxy composites with mixed-mode bending apparatus. Compos Sci Technol 56(4):439–449 Campilho RD, Banea MD, Neto JA et al (2012) Modelling of single-lap joints using cohesive zone models: effect of the cohesive parameters on the output of the simulations. J Adhes 88(4–6):513– 533

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da Silva LF, das Neves PJ, Adams RD et al (2009a) Analytical models of adhesively bonded joints—part I: literature survey. Int J Adhes Adhes 29(3):319–330 da Silva LF, das Neves PJ, Adams RD et al (2009b) Analytical models of adhesively bonded joints—part II: comparative study. Int J Adhes Adhes 29(3):331–341 Davila CG, Camanho PP (2001) Decohesion elements using two and three-parameter mixed-mode criteria. In: American helicopter society conference Delbariani-Nejad A, Malakouti M, Farrokhabadi A (2019) Reliability analysis of metal-composite adhesive joints under debonding modes I, II, and I/II using the results of experimental and FEM analyses. Fatigue Fract Eng M 42(12):2644–2662 Dugdale DS (1960) Yielding of steel sheets containing slits. J Mech Phys Solids 8(2):100–104 He X (2011) A review of finite element analysis of adhesively bonded joints. Int J Adhes Adhes 31(4):248–264 Jogi BF, Brahmankar PK, Nanda VS et al (2008) Some studies on fatigue crack growth rate of aluminum alloy 6061. J Mater Process Tech 201(1–3):380–384 Johar M, Wong KJ, Rashidi SA et al (2020) Effect of strain-rate and moisture content on the mechanical properties of adhesively bonded joints. J Mech Sci Tech 34(5):1837–1845 Katsivalis I, Thomsen OT, Feih S et al (2020) Development of cohesive zone models for the prediction of damage and failure of glass/steel adhesive joints. Int J Adhes Adhes 97:102479 Khosravani MR, Anders D, Weinberg K (2019) Influence of strain rate on fracture behavior of sandwich composite T-joints. Eur J Mech A-Solid 78:103821 Lai WL, Cheah AY, Ruiz RC et al (2017) A simple portable low-pressure healant-injection device for repairing damaged composite laminates. Int J Mech Eng Educ 45(4):360–375 Lai WL, Saeedipour H, Goh KL (2020) Mechanical properties of low-velocity impact damaged carbon fibre reinforced polymer laminates: effects of drilling holes for resin-injection repair. Compos Struct 235:111806 Lai WL, Saeedipour H, Goh KL (2021) Experimental assessment of drilling-induced damage in impacted composite laminates for resin-injection repair: Influence of open/blind hole-hole interaction and orientation. Compos Struct 271:114153 Machado JJ, Marques EA, Campilho RD et al (2017a) Mode I fracture toughness of CFRP as a function of temperature and strain rate. J Compos Mater 51(23):3315–3326 Machado JJ, Marques EA, Campilho RD et al (2017b) Mode II fracture toughness of CFRP as a function of temperature and strain rate. Compos B Eng 114:311–318 Rahman MAASB, Lai WL, Saeedipour H, Goh KL (2019) Cost-effective and efficient resininjection device for repairing damaged composites. Reinf Plast 63(3):156–160 Sadeghi MZ, Gabener A, Zimmermann J et al (2020) Failure load prediction of adhesively bonded single lap joints by using various FEM techniques. Int J Adhes Adhes 97:102493 Tserpes K, Barroso-Caro A, Carraro PA et al (2021) A review on failure theories and simulation models for adhesive joints. J Adhes 1–61 Yasaee M, Mohamed G, Pellegrino A et al (2017) Strain rate dependence of mode II delamination resistance in through thickness reinforced laminated composites. Int J Impact Eng 107:1–11 You H, Yum YJ (1997) Loading rate effect on mode I interlaminar fracture of carbon/epoxy composite. J Reinf Plast Compos 16(6):537–549

Chapter 10

Design Optimization of Shell and Tube Heat Exchangers: Effect of Baffles Design Siti Noor Zaerah Zazoly, Munir Faraj Mabrouk Alkbir, Adnan Bakri, Mahzan Johar, Shahrulzaman Shaharuddin, Mohamad Shahrul Effendy Kosnan, Ardiansyah Syahrom, and Mohd Al Fatihhi Mohd Szali Januddi Abstract All industrial applications use a heat exchanger as a device for transferring heat in both cooling and heating processes. Heat exchangers can be divided into several types but the present study focuses on shell and tube heat exchangers (STHX). Nowadays, the STHX type is preferable due to its capacity to transfer heat in a large amount. The present study aims for optimum design parameter identification for the baffles of STHX. The STHX with newly designed baffle was analyzed for its performance in terms of the rate of pressure drop and the heat transfer coefficient of STHX.

S. N. Z. Zazoly Nexus-Venture Holding Limited, Federal Territory of Kuala Lumpur, Kuala Lumpur, Malaysia e-mail: [email protected] M. F. M. Alkbir · A. Bakri · M. Johar · S. Shaharuddin · M. S. E. Kosnan · M. A. F. M. S. Januddi (B) Advanced Facilities Engineering Technology Research Cluster (AFET), Plant Engineering Technology (PETech) Section, Malaysian Institute of Industrial Technology, Universiti Kuala Lumpur, Pasir Gudang, Malaysia e-mail: [email protected] M. F. M. Alkbir e-mail: [email protected] A. Bakri e-mail: [email protected] M. Johar e-mail: [email protected] S. Shaharuddin e-mail: [email protected] M. S. E. Kosnan e-mail: [email protected] A. Syahrom Medical Devices and Technology Centre (MEDiTEC), Universiti Teknologi Malaysia, Johor Bahru, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 A. Ismail et al. (eds.), Materials Innovations and Solutions in Science and Technology, Advanced Structured Materials 173, https://doi.org/10.1007/978-3-031-26636-2_10

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Keywords Shell and tube heat exchanger · STHX · Heat transfer · Fluid flow · Heat transfer coefficient · Baffle design

10.1 Introduction Generally, a heat exchanger transfers heat from solid to fluid, or in between fluids (Meilinger and Torok 2013). The transfer of heat ensures the fluid flowing is at the right temperature and at the pressure suitable for the next process. Condensed vapors and evaporated liquids are the resultant products from heat exchangers (Ibrahim 2012; Abhishek Arya 2015; Melissa 2021; Shukla et al. 2015). The performance of a heat exchanger is governed by the cost, productivity and the quality of the energy produced. These factors are influenced by the design of the baffle in the heat exchanger (Ikenna and Chinenye 2018; Wenjing et al. 2014; Akii et al. 2009; Factors and in Heat Exchanger. HRS 2016; Fakheri 2014). Shell and tube heat exchangers (STHX) are the common heat exchangers used in most industries (Govindaraj et al. 2018) due to their capacity to transfer large amount of heat. Josef et al. (Anoop and Ravindra 2017) recognized the design of the baffle is one of the most important parameters to be considered for heat exchanger optimization in order to ensure better performance. Further, the profitability of the process is highly depended on the operating parameter of the heat exchanger, in which this factor is influenced by the input and output temperature. Shape and patterns on baffles also play an important role in the heat transfer coefficient, pressure drop rate, velocity and the log mean temperature of shell and tube heat exchangers (STHX) (Factors and in Heat Exchanger. HRS. 2016). Baffles with helical pattern have been found to produce smooth flow of fluid in the heat exchanger (Govindaraj et al. 2018). This gives the heat exchanger its ability to prevent flow-induced vibration. Baffles also allow the change in the direction of fluid flow, enhancing turbulent and avoiding plug flow in STHX (Ikenna and Chinenye 2018). The more baffles incorporated in the heat exchanger, the more efficient it becomes. In the present work, the shell-side pressure drop and the heat transfer coefficient was analyzed mathematically using the Kern method. It was aimed to identify the optimum design for high performance STHX.

10.2 Methodology 10.2.1 Design Development Design work of the baffles was done using SolidWorks (Dassault Systèmes, USA). Two types of baffle were designed for the STHX. The preliminary design of the baffles is shown in Fig. 10.1. Two designs were constructed; the standard design

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Fig. 10.1 Design of heat exchanger–segmental (a) and helical baffles (b)

(design A) and the continuous helical pattern (design B). Figure 10.2 shows the 3-dimensional design of the heat exchanger used in computational flow analysis.

10.2.2 Fluid Flow Analysis Fluid flow analysis was done using COMSOL Multiphysics (COMSOL Inc., Sweden). Specific measurement for the STHX designed in this study is tabulated in Table 10.1. Turbulent flow of water was numerically simulated on the designed STHX at different Reynolds numbers.

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Fig. 10.2 Design in 3-dimensional for flow analysis

Table 10.1 Geometrical parameters of a heat exchanger No.

Description

Unit

Value

1

Heat exchanger length, L

Meter

0.600

2

Shell inner diameter, Di

Meter

0.092

3

Shell outer diameter, Do

Meter

0.090

4

Tube length, l

Meter

0.500

5

Tube inner diameter, d i

Meter

0.019

6

Tube outer diameter, d o

Meter

0.020

7

Number of tubes, N t

–

7

8

Tube pitch triangular, Pt

Meter

0.30

9

Baffle spacing, B

Meter

0.025

10

Side plate diameter, Dsp

Meter

0.090

11

Baffle thickness ΔRT

Meter

0.001

10.2.3 Mathematical Analysis 10.2.3.1

Thermal Analysis of Segmental Baffles Heat Exchange

Kern method was used in the present study to do the thermal analysis on the STHX to determine its performance. The pressure drop and heat transfer coefficient in the tube and shell side was determined by using the equation as stated in the Sect. 10.2.3.2.

10 Design Optimization of Shell and Tube Heat Exchangers: Effect …

10.2.3.2

113

Thermal Analysis of Helical Baffles Heat Exchanger

The thermal analysis was also conducted on the STHX with helical heat exchanger. Results were then compared to determine which STHX design gives out optimum performance. Tube clearance, C = Pt − Dot

(10.1)

Baffle spacing, L b = π × Dis × Tan ∅

(10.2)

Cross-flow area, As = (Dis × C × B)/Pt

(10.3)

Equivalent diameter, DE = 4

[(

Pt ×

√ 2

) ( π )] /[π × do /2] 3/4 − do2 × 8

Maximum velocity, Vmax =

Qs As

Reynolds’ number, Re = ρ × Vmax ×

(10.4) (10.5)

DE μS

(10.6) 1

0.36 × K s × Re0.55 × Pr 3 Heat transfer coefficient, h s = DE

(10.7)

Number of baffles, Nb = L s (L b + ΔBT)

(10.8)

[ Pressure drop, Δps =

] f s × G 2s (Nb + 1)DS × DE × ϕs 2ρs

Losses, f = exp(0.576 − 0.19 ln Re) where 400 < Re =

(10.9)

G s Ds ≤ 1 × 106 μ (10.10)

where L is the heat exchanger length, Di is the shell inner diameter, Do is the shell outer diameter, l is the tube length, di is the tube inner diameter, do is the tube outer diameter, f s is entrance and exit losses, Nt is the number of tubes, Pt is the tube pitch triangular, ∅ is the tube and baffle angle, Q s is the flow rate, B is the baffle spacing, Dsp is the side plate diameter, μs is viscosity and ΔBT is the baffle thickness.

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Fig. 10.3 Heat transfer coefficient versus baffles design

10.3 Results and Discussion The geometry and differences in design of the baffle in STHX were studied computationally in the present work. Figure 10.3 shows that a higher heat transfer coefficient is recorded for STHX with helical pattern baffle in comparison to STHX with segmental pattern baffle (Dipankar et al. 2017). Differences were found to be 24%, which demonstrate the better performance in the STHX with helical baffle. Less number of baffle means less complicated maintenance work for the STHX as better efficiency can be achieved easily. Youcef and Saim (2022) found that the fluid velocity of the STHX affected the number of swirl zones, which eventually affected the heat transfer coefficient directly (Chang and Tinker 1969). Noticeable variance in pressure drop at 68% difference was also recorded in between the STHX with different baffle design (Fig. 10.4). Helical pattern baffles exhibit smooth fluid flow without sudden stop. Furthermore, STHX with helical baffles has decreased in flow turbulence thus the pressure drop was lower than that of STHX with segmental baffles. Efficient heat transfers and pressure drop was recorded on the STHX with helical baffle at 30° angle (Figs. 10.5 and 10.6). Table 10.2 shows the fluid properties for both shell and tube sides.

10.4 Conclusion The efficiency of STHX is highly dependent on the baffle’s parameters such as design, pattern and geometry. This study focused on the STHX with two types of baffles, which were computationally analyzed in terms of the heat transfer performance and the pressure drop. For improved performance, it was found that helical baffles are the best optimization that can be done and implemented into STHX. Furthermore, the optimal angle of the baffles was at 30°. However, further analysis can be done in order to see other performance factors that can be influenced by the helical baffles.

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Fig. 10.4 Pressure drop versus different baffles design

Fig. 10.5 Heat transfer coefficient versus angle of helix for helical designed baffles

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Fig. 10.6 Pressure drop value versus angle of helix for helical designed baffles

Table 10.2 Fluid properties

Fluid flow

Temperature (K)

Density (kg/m3 )

Thermal conductivity (W/mk)

Shell side

298

998

0.6129

Tube side

353

974

0.6687

Acknowledgements Authors thank to facilities provided by Universiti Kuala Lumpur Malaysian Institute of Industrial Technology (UniKL MITEC) especially for Plant Engineering Technology (PETech) Section.

References Abhishek Arya1 DS (2015) Optimization of shell and tube heat exchanger. Int J Adv Sci 27–35 Akii OAI, Igbafe AI, Anyata BU (2009) The effect of baffles in shell and tube heat exchangers. Adv Mat Res 62(64):694–699 Anoop K, Ravindra M (2017) Comparative analysis of heat exchanger for different materials. Int J Eng Technol 3(2) Chang DRC, Tinker EB (1969) The effect of baffle spacing on the dynamics of shell and tube heat exchangers. Can J Chem Eng 47(4):336–338 Dipankar D, Tarun KP, Santanu B (2017) Helical baffle design in shell and tube type heat exchanger with CFD analysis. Int J Heat Technol 35(2):378–383 Fakheri A (2014) Efficiency analysis of heat exchangers and heat exchanger networks. Int J Heat Mass Transf 76:99–104 Fouling Factors in Heat Exchanger (2016) HRS. https://www.hrs-heatexchangers.com/resource/fou ling-factors-heat-exchangers. Accessed 26 Jul 2022

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Govindaraj K, Ravichandran S, Ponnukutti D, Ramar V, Nathamani SK (2018) Numerical analysis of baffle cut on shell side heat. Heat Transf Eng 39(13–14):1156–1165 Ibrahim HA (2012) Fouling in heat exchangers. In: MATLAB-A fundamental tool for scientific computing and engineering applications, vol 3. Intech Open, UK, pp 57–93 Ikenna N, Chinenye AI (2018) Design of shell and tube heat exchanger with double passes. J Eng Res Reports 3(4):1–12 Meilinger A, Torok I (2013) The importance of friction stir welding tool. Prod Process Syst 6(1):25– 34 Melissa F (2021) Fouling in heat exchangers. Central States Industrial Equipment (CSI). https:// www.csidesigns.com/blog/articles/fouling-in-heat-exchangers. Accessed 26 Jul 2022 Shukla A, Kumar P, Tiwari DD (2015) Design procedure of shell and tube heat exchanger. Int J Eng Res 3(12):116–120 Wenjing DU, Hongfu W, Lin C (2014) Effects of shape and quantity of helical baffle on the shell-side heat transfer and flow performance of heat exchangers. Chin J Chem Eng 22(3):243–251 Youcef A, Saim R, Kourti MC, Benhamou M (2022) Numerical analysis termal fluid in a heat exchanger with baffles inclination. J Renew Energies 21:237–44

Chapter 11

The Performance of Palm Broom as Eco-friendly Paper Mohamad Sazali Said, Muhammad Iqbal Adnan, Mohamad Alif Akmal Mohd Khairi, Muhammad Izzat Kamarudin, Muhamad Salihin Abd Razak, and Mohd Shahrizan Yusoff Abstract These days, trends show that people are becoming interested in using eco-friendly products. Many people start to realize and take concern about safety of families and the planet. Therefore, this project will create an environmentally friendly paper and show the performance of this paper. In Malaysia, the waste from agriculture is becoming enormous especially from oil palm plantation. The wastes have increased by more than threefold yet the remaining of this waste material can make environmental issues. Oil palm fronds, which are made up of leaflets and petioles, are one of the most common waste products in Malaysia’s oil palm plantations. Oil palm fronds are available every day of the year when the palms are trimmed during the harvesting of fresh fruit bunches for oil production. Therefore, this unuseful waste that become a major problem to handle will be transformed into a paper. At the beginning, a study about the effect of oil palm waste on the environment has been measured. Based on the confirmation, the oil palm brooms were selected in the process making of the paper. Oil palm brooms are from oil palm leaflets waste. The production of paper starts with the brooms which, will be crushed into pulp after being combined with water. After that, the pulp will be dried to make the paper. The paper will next be subjected to the Cobb test to identify the water absorbency of the M. S. Said (B) · M. I. Adnan · M. A. A. M. Khairi · M. I. Kamarudin · M. S. A. Razak · M. S. Yusoff Manufacturing Section, Universiti Kuala Lumpur Malaysian Spanish Institute, Kulim Hi-Tech Park, 09000 Kulim Kedah, Malaysia e-mail: [email protected] M. I. Adnan e-mail: [email protected] M. A. A. M. Khairi e-mail: [email protected] M. I. Kamarudin e-mail: [email protected] M. S. A. Razak e-mail: [email protected] M. S. Yusoff e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 A. Ismail et al. (eds.), Materials Innovations and Solutions in Science and Technology, Advanced Structured Materials 173, https://doi.org/10.1007/978-3-031-26636-2_11

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material. Based on testing process, the material shows a positive reaction for water absorption. The average rate of absorption is below 2%. This data show that the material did not absorb water strongly. Furthermore, this paper with more oil palm broom compared to the starch shows the lowest rate of absorption. In conclusion, the waste of oil palm frond can be controlled yet adding its value into eco-friendly products. Besides, this material is fully renewable. Therefore, people can use this product in the future in order to preserve nature for our safety and health. Keywords Eco-friendly paper · Oil palm waste · Cobb test

11.1 Introduction Paper is a one of materials that can be turned into eco-friendly alternative products for packaging. It has also become a fundamental part of most aspects of society. Each day, approximately 300 million metric tons of paper are produced worldwide, with approximately 90% of this paper produced from mature pulp wood. It is used to make carry bags, sachets, books, and many other items. Paper production consumes a significant portion of the world’s commercially cut timber. Over one million tons of paper were produced in Malaysia in 2005 (Jean and Roda 2006). The life cycle of paper is harmful to the environment. It starts with a tree being cut down and ends with the tree being burned, releasing carbon dioxide into the atmosphere (Sheth et al. 2014). Most of the paper manufacturing processes involve using pulp made from timber. Other environmentally conscious techniques include producing recycled paper (Fahmy et al. 2017), producing paper from agricultural waste like banana fibers cotton stalks, wheat, and rice residues, etc. (Fahmy et al. 2017). Paper can be made from any raw material that can be shaped into a continuous sheet. The properties of paper pulp and the papers that follow are directly affected by the fiber qualities. The processing they undergo has a significant impact on their morphology and strength; in general, most of the lignin must be removed to produce the best pulp. The most common reasons for selecting one fiber over another are length, diameter, and thickness of its wall, lumen size, flexibility, and rigidity. The first factor used to evaluate good pulp is the relationship between the length of the diameter of the fiber and the thickness of its wall. According to Wan et al. (2009) production of pulp from oil palm fronds has been demonstrated for papermaking. As a result, in order to maximize the use of the abundant biomass generated by Malaysia’s palm oil industry, this study was carried out with the goal of investigating the papermaking potential of this industrial byproduct. Oil palm leaves were used in this study because they are thought to be a potential non-wood lignocellulosic compound for paper production because they contain 43.8% cellulose, which is within the acceptable range of wood fiber (40– 45%). Meanwhile, the lignin content of oil palm leaves has been reported to be

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around 19%, which is in the low range of those found in wood resources (18–25%). As a result, these compositions found in oil palm leaves are thought to be suitable for paper manufacturing. In Malaysia, agricultural waste particularly from oil palm plantations, is becoming massive. This large volume of waste can cause environmental issues. With an annual production capacity of approximately 58 million tons in 2011, oil palm fronds are the most abundant type of oil palm waste. This amount is expected to reach 110 million tons in Malaysia alone by 2020 (Che et al. 2014). The oil palm frond is 2–3 m long and weighs about 10 km (wet weight). It consists of the petiole (the stem) and many long leaflets on either side of the stem. Currently, OPF is either burned or left to decompose in the natural environment. These activities are wreaking havoc on the ecosystem, necessitating the development of new methods for utilizing this abundant resource. The current project aims to make biodegradable paper out of oil palm fronds. Based on the confirmation research, the oil palm brooms were used in the papermaking process. This would aid in the preservation of the environment by preventing deforestation and improper management of oil palm waste. The brooms will be crushed into pulp after being combined with water. After that, the pulp will be dried to make paper. The paper will then undergo physical testing, i.e., the Cobb test to determine the water absorbed into the biocomposite.

11.2 Methodology The oil palm fronds that have been collected will be chopped into smaller pieces of about 3 cm. The OPF will be dried in a forced-air drying oven to remove the moisture content. Following that, the dry OPF will be ground into powder. The powder will then be sieved through smaller mesh sizes. Following that, the powder will be mixed with corn starch. The composite will be cured for 24 h. After the composites have been fixed, they will be demolded. The broom that has been collected will be cut into small pieces. All uniformly cut parts are then soaked in a mixture of water and baking soda. Furthermore, baking soda aids in the preservation of water’s alkalinity. After soaking, all of the soaked matter is boiled for 2 h to make it easier to blend the materials into a smooth and fine pulp. In this project, dyeing is used rather than bleaching. After boiling, the residuals are dyed to color the paper. Binder is created concurrently (Solsi and Mohammad 2020). The Binder is just as important as residual sources because it holds fibers together and gives the paper the necessary strength. Corn flour is used because it is a starch that gives paper its stickiness and acts as a suitable natural binder. Then, all the dyed materials, along with the prepared binder and warm water, are blended with the blender by following predefined percentage. After blending, the pulp which is obtained undergoes beating to obtain uniformity and consistency in the pulp. The pulp is spread on paper, making the frame the same size as the frame while removing excess water.

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The pulp is then transferred to a paper towel for drying. Pressing is used for the paper to speed up the drying process. An electric iron is used to press the paper between the layer of the paper towel to obtain flat and straight paper. The paper is left for 24 h to ensure that it is completely dried. After that, the paper will undergo mechanical testing, which is a Cobb test to check the absorbency results. The collected data will be evaluated to determine which is the best performance of paper according to factors that are already set up in the Taguchi method.

11.2.1 Mechanical Testing The Cobb test measures the amount of water absorbed into the surface by a sized paper, paperboard, and corrugated fiberboard paper or paperboard sample in a given time period. The absorbency of water is measured in grams per square meter (g/m2 ). In our project, we use 30, 60, and 90 s. A material’s water absorbency can have a significant impact on printability and the setting rate of water-based adhesives. For the Cobb test, the samples were cut into a square shape and it was done in accordance with ASTM D5802.

11.3 Results and Discussion For applying the Taguchi method, the Minitab software is used in this experiment. The Minitab software is used to develop an orthogonal array design matrix. Two factors that are conducted for this experiment and three levels to be tested for each factor (Table 11.1). The papers were measured using the absorbency test of three sample with different weight percentage of oil palm broom (OPB) which is 50, 55, and 60%. The different amount of binder which is corn starch also were measured in 40, 45, and 50%. The Table 11.1 Orthogonal array matrix design

Sample

Weight of OPB (%)

Time taken for absorbency (s)

1

60

30

2

60

60

3

60

90

4

55

30

5

55

60

6

55

90

7

50

30

8

50

60

9

50

90

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Table 11.2 Paper sample with 60% weight of oil palm broom (OPB) and 40% weight of starch Sample

Time taken (s)

Before

After

Weight (g)

Weight (g)

Rate of absorption

1

30

4

14

0.53

2

60

10

16

0.6

3

90

13

20

1.8

Table 11.3 Paper sample with 55% weight of oil palm broom (OPB) and 45% weight of starch Sample

Time taken (s)

Before

After

Weight (g)

Weight (g)

Rate of absorption

4

30

14

28

1.00

5

60

14

31

1.21

6

90

13

35

1.69

Table 11.4 Paper sample with 50% weight of oil palm broom (OPB) and 50% weight of starch Sample

Time taken (s)

Before

After

Weight (g)

Weight (g)

Rate of absorption

7

30

12

27

1.25

8

60

12

30

1.50

9

90

14

34

1.42

time taken for each paper sample also were measured with different period in 30, 60, and 90s. Hence, the result average rate of absorption for various sample are presented in Tables 11.2, 11.3 and 11.4. The average rate of absorption for Table 11.2 is 0.97 which is very low. The highest being 1.39 were obtained from Table 11.3. The results of performance of oil palm broom are presented in Figs. 11.1 and 11.2. From the Fig. 11.1, sample 3 with 60% weight of oil palm broom measured within 90 s shows the highest which is 1.80. The lowest being sample 1 with 60% weight of oil palm broom measured within 30 s that obtained only 0.53. From the Fig. 11.2, sample with 50% weight of oil palm broom shows the highest result which is 1.39. The lowest being sample with 60% weight of oil palm broom which is 0.97 (Figs. 11.3 and 11.4). By using the delta and rank value, the variables which have the largest influence on each respond attribute can be determined. This also can determine which level of those variables match with the objective. The ideal factor level for one response characteristic may differ from the optimal level for another response characteristic. To solve this problem, it can be good to predict the result of various possible combinations of component values to see which one produces the best result. The optimization rate absorption of paper eco-friendly by signal-to-noise ratios from weight percentage is 50% and time taken for absorption is 90 s.

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Fig. 11.1 Performance of paper eco-friendly by samples

Fig. 11.2 Performance of paper eco-friendly by weight of OPB

Fig. 11.3 Main effects plot for SN ratios

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Fig. 11.4 Main effects plot for means

11.4 Conclusion In this study, the effect of water absorbency were studied by performing the Cobb test on the composite. From the study, it was concluded that the more amount of oil palm broom compared to starch gives less ability to absorb water. The average rate of 60% of oil palm broom is 0.97 while for 40% of palm broom is 1.39. After comparison between the 3 ratios used, it is concluded that the average rate of absorption is below 2%. This data show that the material did not absorb water strongly. Besides, this composite has a future in preserving nature for our safety and health. Acknowledgements The work is ostensibly supported the Dana Penyelidikan & Inovasi MARA (DPIM) 2021, MARA 600-6/4/3 Project.

References Che MCMH, Ariffin H, Hassan MA, Shah UKM, Shirai Y (2014) Oil palm frond juice as future fermentation substrate: a feasibility study. Biomed Res Int 48:92–99 Fahmy Y, Fahmy T, Mobarak F, El-Sakhawy M, Fadl M (2017) Agricultural residues (wastes) for manufacture of paper, board, and miscellaneous products: background overview and future prospects. Int J Chemtech Res 10(2):424–448 Jean M, Roda SR (2006) Feeding China’s expending demand for wood pulp: a diagnostic assessment of plantation development, fiber supply, and impacts on natural forests in China and in the South East Asia region. Malaysia Report, Malaysia: Ffeeding China’s expanding demand for wood pulp, pp 1–28

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Sheth TR, Gokhe AA, Kumar PN, Shridhar K (2014) Recycling flower and kitchen waste to make biodegradable paper. Environ J 10(1):35–38 Soloi S, Mohammad AA (2020) Characterization of oil palm leaf paper with starch as binder. myJAFE 41:1–8 Wan RWD, Mazlan I, Law KN (2009) Effects of kraft pulping variables on pulp and paper properties of Acacia mangium kraft pulp. Cellul Chem Technol 43(1–3):9–15

Chapter 12

Mechanical and Thermal Properties of Polylactic Acid Composites Filled with Iron Particles Muhammad Remanul Islam, Mohd Al-Fatihhi Mohd Szali Januddi, Mohd Haziq Zakaria, Sairul Izwan Safie, Ahmad Naim Ahamd Yahaya, Md Golam Sumdani, and Amin Firouzi Abstract An additive manufacturing process was used to fabricate different samples using polylactic acid and iron particle filament. Different processing parameters like temperature were used to produce different samples. The samples were tested for the mechanical and thermal testing using tensile, flexural, structural and thermogravimetric and differential scanning calorimetry, respectively. Results showed that the composites showed a lower trend of mechanical properties compared to the neat polylactic acid. It was also noticed that the parameters had minimal effects on the thermal properties of the composites. The structural changes were also noticed minimal. Keywords Additive manufacturing · PLA/Iron · Filament · Mechanical · Thermal M. R. Islam (B) · M. A.-F. M. S. Januddi · S. I. Safie Plant Engineering Technology, Malaysian Institute of Industrial Technology, Universiti Kuala Lumpur, Persinaran Seri Alam, 81750 Pasir Gudang, Johor Bahru, Malaysia e-mail: [email protected] M. A.-F. M. S. Januddi e-mail: [email protected] S. I. Safie e-mail: [email protected] M. H. Zakaria Quality Engineering Technology, Malaysian Institute of Industrial Technology, Persinaran Seri Alam, 81750 Pasir Gudang, Johor Bahru, Malaysia e-mail: [email protected] A. N. A. Yahaya Institute of Post Graduate Studies, Universiti Kuala Lumpur, Kuala Lumpur, Malaysia e-mail: [email protected] M. G. Sumdani South Dakota Mines, Rapid City, SD, USA e-mail: [email protected] A. Firouzi Nanomaterials and Processes, GE Appliances, Louisville, KY, USA e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 A. Ismail et al. (eds.), Materials Innovations and Solutions in Science and Technology, Advanced Structured Materials 173, https://doi.org/10.1007/978-3-031-26636-2_12

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12.1 Introduction There is a growing interest of using bio-based and renewable materials for the buildings, infrastructures and composites in place of traditional petroleum-based polymer matrices. Among some new materials, polymers from bio-based raw materials, for example, polyalkyds, polylactic acid, lignin-based polymers, cellulose, etc. are mentionable. These materials are renewable, environmentally friendly and biodegradable, and show higher stiffness and strength (Hornsby et al. 1997; Heijenrath and Peijs 1996; Sanadi et al. 1994; Bledzki et al. 1996). Polylactic acid (PLA) is one of the prominent thermoplastics for threedimensional (3D) printing filaments. It is an environmentally friendly, biodegradable polymer, could be used as a replacement of different synthetic, and petroleum-based polymers. However, it has some shortcomings such as water solubility and weak mechanical properties. It was found that some inorganic fillers are good to use along with the PLA to overcome some drawbacks (Sawpan et al. 2019; Sumdani et al. 2019; Razi et al. 2019; Islam et al. 2015; Akindoyo et al. 2015a). Among the fillers, some metal particles, such as zinc, iron, platinum, nickel, are already noted to be used to improve the properties. 3D printing is most recent and advanced materials’ processing with having a number of benefits, such as flexibility of the manufacturing process, accuracy and precision on the dimension, shape and design of the products (Akindoyo et al. 2015b, c; Mina et al. 2014; Hanny et al. 2020). In this study, a 3D printer was used to manufacture composite samples from Fe particles-filled PLA filament. Three different processing temperatures were used to fabricate the specimen. The mechanical, structural and thermal properties of the samples were analyzed to find the effect of the processing temperature. It was found that the change in processing temperature has very minimal effects.

12.2 Methodology Materials 3D PLA filament (Protopasta) were used for this study. A 3D printer was used to prepare the samples. Sample Preparation Before the 3D printing process, the SLT files of the samples were prepared. The specimens were design for testing tensile, flexural and impact testing following different ASTM standards. Characterization The tensile testing was conducted by using a universal tensile testing. The samples were prepared according to the ASTM standard D638. The samples dimensions

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were 125 × 12.3 × 3.3 mm with a gauge length of 50 mm and a crosshead speed of 1 mm/min. The tensile strength and Young’s modulus were measured. The flexural strength and flexural modulus were measured using the same machine used for the tensile testing. The span of two points was 50 mm and with a bending speed of 1 mm/min. Structural conformation along with the functional groups of the samples were determined by Fourier transform of infrared (FTIR) spectroscopy. A fisher scientific apparatus was used for the testing. The scanning range was 500–4000 cm−1 and at least 40 scans were performed. The thermal decomposition behavior of the samples was measured by a thermogravimetric analyzer. Differential scanning calorimetry techniques were used to understand the heat flow at different temperature. A temperature range of 30–600 °C was used for the TGA analysis and for DSC analysis a temperature range of 30– 400 °C. Both testing procedures were conducted in the presence of nitrogen gas flow with a rate of 40 ml/s. The heating rate was 10 °C/min. The ramp heating technique was selected for the testing.

12.3 Results and Discussion The mechanical properties of the samples are presented in Figs. 12.1 and 12.2. Figure 12.1 presents the tensile strength (TS) and tensile modulus (TM) of the samples. It can be seen from the figure that the TS and TM of neat PLA was 42.54 MPa and 2.85 GPa, respectively. On the other hand, FE-PLA1, FE-PLA2 and FE-PLA3 showed a decreasing trend of the TS of 36.25, 36.34 and 34.69 MPa, respectively. The TM of the samples were observed as 3.12, 3.14 and 3.53 GPa for FE-PLA1, FE-PLA2 and FE-PLA3, respectively. Figure 12.2 presents the flexural strength (FS) and flexural modulus (FM) of the samples. It can be seen that the FS and FM of neat PLA was 48.12 MPa and 2.80 GPa, respectively. On the other hand, FE-PLA1, FE-PLA2 and FE-PLA3 showed a decreasing trend of the FS of 39.79, 37.29 and 39.98 MPa, respectively. The FM of the samples were observed as 3.02, 3.34 and 3.63 GPa for FE-PLA1, FE-PLA2 and FE-PLA3, respectively. The interfacial relation between the polymer and the reinforcing agent can be determined by the FTIR analysis. In addition, the presence of the functional groups can also be detected by the FTIR analysis. Moreover, the changes, if any, during the processing of the 3D printing and change in parameters could also be reflected by the spectrum. Figure 12.3 represents the FTIR spectra of the composites. It can be seen that the change in processing of the 3D printing did not show any significant effect in terms of structural conformity. From the figure, it is clear that the stretching vibration of the C=O which is obvious at 1752 cm−1 occurred in all the samples. In terms of the intensity of the peaks were observed to be sharped for the case of Fe

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Fig. 12.1 Tensile properties of the neat PLA and the composites

Fig. 12.2 Three point bending properties of the neat PLA and the composites

particles-filled composites at the range of 1050 to 1250 cm−1 . The C–O stretching can also be detected by the absorbance peak at around 1200 cm−1 . The stretching vibration of the presence of the –CH3 group can be detected by the presence of the absorbance band at around 1450 cm−1 .

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Fig. 12.3 FTIR spectra of the samples

The thermal properties of the composites are determined by the thermogravimetric analysis and differential scanning calorimetry. The samples were heated and their onset degradation and melting temperature were observed in nitrogen atmosphere. Figures 12.4 and 12.5 represent the TGA and DTG thermograms of the samples. It can be seen from Fig. 12.4 that the composite samples showed a lower onset degradation temperature than the neat PLA. The neat PLA showed an onset degradation at 330 °C, whereas the onset degradation temperature of the samples falls at 310–312 °C. The effect of processing temperature did not show any significant effects. In comparison with the FE particles-based samples with the neat PLA it was lower, which may be because of the iron particles. During the heating of the composites samples, the heat transfer through the particles was better and therefore, overall, the samples degraded or decomposed faster than the neat PLA. The melting temperature of the neat PLA was found to be 367 °C, whereas that of the samples was around 318 °C, around 49 °C lower than the neat PLA. The residue of the neat PLA was found to be around 7%, whereas the residue of the samples falls around 13%. The higher percentage of the residue in the composites may be due to the FE particles. The DTG curve in Fig. 12.5 indicates the samples showed a one-stage degradation although the composites is filled with iron particles. This result indicated that the presence of the iron fillers did not provide any changes in the structural conformity. The maximum degradation rate occurred at the peak temperature of the samples. The peak of the DTG curve of the neat PLA was 369 °C, whereas that of the samples at 319 °C. The DSC thermograms of the samples are presented in Fig. 12.6. It was found that the melting point of the composites was 319 °C, whereas that of the

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Fig. 12.4 Weight versus temperature curves of the neat PLA and the composites

Fig. 12.5 Derivative weight versus temperature of PLA and the composites

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neat PLA was 369 °C. Overall, it was found that the composites having a lower thermal properties than the neat PLA due to the thermally conductive FE particles (Tables 12.1 and 12.2).

Fig. 12.6 Heat flow versus temperature curves of neat PLA and the composites

Table 12.1 The nomenclature of the samples Specimen

Processing temperature (°C)

PLA

190

FE-PLA1

190

FE-PLA2

200

FEPLA-3

210

Table 12.2 Thermal properties of the samples Specimen

T onset (°C)

T m (°C)

T max (°C)

PLA

330

367

369

Residues (wt.%) 7.01

FE-PLA1

312

319

319

12.78

FE-PLA2

311

318

319

12.99

FEPLA-3

310

317

319

12.25

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12.4 Conclusion PLA filament filled with iron particles was used to prepare composites using a 3D printer. The samples were tested for mechanical, structural and thermal properties’ analysis. Mechanical testing showed that the tensile strength was decreased due to the incorporation of the FE particles. The changes in the processing parameters of different temperature did not show any significant changes in the properties of the samples. The thermal properties of the samples were also found lower than the neat PLA. No additional functional groups or changes in the bond stretching due to the processing temperature was observed. Acknowledgements The authors would like to acknowledge the help by the Universiti Kuala Lumpur, Malaysia for the support through the research grant, UER21014.

References Akindoyo JO, Beg MDH, Ghazali S et al (2015a) The effects of wettability, shear strength and weibull characteristics of fiber reinforced poly(lactic acid) composites. J Polym Eng 36:489–497 Akindoyo JO, Beg MDH, Ghazali S et al (2015b) Preparation and characterization of poly (lactic acid) based composites reinforced with poly dimethyl siloxane/ ultrasound treated oil palm empty fruit bunch. Polym Plast Technol Eng 54:1321–1333 Akindoyo JO, Beg MDH, Ghazali S et al (2015c) The effects of poly dimethyl siloxane on water absorption and natural degradation of poly (lactic acid)/oil palm empty fruit bunch fiber biocomposites. J Appl Polym Sci 132:42784 Bledzki AK, Reihmane S, Gassan J (1996) Properties and modification methods for vegetable fibers for natural fiber composites. J Appl Polym Sci 5:1329–1336 Hanny F, Firouzi A, Islam MR et al (2020) Mechanical and thermal properties of fishbone-based epoxy composites: effects of heat treatment. Polym Compos 42:1224–1234 Heijenrath R, Peijs T (1996) Natural-fibre-mat-reinforced thermoplastic composites based on flax fibres and polypropylene. Ad Comp Let 5(3):81–85 Hornsby PR, Hinrichsen E, Tarverdi K (1997) Preparation and properties of polypropylene composites reinforced with wheat and flax straw fibres, part II analysis of composite microstructure and mechanical properties. J Mater Sci 32:1009–1015 Islam MR, Beg MDH, Jamari SS (2015) The effects of five different types of acid anhydrides and incorporation of montmorillonite nanoclays on thermosetting resins. Polym Bull 72:3007–3030 Mina MF, Beg MDH, Islam MR et al (2014) structures and properties of injection molded biodegradable poly (lactic acid) nanocomposites prepared with untreated and treated multi-walled carbon nanotubes. Polym Eng Sci 54:317–326 Razi ZM, Islam MR, Parimalam M (2019) Mechanical, structural, thermal and morphological properties of a protein (fish scale)-based bisphenol-A composites. Polym Test 74:7–13 Sanadi AR, Cauldfield DF, Rowell RM (1994) Reinforcing polypropylene with natural fibers. Plastic Engin 4:27–38 Sawpan MA, Islam MR, Beg MDH et al (2019) Effect of accelerated weathering on physicomechanical properties of polylactide bio-composites. J Polym Environ 27:942–955 Sumdani MG, Islam MR, Yahaya ANA (2019) The effects of anioninc-based surfactant on the mechanical, thermal, structural and morphological properties of epoxy–MWCNT composites. Polym Bull 18:13–27

Chapter 13

Mechanical and Thermal Properties of Polylactic Acid/Carbon Fiber Composites Muhammad Remanul Islam, Mohd Al-Fatihhi Mohd Szali Januddi, Mohd Haziq Zakaria, Ahmad Naim Ahmad Yahaya, Sairul Izwan Shafie, and Amin Firouzi Abstract Polylactic acid-based composites were prepared using carbon fibers. A 3D printer was used to fabricate different samples using three different temperatures such as 190, 200, and 210 °C. Different testings such as tensile, flexural, and thermogravimetric analysis and Fourier transform of infrared spectroscopy were used to characterize the samples. Result analysis showed that the composite exhibited lower properties than the neat PLA samples. The results for the parameter variation have minimum effects on the properties of the composites. Keywords Additive manufacturing · PLA/carbon · Filament · Mechanical · Thermal

M. R. Islam (B) · M. A.-F. M. S. Januddi · S. I. Shafie Plant Engineering Technology, Malaysian Institute of Industrial Technology, Universiti Kuala Lumpur, Persinaran Seri Alam, 81750 Pasir Gudang, Johor Bahru, Malaysia e-mail: [email protected] M. A.-F. M. S. Januddi e-mail: [email protected] S. I. Shafie e-mail: [email protected] M. H. Zakaria Quality Engineering Technology, Malaysian Institute of Industrial Technology, Universiti Kuala Lumpur, Persinaran Seri Alam, 81750 Pasir Gudang, Johor Bahru, Malaysia e-mail: [email protected] A. N. A. Yahaya Institute of Postgraduate Studies, Universiti Kuala Lumpur, Kuala Lumpur, Malaysia e-mail: [email protected] A. Firouzi Nanomaterials and processes, GE Appliances, Louisville, KY, USA e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 A. Ismail et al. (eds.), Materials Innovations and Solutions in Science and Technology, Advanced Structured Materials 173, https://doi.org/10.1007/978-3-031-26636-2_13

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13.1 Introduction Nowadays, bio-based and renewable materials are promising to manufacture polymer-based composites for different applications, such as vehicle body parts, building materials, furniture, and composites. There are a number of bio-based polymers which are of great importance for these purposes. For example, polyalkydes from vegetable oil, polylactic acid (PLA) from dairy raw materials, and cellulose from biomass are some important polymers that have been used for different applications. The uses of these bio-based materials are safe and environment-friendly (Hornsby et al. 1997; Heijenrath and Peijs 1996; Sanadi et al. 1994; Bledzki et al. 1996). PLA has been used already for the replacement of synthetic petroleum-based polymer matrices. The properties of PLA-based composites are comparable with those of synthetic-polymer-based composites, but still some drawbacks are noticed. For example, PLA based composites showed a brittle nature and very high stiffness. It was documented that some organic and inorganic fillers are used to reinforce the PLA to improve its performances (Hanny et al. 2020; Sawpan et al. 2019; Sumdani et al. 2019). Different types of natural and synthetic fibers were used with PLA for the reinforcing purposes. Among the synthetic fibers, glass fiber, carbon fiber, and aramid or Kevlar fibers are important. The enhancement of the properties due to the reinforcement of the synthetic fibers was also noticed. Three-dimensional (3D) or additive manufacturing are, nowadays, the most advanced manufacturing techniques due to their various benefits towards the fabrication and processing of the polymer-based composites. Some of the benefits include complex designing, different shapes and preciseness of the measurement. The filament of the composites is the processing materials of a 3D printer (Razi et al. 2019; Islam et al. 2015; Akindoyo et al. 2015a, b, c; Mina et al. 2014). There are several parameters, which might have some effects on the properties of the manufactured samples. In this study, a 3D printer was used to fabricate PLA-carbon fiberbased composites samples at different processing temperatures. It was found that the changes in the temperature have minimal effects on the properties of the composites.

13.2 Methodology Materials 3D PLA filament (Protopasta) was used for this study. A 3D printer was used to prepare the samples. Sample Preparation Before the 3D printing process, the .SLT files of the samples were prepared. The specimens were design for testing tensile, flexural and impact testing following different ASTM standards.

13 Mechanical and Thermal Properties of Polylactic Acid/Carbon Fiber … Table 13.1 The nomenclature of the samples

Specimen

Processing temperature (°C)

PLA

190

CF-PLA1

190

CF-PLA2

200

CF-PLA-3

210

137

Characterization The tensile testing was conducted by using a universal tensile testing. The samples were prepared according to the ASTM standard D638. The samples dimensions were 125 × 12.3 × 3.3 mm. The gage length was 50 mm. The crosshead speed was 1 mm/min. The tensile strength and Young’s modulus were measured. The flexural strength and flexural modulus were measured using the same machine used for the tensile testing. The span of the testing was 50 mm, and the speed was 1 mm/min. The structural properties along with the functional groups of the samples were determined by Fourier transform of infrared (FTIR) spectroscopy. A Fisher Scientific apparatus was used for the testing. The scanning range was 500–4000 cm−1 , and at least 40 scans were performed. The thermal properties of the samples were measured using a thermogravimetric analyzer, and a differential scanning calorimeter. A temperature range of 30–600 °C was used for the TGA analysis, and for DSC analysis a temperature range of 30– 400 °C. Both tests were conducted in the presence of nitrogen gas flow with a rate of 40 ml/s. The heating rate was 10 °C/min. The ramp heating technique was selected for the testing (Table 13.1).

13.3 Results and Discussion The mechanical properties of the samples are presented in Table 13.2. The tensile strength (TS) and tensile modulus (TM) of the samples were determined. It can be seen from the table that the TS and TM of neat PLA were 42.54 MPa and 2.85 GPa, respectively. The TS of CF-PLA1, CF-PLA2, and CF-PLA3 was 38.67, 39.27, and 40.23 MPa, whereas the TM of the samples was observed as 3.44, 3.67, and 3.83 GPa for CF-PLA1, CF-PLA2, and CF-PLA3, respectively. The TS was found to be decreased whereas, the TM was found to be increased gradually due to the increment of the processing temperature from 190 to 210 °C. This may be due to the higher molecular mobility of the polymer chain at higher temperature leading to a better reinforcement (Table 13.3).

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Table 13.2 Mechanical properties of the samples Specimen

TS (MPa)

TM (GPa)

FS (MPa)

FM (GPa)

PLA

42.54

2.85

48.12

2.80

CF-PLA1

38.67

3.44

42.45

3.33

CF-PLA2

39.27

3.67

41.99

3.56

CF-PLA-3

40.23

3.83

43.26

3.78

Table 13.3 Thermal properties of the samples Specimen

T onset (°C)

T m (°C)

T max (°C)

Residues (wt. %)

PLA

330

378

360

6

CF-PLA1

335

320

358

7

CF-PLA2

336

318

360

8

CF-PLA-3

338

320

360

9

A similar trend of results was observed for the case of the flexural strength (FS) and flexural modulus (FM). The FS and FM of the neat PLA were 48.12 MPa and 2.80 GPa, respectively. The FS of CF-PLA1, CF-PLA2, and CF-PLA3 showed a decreasing trend; the values were 42.45, 41.99, and 43.26 MPa, respectively. The FM of the samples was observed as 3.33, 3.56, and 3.78 GPa. The functional groups of the samples and established interaction between the fillers and the polymer matrix were observed using FTIR analysis. In addition, the changes of chemical shift of the absorbance peaks due to the processing temperature changes was also observed by the testing. The results of the composites were compared, and the deviation of the absorbance peaks compared with the neat PLA was presented. Figure 13.1 represents the FTIR spectra of the neat PLA and the composites. From the figure, it is clear that the processing of the temperature in 3D printing did not affect much in terms of shifting of the peaks or changing the nature or intensity of the peaks. From the figure, it can be seen that the peak at around 1755 cm−1 is due to the stretching vibration of the carbonyl group. For the composites, it was found slightly shifted to the right may be due to the reinforcement effect. The intensity of the peaks was found also similar as of indicating no effect or zero effect of temperature changes in the processing of the samples. The peak at around 1205 cm−1 was due to the presence of the C–O stretching. The methyl group is detected by the presence of the peak at 1455 cm−1 . The thermal decomposition behavior of the neat PLA and its CF-based composites is analyzed via a thermogravimetric analyzer and differential scanning calorimeter. The onset degradation, completion of the decomposition, and the melting temperature were recorded. The TGA and DTG thermograms are presented in Figs. 13.2 and 13.3,

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Fig. 13.1 FTIR spectra of the samples

Absorbance (a. u.)

CF-PLA

CF-PLA

CF-PLA PLA

1000

1500

2000

2500

3000

3500

4000

-1

Wavenumbers (cm )

respectively. It is clear from the figures that the onset degradation temperature of the composites are close to that of the neat PLA. The CF-PLA1 and CF-PLA3 showed a slightly higher onset degradation temperature compared to the neat PLA. The neat PLA showed an onset degradation at 330 °C, whereas the onset degradation temperature of CF-PLA1, CF-PLA2, and CF-PLA3 was the samples falls at 335–338 °C. Therefore, the onset degradation temperature was increased by 5–8 °C compared to the neat PLA. This is because of the reinforcement effect by the CF. The effect of processing temperature has a minimal effect on the onset degradation 100

PLA CF-PLA1 CF-PLA2 CF-PLA3

90 80

Weight (%)

Fig. 13.2 TGA thermograms of the samples

70 60 50 40 30 20 10 0 50

100 150 200 250 300 350 400 450 500 o

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Fig. 13.3 DTG thermograms of the samples

o

Derivative weight (%/ C)

PLA FE-PLA FE-PLA FE-PLA

50

100 150 200 250 300 350 400 450 500 o

Temperature ( C)

temperature. The 50% of the degradation of the samples are completed by the temperature of 360 °C. The completion of the degradation was recorded by the temperature of 390 °C. The residue of the samples fall in the range of 6–9 wt.%. From the DTG curve of the samples, it is seen that the samples are decomposed in one stage. The maximum peak temperature falls around 360 °C. The DSC thermograms of the samples are presented in Fig. 13.4. It was found that the melting point of the composites was 320 °C, whereas that of the neat PLA was 378 °C. Overall, it was found that the composites having lower thermal properties than the neat PLA.

Heat flow (a. u.) Exo

Fig. 13.4 DSC thermograms of the samples FE-PLA3 FE-PLA2

FE-PLA1

PLA

50

100 150 200 250 300 350 400 450 500 o

Temperature ( C)

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13.4 Conclusion This study was about to investigate the effects of the processing temperature of a 3D printing process to fabricate composite samples from CF-filled PLA filament. The different temperatures were 190, 200, and 201 °C. Different properties such as mechanical, thermal, and structural properties of the samples were investigated. It was found an almost minimal effect of changing the processing temperature during 3D priming of these samples. Acknowledgements The authors are thankful to the center of research and innovation (CoRI) of the Universiti Kuala Lumpur, Malaysia, for providing the financial support for the project through the research grant, UER21014.

References Akindoyo JO, Beg MDH, Ghazali S et al (2015a) The effects of wettability, shear strength and weibull characteristics of fiber reinforced poly(lactic acid) composites. J Polym Eng 36:489–497 Akindoyo JO, Beg MDH, Ghazali S et al (2015b) Preparation and characterization of poly (lactic acid) based composites reinforced with poly dimethyl siloxane/ultrasound treated oil palm empty fruit bunch. Polym Plast Technol Eng 54:1321–1333 Akindoyo JO, Beg MDH, Ghazali S et al (2015c) The effects of poly dimethyl siloxane on water absorption and natural degradation of poly (lactic acid)/oil palm empty fruit bunch fiber biocomposites. J Appl Polym Sci 132:42784 Bledzki AK, Reihmane S, Gassan J (1996) Properties and modification methods for vegetable fibers for natural fiber composites. J Appl Polym Sci 5:1329–1336 Hanny F, Firouzi A, Islam MR et al (2020) Mechanical and thermal properties of fishbone-based epoxy composites: effects of heat treatment. Polym Compos 42:1224–1234 Heijenrath R, Peijs T (1996) Natural-fibre-mat-reinforced thermoplastic composites based on flax fibres and polypropylene. Ad Comp Let 5(3):81–85 Hornsby PR, Hinrichsen E, Tarverdi K (1997) Preparation and properties of polypropylene composites reinforced with wheat and flax straw fibres, part II analysis of composite microstructure and mechanical properties. J Mater Sci 32:1009–1015 Islam MR, Beg MDH, Jamari SS (2015) The effects of five different types of acid anhydrides and incorporation of montmorillonite nanoclays on thermosetting resins. Polym Bull 72:3007–3030 Mina MF, Beg MDH, Islam MR et al (2014) structures and properties of injection molded biodegradable poly (lactic acid) nanocomposites prepared with untreated and treated multi-walled carbon nanotubes. Polym Eng Sci 54:317–326 Razi ZM, Islam MR, Parimalam M (2019) Mechanical, structural, thermal and morphological properties of a protein (fish scale)-based bisphenol-A composites. Polym Test 74:7–13 Sanadi AR, Cauldfield DF, Rowell RM (1994) Reinforcing polypropylene with natural fibers. Plastic Engin 4:27–38 Sawpan MA, Islam MR, Beg MDH et al (2019) Effect of accelerated weathering on physicomechanical properties of polylactide bio-composites. J Polym Environ 27:942–955 Sumdani MG, Islam MR, Yahaya ANA (2019) The effects of anioninc-based surfactant on the mechanical, thermal, structural and morphological properties of epoxy–MWCNT composites. Polym Bull 18:13–27

Chapter 14

Antioxidant and Antibacterial Activities in Kaffir Lime (Citrus hystrix) Essential Oil Extracted by the Hydro-distillation Method Mazlin Mohideen, Nik Nur Syahidatul Jannah Mahadi, Nur Aina Nabilah Suhaimi, and Nur Azzalia Kamaruzaman Abstract Kaffir lime (Citrus hystrix), also known among the locals as ‘limau purut’, is one of Malaysia’s most lucrative commercial fruit harvests. Apart from being a staple ingredient in most Asian cuisines, the essential oil extracted from the fruit has a wide range of applications. Essential oil, also known as aromatic oil, is a colourless and concentrated hydrophobic liquid with the presence of several chemical components such as phenols, flavonoids, and terpenoids. These major chemical components contribute to the pleasant and intense aromatics of essential oil. Extraction of essential oil may derive from peels or leaves by various extraction methods. A few synthetic antioxidant supplements have been reported to be harmful and toxic to the human body. Additionally, the emergence of pathogenic microorganisms has led to the development of resistance to major classes of antibacterial drugs. Hence, a potential natural antioxidant and antibacterial agents with special active compounds in the herbal plants that are safer for human consumption need to be identified. This study aims to determine and evaluate the antioxidant and antibacterial activities of Kaffir lime essential oil by the DPPH (1,1–diphenyl-2-picryl hydroxyl) assay and disc diffusion method, respectively. Resultantly, the Kaffir lime essential oil obtained through the hydro-distillation process was stable with potent antioxidant activity against free radicals. Kaffir lime is easily accessible, and the essential oil extracted by the hydrodistillation method in this study has low handling cost and potential activity against various types of bacteria. This study provides a natural antioxidant and antibacterial M. Mohideen (B) · N. N. S. J. Mahadi · N. A. N. Suhaimi Faculty of Pharmacy and Health Sciences, Universiti Kuala Lumpur Royal College of Medicine Perak, Ipoh, Perak, Malaysia e-mail: [email protected] N. N. S. J. Mahadi e-mail: [email protected] N. A. N. Suhaimi e-mail: [email protected] N. A. Kamaruzaman National Poison Centre, Universiti Sains Malaysia, 11800 Minden, Pulau Pinang, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 A. Ismail et al. (eds.), Materials Innovations and Solutions in Science and Technology, Advanced Structured Materials 173, https://doi.org/10.1007/978-3-031-26636-2_14

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source to ensure consumers’ good health and well-being. These health benefits may assist in preventing several chronic diseases, including inflammation and cancer. Findings from this study will also be beneficial as a future reference for researchers to develop new formulations for antioxidant and antibacterial purposes. Keywords Antioxidant · Antibacterial · Phytochemicals · Hydro-distillation · Essential oil

14.1 Introduction Medicinal plants or herbal medicines have been known to be useful in maintaining human health since ancient times. These events had led to the development and practice of using such plants as sources of medications worldwide (Srivastava 2018). Kaffir lime tree (Citrus hystrix) is a tropical herb with powerful aromatics found in Southeast Asia countries. Each part of the Kaffir lime tree has several uses and advantages. Kaffir lime fruits are usually used as a condiment in some Malaysian and Thai cuisines (Wulandari et al. 2017). Kaffir lime is locally known as ‘limau purut’ in Malaysia, ‘makrut lime’ in Thailand, ‘chanh kaffir’ in Vietnam, and ‘jeruk purut’ in Indonesia (Samraj and Rajamurgugan 2017). The biological classification of the Kaffir lime tree is classified as shown in Table 14.1. The Kaffir lime tree is small, shrubby, and grows approximately 3–5 m in height. The tree has aromatic dark green leaves about 7.5–10 cm long and 5 cm wide. The leaves are dark green, are found in distinctive “double” shapes, and grow about 3 to 6 m tall (Ali et al. 2015). The tree also has white flowers with 4–6 petals with a diameter ranging from 5 to 7 cm. The dark green Kaffir lime fruit has a diameter of about 5.0–7.5 cm with a wrinkle on its surface. The fruit is pear-shaped, has a sour taste, and turns to a yellow shade upon maturation (Md Othman et al. 2016). Essential oil, also known as aromatic oil, is a colourless and concentrated hydrophobic liquid with the presence of many bioactive components such as phenols, flavonoids, and terpenoids. These major bioactive components can produce pleasant and intense aromatics in essential oil (Rassem et al. 2016). Additionally, the therapeutic effects of the plants are mostly due to the presence of bioactive compounds or phytochemical constituents. Each part of the plant possesses different bioactive compounds in various amounts. The higher the amount of these bioactive compounds, Table 14.1 Biological classification of Kaffir lime tree (Samraj and Rajamurgugan 2017)

Kingdom

Plantae

Order

Spindales

Family

Rutaceae

Genus

Citrus S

Species

Citrus hystrix DC

Scientific name

Citrus hystrix

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the higher the plant’s therapeutic effect or medicinal value. The bioactive compounds are identified through phytochemical screening or phytochemical tests (Oladeji 2016). Various extraction methods are employed to extract the essential oil from peels or leaves. Apart from being a common ingredient in Asian cuisines, the extracted essential oil has diverse applications (Sauid and Aswandi 2018). Furthermore, essential oil is widely extracted and used for medicinal purposes due to its economic and biological values (Lourenço et al. 2019). An antioxidant is a stable molecule that can terminate or neutralize free radicals by transferring electrons and preventing cell damage. The antioxidant has radical scavenging activity properties that can safely interact with free radicals and inhibit the chain before the macromolecules or cells are damaged (Lobo et al. 2010). Generally, antibacterial activity of a substance is defined as the substance’s ability to inhibit growth of bacteria or kill bacteria colonies. This is particularly applicable for the human body in terms of treating skin infections and other related diseases (Varsha and Chaudhari 2016). Scientific research states that Kaffir lime oil exhibits profound medicinal values, such as antioxidant, antibacterial, and antileukemic (Chueahongthong et al. 2011). Due to its diverse medicinal values, the plant was selected in this study as a sample to observe its antioxidant and antibacterial activities. A study found that flavonoids and phenols in Kaffir lime leaves play a significant role in their potent antioxidant property (Pham-Huy et al. 2008). Therefore, this study will focus on the antioxidant and antibacterial properties of Kaffir lime essential oil extracted by the hydrodistillation method, which is commonly used to extract essential oils from plant samples. Moreover, this method protects the leaves’ original quality and prevents damage (Wulandari et al. 2019).

14.2 Methodology 14.2.1 Plants Material Collection of plants Fresh Kaffir lime fruits were purchased from Econsave Supermarket, Ipoh. The fruits’ peels and leaves were dried in an oven for at least five days at 50 °C. The cleaned and dried plant samples were ground to a fine powder for the extraction step. Essential oil extraction A distilling flask with 600 ml of distilled water was used to soak in about 100 g of Kaffir lime sample, whereby the hydro-distillation method utilized a Clevenger type apparatus (Al-Hilphy 2017), and the process was run for three hours. To avoid

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excess evaporation, extraction temperature was maintained below 100 °C. Subsequently, dried anhydrous sodium sulphate was used to separate the oily layer from the distillate. Yield of essential oil was obtained after three hours and kept in the dark glass bottle at 4 °C for further analysis.

14.2.2 Essential Oil Screening for Antioxidant Potential The 1,1-Diphenyl-2-Picrylhydrazil (DPPH) method was used to determine antioxidant properties in Kaffir lime leaves. The assay was performed at room temperature and dark environment. A DPPH solution was prepared by dissolving 2.4 mg of DPPH powder in 100 ml of methanol. Next, 0.3 ml of each sample containing different concentrations of plant extract and methanol was pipetted into another test tube. Thereafter, 2.7 ml of DPPH solution was added to each test tube and mixed using a vortex mixer. The mixture in all tubes was incubated for one hour, and the absorbance values were determined at a 517 nm spectrophotometer. Finally, the percentage of the inhibition activity was calculated, see Eq. (14.1) (Kumara et al. 2018). (Ao − Ax) × 100% Ao

(14.1)

14.2.3 Antibacterial Screening All the bacterial test strains against human subjects were obtained from the laboratory of UniKL-RCMP. The bacterial strain isolated was identified as Gram-positive bacteria (S. aureus and S. epidermidis) and Gram-negative bacteria (E. coli and S. dysenteriae). All bacteria were subcultured and maintained in a semisolid medium of Nutrient Agar (NA) plates by streaking method and stored at 4 °C. Bacterial Suspension Preparation A single colony of each Gram-positive and Gram-negative bacteria culture was transferred in 10 ml of Mueller Hinton Broth (MHB). To reach the exponential phase of 0.5 McFarland standard, the prepared bacterial suspension was incubated at 37 °C for three hours. Turbidity check was conducted by subjecting each bacterial suspension to a single-beam spectrophotometer at 600 nm. Based on 0.5 McFarland standard, an absorbance reading of between 0.08 and 0.1 is acceptable. The following antibacterial assay utilized the prepared bacterial suspensions directly. Method of Disc Diffusion The antibacterial test of Kaffir lime peel was evaluated using the disc diffusion method. Using a sterile cotton swab, the surface of Mueller Hinton (MH) agar was spread homogeneously with bacterial suspension. A 6 mm disc paper (Whatman

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filter paper) was saturated with 20 µl essential extracts oil. The discs were aseptically placed apart on each agar plate and gently pressed to ensure contact with the agar surface. Two standard antibiotic discs of Gentamycin and Streptomycin were used as a positive control, and 20 µl of 1% DMSO impregnated disc was used as a negative control. Each test plate contained four discs: two positive controls, one negative control, and the essential oil extract. Each bacterial assay was performed in triplicates. The plates were incubated for 24 h at 37 °C in the incubator. The antibacterial activity against the selected bacteria was ascertained based on the zone of inhibition. The activity strength was evaluated by measuring the inhibition zone of the diameter of the bacterial growth on the plates (Abdallah 2016). The inhibition zone diameter (IZD) of C. hystrix peel’s essential oil was measured and interpreted based on the following criteria: no activity, IZD = 6 mm; weak activity, IZD = 6 to 2 mm; moderate activity, IZD = 12–20 mm; and strong activity, IZD = more than 20 mm (Lv et al. 2011).

14.3 Results and Discussion 14.3.1 Extraction of Essential Oil The percentage yield of essential oil was obtained after three hours. The volume of essential oil in Kaffir lime obtained in three hours varied in each trial of extraction using the hydro-distillation method due to various factors. This is mainly attributed to process parameters, which are temperature, environmental conditions, and techniques during the extraction. The essential oil yield obtained is presented in Table 14.2 for peels and leaves, respectively. The percentage of yield of essential oils was calculated, see Eq. (14.1): Yield =

Table 14.2 Percentage extraction yield of essential oil

Weight of essential oils obtained × 100 Weight of initial Kaffir Lime peels

(14.2)

Kaffir lime sample Extraction yield (% Physical appearance w/w) Peel

7.63

Colourless

Leaves

1.03

Colourless

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14.3.2 DPPH Radical Scavenging Activity For the DPPH of Kaffir lime leaves essential oil, Fig. 14.1 depicts that tubes 1 and 2 are purple colour solutions at a low concentration of 31.25 and 62.5 µg/ml, respectively. While tubes 3, 4, 5 and 6 (125, 250, 500, and 1000 µg/ml, respectively) reflected a yellow colour solution that indicates decolourization. The decolourization revealed the antioxidant activity in Kaffir lime leaves essential oil. The higher the decolourization, the higher the reducing ability (Lobo et al. 2010). The free radical of DPPH got neutralized by accepting hydrogen atoms from antioxidants. The DPPH for the standard ascorbic acid (Fig. 14.2) revealed a yellow colour in all test tubes. This might be due to the high radical scavenging activity in ascorbic acid. Hence, yellow colouration is still produced at a low concentration. Theoretically, the absorbance value decreases from low to high concentration as the reduction of DPPH occurs. In this study, as the absorbance value of Kaffir lime leaves essential oil decreases, the radical scavenging activity (RSA %) increases from low concentration to high concentration (Fig. 14.3). The DPPH results are expressed as IC50 , which indicates the concentration providing 50% inhibition (IC50 ) values or in other words, the amount required to scavenge 50% DPPH free radicals. The high value of IC50 indicates low radical scavenging activity or low antioxidant activity (Phuyal et al. 2020). In this experiment, the Kaffir lime leaves essential oil was higher in absorbance value and had lower antioxidant activity than ascorbic acid. Meanwhile, the IC50 of standard ascorbic acid was 20.898 µg/ml compared to that of Kaffir lime leaves essential oil at 142.767 µg/ml, which is higher than standard ascorbic acid. Another study reported that the DPPHIC50 of Kaffir lime leaves varied from 65 to 300 µg/ml, depending on solvent and extraction method (Jamilah et al. 2011).

Fig. 14.1 DPPH of Kaffir lime leaves essential oil

Fig. 14.2 DPPH of standard ascorbic acid

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Fig. 14.3 Radical scavenging activity versus different concentrations of essential oil and ascorbic acid

14.3.3 Disc Diffusion Antibacterial Activity Assay Antibacterial activity of Kaffir lime peel essential oil against two clinically isolated bacterial strains, Gram-positive and Gram-negative bacteria, is shown in Table 14.3. The screening of the antibacterial activity was carried out by agar disc diffusion. According to Lv et al. (2011), a potent antibacterial property of essential oils is when the inhibition zone of diameter is more significant than 20 mm (Lv et al. 2011). The results demonstrated that the essential oil of Kaffir lime peel displayed good antibacterial activities against S. epidermidis (Fig. 14.4) as similar to S. aureus (Fig. 14.5). For S. aureus, the bacteria were more susceptible to the extracts than the positive control. Both gentamicin and streptomycin yielded a moderate inhibition of bacterial growth. For S. epidermidis, the bacteria were more susceptible to only one of the positive controls, which was gentamicin. However, the bacteria demonstrated resistance against streptomycin. This suggests that Kaffir lime peel essential oil, when applied to the genus Staphylococcus demonstrated antibacterial activity. Table 14.3 Antibacterial activity of Kaffir lime peel essential oil against bacterial strains Bacteria

Zone of inhibition diameter (mm) Essential oil extracts

Gentamicin

Streptomycin

1% DMSO

S. aureus

19.3 ± 1.5

15 ± 0.0

13 ± 1.0

–

S. epidermidis

19.3 ± 0.6

50.7 ± 0.6

–

–

8.3 ± 0.6

23.7 ± 0.6

17.7 ± 0.6

–

11.7 ± 0.6

27.3 ± 0.6

24.7 ± 0.6

–

E. coli S. dysentriae

– is no inhibition zone

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Fig. 14.4 S. aureus inhibition zone

Fig. 14.5 S. epidermidis inhibition zone

For Gram-negative bacteria, the C. hystrix peel essential oil exhibited weak and moderate levels of antibacterial activity for E. coli (Fig. 14.6) and S. dysenteriae (Fig. 14.7), respectively. Compared to the plant extracts, the bacteria showed higher susceptibility to the positive controls, as evidently, gentamicin and streptomycin produced higher diameter of inhibition zone, thus eliciting stronger bacterial inhibition. The results obtained from this study were supported by another study conducted by Sreepian et al. (2019), where it was found that Kaffir lime essential oil exhibited moderate and weak levels of antibacterial activity against S. aureus and E. coli, respectively (Sreepian et al. 2019). The current study reported Gram-positive Fig. 14.6 E. coli inhibition zone

Fig. 14.7 S. dysentriae inhibition zone

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bacteria to exhibit higher sensitivity to the plant extracts in comparison to Gramnegative bacteria. This is further justified as the presence of complex cell wall components for Gram-negative bacteria when compared to Gram-positive bacteria (Nazzaro et al. 2013). In addition, permeability of essential oil for Gram-negative bacteria cell penetration is limited in the presence of lipopolysaccharide layer (Chimnoi et al. 2018). Furthermore, the positive control, gentamicin, was recorded to have a good inhibition zone diameter in all tested bacteria, whereby a zone diameter of inhibition ≥15 mm is considered a standard susceptibility. Meanwhile, only S. epidermidis was resistant to Streptomycin as no antibacterial activity was observed in the three replications.

14.4 Conclusion In conclusion, about 7.3 and 1.03% yield of Kaffir lime peels and leaves essential oil have been successfully extracted using the DPPH and hydro-distillation methods, respectively. In the DPPH of Kaffir lime leaves assay, the decolourization from purple to yellow colour solution revealed the antioxidant activity. The DPPH-IC50 of Kaffir lime leaves essential oil was 142.767 µg/ml, with lower antioxidant activity than standard ascorbic acid. The Kaffir lime peel’s essential oil possessed antibacterial activity against all tested bacteria by measuring the diameter of the inhibition zone around the discs. These findings revealed the promising potential of Kaffir lime essential oil as an antioxidant and an antibacterial agent for therapeutic applications. Acknowledgements The authors were grateful to Universiti Kuala Lumpur Royal College of Medicine Perak (UniKl RCMP), Ipoh, Perak, Malaysia, for the provision of facilities and services for the completion of this study. Special thanks to everyone for the support and contribution involved during the completion of this study.

References Abdallah EM (2016) Preliminary phytochemical and antibacterial screening methanolic leaf extract of Citrus aurantifolia. Pharm Biotechnol Curr Res 1(1):1–5 Al-Hilphy A (2017) Engineering interventions for extraction of essential oils from plants. Eng Interv Foods Plants. Apple Academic Press Ali B, Al-Wabel NA, Shams S et al (2015) Essential oils used in aromatherapy: a systemic review. Asian Pac J Trop Biomed 5(8):601–611 Chimnoi N, Reuk-Ngam N, Chuysinuan P et al (2018) Characterization of essential oil from Ocimum gratissimum leaves: antibacterial and mode of action against selected gastroenteritis pathogens. Microb Pathog 118:290–300 Chueahongthong F, Ampasavate C, Okonogi S et al (2011) Cytotoxic effects of crude Kaffir Lime (Citrus hystrix, DC.) leaf fractional extracts on leukemic cell lines. J Med Plant Res 5(14):3097– 3105

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Jamilah B, Abdulkadir Gedi M, Suhaila M et al (2011) Phenolics in Citrus hystrix leave obtained using supercritical carbon dioxide extraction. Int Food Res J 18(3):941–948 Kumara P, Sunil K, Arun KB (2018) Determination of DPPH free radical scavenging activity by RP-HPLC, rapid, sensitive method for the screening of berry fruit juice freeze-dried extract. Nat Prod Chem Res 6(5):1000341 Lobo V, Patil A, Phatak A et al (2010) Free radicals, antioxidants, and functional foods: impact on human health. Pharmacogn Rev 4(8):118–126 Lourenço SC, Moldão-Martins M, Alves VD (2019) Antioxidants of natural plant origins: from sources to food industry applications. Molecules 24(22):4132 Lv F, Liang H, Yuan Q et al (2011) In vitro antimicrobial effects and mechanism of action of selected plant essential oil combinations against four food-related microorganisms. Food Res Int 44:3057–3064 Md Othman SNA, Hassan MA, Nahar L et al (2016) Essential oils from the Malaysian Citrus (Rutaceae) medicinal plants. Med 3(2):13 Nazzaro F, Fratianni F, De Martino L et al (2013) Effect of essential oils on pathogenic bacteria. Pharm 6(12):1451–1474 Oladeji O (2016) The characteristics and roles of medicinal plants: some important medicinal plants in Nigeria. Nat Prod Indian J 12(33):102 Pham-Huy LA, He H, Pham-Huy C (2008) Free radicals, antioxidants in disease and health. Int J Biomed Sci: IJBS 4(2):89–96 Phuyal N, Jha PK, Raturi PP et al (2020) Total phenolic, flavonoid contents, and antioxidant activities of fruit, seed, and bark extracts of Zanthoxylum armatum DC. Science World J 8780704 Rassem HH, Nour AH, Yunus RM (2016) Techniques for extraction of essential oils from plants: a review. Aust J Basic Appl Sci 10(16):117–127 Samraj S, Rajamurgugan S (2017) Qualitative and quantitative estimation of bioactive compounds and antioxidant activity in Citrus hystrix. Int J Eng Sci Comput 7(6):13154–13163 Sauid SM, Aswandi FA (2018) Extraction methods of essential oil from Kaffir Lime (Citrus hystrix): a review. Malaysia J Chem Eng Technol 1:56–64 Sreepian A, Sreepian PM, Chanthing C et al (2019) Antibacterial activity of essential oil extracted from Citrus hystrix (Kaffir Lime) peels An in vitro study. Trop Biomed 36(2):531–541 Srivastava AK (2018) Significance of medicinal plants in human life. Synth Med Agents Plants. https://doi.org/10.1016/B978-0-08-102071-5.00001-5 Varsha M, Chaudhari (2016) Studies on antimicrobial activity of antiseptic soap and herbal soaps against selected human pathogens. J Sci Innov Res 5(6):201–204 Wulandari WY, Darmadji P, Kurniawati L (2017) Antioxidant properties of Kaffir Lime oil as affected by hydro-distillation process. Proc ICTESS (int Conf Technol Educ Soc Sci) 1(1):242– 248 Wulandari YW, Supriyadi S, Anwar C (2019) Comparison between hydro-distillation with steam explosion and conventional hydro-distillation in Kaffir Lime oil extraction. Agric-Tech 39(4):306–314

Chapter 15

Thermal and Microbiological Properties of Spray Dried Lactobacillus Plantarum-Banana Peel Powder Nurul Hafifah Abdul Wahid, Nur Ain Syuhada Zamri, Mohd Al-Fatihhi Mohd Szali Januddi, and Shahrulzaman Shaharuddin Abstract This research aimed to improve the survivability of Lactobacillus plantarum (LP) during the microencapsulation process and simulated heat exposure by immobilization with banana peel (BP) and maltodextrins as microencapsulating agent. Different BP content of 0%, 2% and 4% and two chemical grades of maltodextrin which are chemical pure grade (Cp) and commercial grade (Com) were applied in producing the microcapsules. Significance enhancement in the microencapsulation efficiency and cell survivability after simulated heat exposure of 90 °C for 30 s was achieved via the probiotic immobilization before microencapsulation process. The 4% inclusion of BP in microencapsulated LP with Cp maltodextrin was the best samples that attained the highest cell survivability after microencapsulation and heat exposure (82.06% and 66.01%, respectively). The loss of mass was slowed down with the inclusion of higher percentage of BP. The incorporation of BP has enhanced the survivability of probiotic during microencapsulation and simulated heat exposure, thus creating an opportunity of probiotic application in high thermal processing units. Keywords Lactobacillus · Immobilization · Banana peel · Microencapsulation · Thermal · Microbiological N. H. Abdul Wahid · N. A. S. Zamri Section of Food Engineering Technology, Malaysian Institute of Chemical and Bioengineering Technology, Universiti Kuala Lumpur, Lot 1988 Vendor City, Taboh Naning, 78000 Alor Gajah, Melaka, Malaysia e-mail: [email protected] N. A. S. Zamri e-mail: [email protected] M. A.-F. Mohd Szali Januddi · S. Shaharuddin (B) Advanced Facilities Engineering Technology, Plant Engineering Technology Section, Malaysian Institute of Industrial Technology, Universiti Kuala Lumpur, Jalan Persiaran Sinaran Ilmu, Bandar Seri Alam, 81750 Masai, Johor, Malaysia e-mail: [email protected] M. A.-F. Mohd Szali Januddi e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 A. Ismail et al. (eds.), Materials Innovations and Solutions in Science and Technology, Advanced Structured Materials 173, https://doi.org/10.1007/978-3-031-26636-2_15

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15.1 Introduction FAO/WHO describes probiotic as microorganisms that provide one or more health benefits for the hosts when administered in an adequate amount (Dianawati et al. 2016). Probiotics promote a desirable gastrointestinal microflora which is known to enhance the overall wellness (Othman et al. 2018). Probiotic bacteria play a role in health promotion and maintenance (Amara and Shibl 2015). Consuming a sufficient dose of probiotic bacteria is necessary to provide health benefits. Since probiotics must be protected against oxygen, heat and other environmental challenges during drying, processing and storage, as well as low pH and protease in the gastrointestinal tract, it is critical to select the correct wall material (Palanivelu et al. 2022). Thus, protection from adverse conditions yet allowing the release of viable and metabolically active probiotics in the intestine is the main purpose of encapsulation (Misra et al. 2022). Probiotic can be including the lactic acid bacteria (LAB), non-lactic acid bacteria and yeast as it can survive until intestine and provide advantages on the health of the host. Among most important probiotic known to have advantageous effects on the host gastrointestinal (GI) tract are lactic acid bacteria (Burgain et al. 2011). In addition, lactobacilli species has great potential for use in the probiotic industries because of its high stability during processing and resistance to gastrointestinal acid and bile condition (Othman et al. 2018). Dietary fibers can be defined as edible and non-digestible carbohydrates that pass relatively unchanged through gastric and intestine (Anekella and Orsat 2013). Dietary fiber can be classified into two which are soluble and insoluble fiber. Consumption of soluble dietary fiber can lower the serum cholesterol and helps in reducing the risk of colon cancer, while insoluble dietary fiber has been shown to be beneficial for intestinal regulation and increasing stool volume (Ramli et al. 2010). Dietary fibers can serve as prebiotics which encouraging the growth of favorable gut bacteria. Prebiotics play important role in promoting gut and promote the growth of probiotics in the colon by stimulating proliferation and host immunological response or probiotic ´ 2017). Along with prebiotics, microencapsulaactivity (Markowiak and Slizewska tion of probiotic bacteria is instrumental in viability enhancement during processing and the gastrointestinal tract-targeted delivery (Mortazavian et al. 2007). Fruit wastes are accumulated in enormous numbers due to the heavy food consumption and industrial demand region (Ibrahim et al. 2017). One of the most common waste products created during the processing of bananas is banana peel. Bananas comprise of 60% pulp and 40% peel, with 7.25 kg of peel generated from an 18.14 kg banana box. These wastes create an unpleasant odor and release gases that contribute to the greenhouse impact if they are not properly treated (Alzate Acevedo et al. 2021). However, according to Syed Abu Bakar et al. (2018) banana peel consisted of dietary fiber. The dietary fiber can act as prebiotic that plays a function to promote probiotics growth and activity. To our best knowledge, there is

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no findings reported on incorporation of banana peel with encapsulated microbe in spray drying process. Therefore, this research aims to produce microencapsulated probiotic (LP) powder with incorporated BP. The microencapsulation process was performed using spray drying that used maltodextrin as encapsulant.

15.2 Methodology 15.2.1 Preparation for Lactobacillus Plantarum ATCC8014 Growth The Lactobacillus plantarum ATCC8014 was purchased from Microbiologics KwikStik. The MRS broth (Oxoid) was used to grow the probiotic at 37 °C for 24 h in the incubator shaker. After incubation, the cell was centrifuged at 3500 rpm for 15 min at 4 °C. The suspended cells were washed twice with sterile buffered peptone water (Oxoid).

15.2.2 Preparation of Banana Peel In this research, banana peel from Musa paradisiaca was used as a fiber and it was collected from a local company that produces banana chips at Alor Gajah, Melaka. The banana peel was washed and dried in a convection oven at 60 °C for 12 h. The dried peels were grinded, sieved (octagon digital with