INDUSTRIAL TRAINING REPORT Name : Mohamad Wishal Kurnia bin Azmy Programme : EH220 ID : 2018437792 LI Duration : 15/2/2021 until 23/4/2021 Supervisor : (Ms.) Rafiqqah binti Sabri Company Address : Lot 3147, Block 14, Jalan Sultan Tengah, 93055, Kuching, Sarawak Visiting Lecturer : PM DR. Kamariah ACKNOWLEDGEMENT In the name of Allah the most Beneficent and most Merciful, All praises to Allah, Lord of the universe and peace be upon His Messenger. I want to acknowledge Him on top of al for blessing me with patience and tenacity of mind to complete the internship report. It is undeniably a vital requirements for certified Bachelor Degree (Hons.) with flying colours and I have received outstanding helps from many quarters which I would like to put on record here with great pleasure and deep gratitude. I would humbly pay my gratitude and humble thanks to CRAUN’s management for my industrial training acceptance. It is definitely a special honour to be a part of the firm for 10 weeks. All the sense of concern towards me are tremendous and unforgettable from the staffs. It is a beautiful experience to engage with the prestige firm, therefore, the least I can hope is that my hard work and training can be the great epitome to a better application of Chemical Engineering course in the near future. Firstly, I would like to express my deep and sincere gratitude to my supervisor, (Ms) Rafiqqah binti Sabri for giving me the opportunity to acquire various analytical knowledge while providing invaluable guidance throughout this research. Without her endless efforts and wit, any progress and understanding would never be identified. Most thanks for her support, feedbacks and all the worthwhile lessons. I am also extending my heartfelt thanks to Dr. Nurleyna Yunus, Sir Peter, Mr. Shukri and others for their acceptance and patience in assisting me to perform the laboratory works. In addition, I would also want to express my gratitude to dear lecturers who guided me and other companions throughout the internship programme from the very beginning till its completion. Their expert lead, suggestion in class, and all the updating notices, had provided me relevant information in reaching the concept and objectives of this compulsory report. Surely, without such commitment and tolerance, I may not have finished any chapter efficiently. Last but not least, I dedicated this to my practical mates, I do appreciate all the helping hands they lend while I had loss the courage at certain point and they for sure had gathered me back into conscience effortlessly. Not to forget, I value all the contributions whose articles and publications play part in my working papers. I owe my indebtedness to all those authors which had been great use to me. They are very precious people that I couldn’t name personally. CONTENTS 1.0 INTRODUCTION…………………………………………………………………. 1 2.0 COMPANY DETAILS……………………………………………………………. 2 2.1 Company History……………………………………………………….. 2 2.2 Organizational Chart………………………………………………….. 2 2.3 Vision……………………………………………………………………. 2 2.4 Mission…………………………………………………………………… 2 2.5 R&D Thrust Areas……………………………………………………… 3 2.6 Industrial Training Supervisor…………………………………………. 3 FIELD OF STUDY……………………………………………………………….. 4 3.1 Volatile Fatty Acid (VFA) Analysis……………………………………. 4 3.2 Chemical Oxygen Demand (COD) Analysis……………………….. 7 3.3 TSVS and TSSVSS Analysis…………………………………………. 8 3.0 4.0 5.0 WEEKLY ACTIVITY……………………………………………………………… 11 4.1 Week 1…………………………………………………………………… 11 4.2 Week 2…………………………………………………………………… 11 4.3 Week 3…………………………………………………………………… 11 4.4 Week 4…………………………………………………………………… 12 4.5 Week 5…………………………………………………………………… 12 4.6 Week 6…………………………………………………………………… 12 4.7 Week 7…………………………………………………………………… 12 4.8 Week 8…………………………………………………………………… 13 4.9 Week 9…………………………………………………………………… 13 4.10 Week 10…………………………………………………………………. 13 CONCLUSION……………………………………………………………………. 14 1.0 INTRODUCTION This written industrial training report describes the internship performance of me, Mohamad Wishal Kurnia bin Azmy throughout my internship programme at respective CRAUN Research Sdn Bhd. The industrial training lasts for 10 weeks from 15th February 2021 to 23rd March 2021 and compulsory for any Bachelor Degree of Engineering (Hons.) Chemical undergraduate before completing the EH220 programme. Internship conducted are guided by Dr. Azrini. Industrial training is an important component in engineering curriculum. Theories learnt in the entire core and non-core courses will have to be applied into the real working environment in engineering industries, specifically to get them involved in chemical and relevant engineering projects. Prior to the actual training in industries students are required to make job applications before stepping into the real working environment. Minimum industrial training duration is 10 weeks with 5 credit hours. The purpose of this program is to fulfil the course in order to complete the Bachelor Degree as well as graduate from the college. The training refers to work experience that is relevant to professional development prior to graduate. It also to provide real-world experience that enables me to apply every knowledge learnt into action. In total, it is the phase of time for students when they are trained for their skill and allow them to apply and perform practical experimentation in industries. In all courses, there will definitely be objectives and target to achieve. First of all, internship students are expected to practice basic engineering or research activities, including technical writing and project management. Besides that, demonstrate the effective communication with fellow workers and supervisors on issues related to given project. Lastly, students are expected to practice higher level of integrity, ethical and accountability in practicing engineering. Throughout my internship programme, I have definitely acquired various knowledges while developing interpersonal and communication skills in performing distinct analysis. This includes learning different theoretical and experimental knowledge to different scope of project, which is Volatile Fatty Acid (VFA) analysis, Chemical Oxygen Demand (COD) analysis, Total Solid Volatile Solid (TSVS) analysis, Total Suspended Solid Volatile Suspended Solid (TSSVSS) analysis as well as Total Starch Content (TS) analysis. In regards to knowledges on the procedure, I have acquired several instrumentation measure and safety precautions needed to be taken while performing different lab works. This is to ensure that any instrumentation and major operating unit belong to the organization are well taken care of. Precision and persistent can always be ensured when each of the steps from preparing up until apparatus cleaning are conducted in a well manner. All in all, it is definitely tremendous experience and honour to be a part of the CRAUN Research Sdn Bhd organization. 1|Page 2.0 COMPANY DETAILS 2.1 Company History CRAUN was established on 22nd July 1993 by the Sarawak State Government. Upon the approval of the Sarawak State Government on 1st April 1997, CRAUN was corporatized and known as CRAUN Research Sdn Bhd. CRAUN began its operations at the Food Technology Research Laboratories of the Malaysian Agriculture Research and Development Institute (MARDI), Sarawak Branch on 15th February 1994. On 1st July 1994, the Farm Management & By-Product Utilisation Section of CRAUN began its operation at the 1st and 2nd floor, Lot 500, Block 68, Mukah New Township, Mukah and on 17th September 1994 Sungai Talau Research Station of the Agriculture Department Sarawak, was taken over by CRAUN. However, the overall operation of CRAUN Mukah Office has been sited to Sungai Talau Research Station since August 2011. CRAUN’s headquarters at Lot 3147, Block 14, Jalan Sultan Tengah, Kuching, occupying approximately seven acres, commenced construction on 17 th November 1994 and began its operations on 11th September 1995. By virtue of the Sarawak Gazette Part II dated 22nd May 2017, CRAUN Research Sdn Bhd is an agency placed under the Ministry of Education, Science and Technological Research and Biotechnological Council. 2.2 Organizational Chart Figure 1: CRAUN’s organizational chart 2.3 Vision Be at the Forefront on Crops & Products Research and Innovation Focusing on Sago. 2.4 Mission Advance in Sago Industry through Effective Research and Innovation 2|Page 2.5 R&D Thrust Areas 1) Crop improvement for high yield, good quality starch and maturity palms. 2) Mass propagation for production of high quality planting materials. 3) Understanding peat characteristics, reclamation and management techniques for optimum sago growth. 4) Agronomic and cultural practices. 5) Field mechanisation and post-harvest handling. 6) Milling technology. 7) By-product utilisation. 8) Product development. 9) Market studies, innovation and commercialisation. 2.6 Industrial Training Supervisor Name : Rafiqqah binti Mohd Sabri Position : Research Officer Department : Downstream Technology Division Lab : 2 Telephone No : (+60)19-5407616 Email : rafiqqah@gmail.com Highest level of education : Master of science (MSc) 3|Page 3.0 FIELD OF STUDY 3.1 Volatile Fatty Acid (VFA) Analysis 3.1.1 Background Biogas platform producing methane gas from wastes through an anaerobic digestion (AD) process exploits rapid acidogenesis and slow methanogenesis. The acidogenesis stage is the production step of volatile fatty acids (VFAs), which are short-chain fatty acids composed mainly of acetate and butyrate and are rapidly produced from nonwoody biomass by the natural consortia of mixed anaerobic bacteria. The AD process, which converts all parts of biomass (carbohydrates, lipids and proteins) except for lignin to VFAs, is suitable for organic waste treatment and does not need a high cost pre-treatment step or additional hydrolysis enzymes. 3.1.2 Anaerobic digestion Initially employed mainly for food and beverage production, anaerobic conversions are among the oldest biological process technologies utilized by mankind. They have been applied and developed over many centuries, although the most dramatic advances have been achieved in the last few decades with the introduction of various forms of high-rate treatment processes, particularly for industrial wastewater. AD involves a transformation of organic matter by a mixed culture bacterial ecosystem without oxygen. It is a natural process that produces a gas principally composed of methane and carbon dioxide. The first step of AD is the hydrolysis of animal or plant matter. This step breaks down biopolymers and other organic material to smaller molecules: Lipids → Fatty acids Polysaccharides → Monosaccharides Protein → Amino acids Nucleic acids → Purines and pyrimidines The second step is the conversion, by acetogenic bacteria, of products of the first step to organic acids, carbon dioxide and hydrogen. Acetogenic bacteria produce acetic acid; however other organic acids are also produced. The principal organic acids produced are acetic acid, propionic acid and butyric acid. Ethanol and other products are also produced. The final step is methanogenesis. Methane and carbon dioxide are produced from acetate, ethanol and other intermediates. The advantage of this method is that it couples the treatment of waste with energy production (methane). Reactor acidification through reactor overload is one of the common reasons for process deterioration in anaerobic digester. This occurs because of a build-up of volatile fatty acids (VFAs) which are produced by acidogenic and acetogenic bacteria, and reflects a kinetic uncoupling between the acid producers and consumers. High VFA concentrations cause pH values to decrease, and result in toxic conditions in the reactor. 4|Page 3.1.3 Instrumentation VFA analysis forms an important means of assessing the effectiveness of the digestion process within a wastewater treatment plant. The analysis of VFA concentrations and their changes on a regular basis allows early detection and diagnosis of anaerobic digester process upset. Volatile fatty acids can be identified by titration, distillation, steam distillation and chromatography. In our lab analysis, we used a Gas Chromatography (GC) coupled with Mass Spectrometry (MS) to perform and evaluate the VFA content. FIGURE 1: Gas-Chromatography Mass Spectrometry (GC-MS) It is a two instrumental method of scientific analysis. On the other hand, when used concurrently, it eventually able to separate out the individual components of a mixture. Its objective is to tell what does a substance composed of. Gas Chromatograph comprises of a heated inlet port, oven, and a fused silica column (essentially a coiled glass tube) which has been coated with a special material called the stationary phase. It produces a graph called chromatogram, where each separated substance is represented by a peak. The output is a plot of detector signal abundance versus time. Working principle involves in a gas chromatograph (GC) involves 4 separates stages; sample preparation, vaporization, separation and detection. First of all, samples are generally dissolved or diluted in a solvent before injected onto the inlet port. Other methods include solid phase extraction (SPE) and derivatisation may also be required. Next, liquid sample is vaporized in the hot inlet and becomes a gas. Mobile phase (inert gas i.e., helium) carries the sample through the column. Different substances interact differently with the column’s stationary phase (depend on their chemistry). It causes them to travel through the column at different speeds and eventually enables them to separate. The separated compounds leave the column one after the other, and enter a detector (MS). The time taken for a compound to travel through the column is called its retention time. In chromatogram, the number of peaks shows the number of separated compounds in the sample. The position of each peak shows the retention time for each compound. 5|Page MS, on the other hand is commonly used as a GC detector. First, MS will break each separated compound coming from the GC into ionized fragments. A high energy beam of electrons is passed through the sample molecule. It produces electrically charged particles or ions and fragments can be large or small pieces of the original molecule. Each charged fragments will have a certain mass and mass of the fragment divided by the charge is called the mass to charge ratio (m/z). Second, the fragments go through a process of acceleration and deflection whilst travelling through a short tunnel while exposed to a magnetic field. It eventually hit a detection plate at the end of the tunnel. Mass to charge ratio and relative abundance is calculated. It produces a graph called mass spectrum which shows the signal intensity or abundance of each detected fragment’s mass to charge ratio. Mass spectrum produced by a given chemical compound is the same every time it is analysed. It can be considered a fingerprint for the molecule. It allows the compound to be identified. In total, it acts as a recording of the masses of each of the ionized fragments, representing a unique fingerprint of a molecule that can be used in identification. 3.1.4 Sample preparation procedure 1) Collect samples. 2) Transfer the samples into microcentrifuge tube. 3) Centrifuge the sample at 1400 RPM for 2 minutes. 4) Filter them by using a syringe filter. 5) Place the sample in a vial. 6) Arranged vials in GC accordingly. 3.1.5 Lab analysis FIGURE 2: Experimental procedure 6|Page 3.2 Chemical Oxygen Demand (COD) Analysis 3.2.1 Background Chemical Oxygen Demand (COD) is a quick, inexpensive means to determine organics in water. COD samples are prepared with a closed-reflux digestion followed by analysis. It also determines the amount of oxygen required for chemical oxidation of organic matter using a strong chemical oxidant, such as potassium dichromate under reflux conditions. This test is widely used to determine the degree of pollution in water bodies and their self-purification capacity, efficiency of treatment plants, pollution loads, and provides rough idea of biochemical oxygen demand (BOD) which can be used to determine sample volume for BOD estimation. 3.2.2 Working principle The limitation of the test lies in its inability to differentiate between the biologically oxidizable and biologically inert material and to find out the system rate constant of aerobic biological stabilization. Most of the organic matters are destroyed when boiled with a mixture of potassium dichromate and sulphuric acid producing carbon dioxide and water. The amount of dichromate consumed is proportional to the oxygen required to oxidize the oxidizable organic matter. During the digestion the sample’s organic carbon (c) material is oxidized with the hexavalent dichromate ion (Cr2O72-) found in potassium dichromate (K2Cr2O7). The dichromate readily gives up oxygen (O2) to bond with carbon atoms to create carbon dioxide (CO 2). The oxygen transaction from Cr2O72- to CO2 reduces the hexavalent Cr2O72- ion to the trivalent Cr3+ ion. In essence a COD test determines the amount of carbon based materials by measuring the amount of oxygen the sample will react with. This oxygen transaction is the source of the test’s name, Chemical Oxygen Demand. 3.2.3 Procedure 1) Wash the tubes and caps with 20% H2SO4 before first use to prevent contamination. 2) By using concept of dilution factor, an amount of sample with water will be pipetted into the test tubes. 3) Mercury sulphate solution will be added into the test tubes followed by sulphuric acid solution. 4) Digest in preheated block digester at 150oC for 2 hours. 5) After the samples has cooled down to room temperature, proceed to UV spectrophotometer. 6) Record and analyse the COD content. 7|Page 3.2.4 Lab analysis FIGURE 3: Experimental procedure 3.3 TSVS and TSSVSS Analysis 3.3.1 Terms and definition 1) Total solids (TS) : The residue remaining after a wastewater sample has been evaporated and dried at a specified temperature (103oC to 105oC) 2) Total volatile solids (TVS) : Those solids that can be volatilized and burned off when the TS are ignited (500 ± 50oC) 3) Total fixed solids (TFS) : The residue that remains after TS are ignited (500 ± 50oC) 4) Total suspended solids (TSS) : Portion of the TS retained on a filter with a specified pore size, measured after being dried at a specified temperature (105 oC). The filter used most commonly for the determination of TSS is the Whatman glass fibre filter, which has a nominal pore size of about 1.58µm 5) Volatile suspended solids (VSS) : Those solids that can be volatilized and burned off when the TSS are ignited (500 ± 50oC) 6) Fixed suspended solids : The residue that remains after TSS are ignited (500 ± 50oC) 8|Page Total dissolved solids (TDS = TS- : TSS) Those solids that pass through the filter, and are then evaporated and dried at specified temperature. It should be noted that what is measured as TDS is comprised of colloidal and dissolved solids. Colloids are typically in the size range from 0.001 to 1µm 7) Total volatile dissolved solids (VDS) : Those solids that can be volatilized and burned off when the TDS are ignited (500 ± 50oC) 8) Fixed dissolved solids (FDS) : The residue that remains after TDS are ignited (500 ± 50oC) 9) Settleable solids : Suspended solids, expressed as millilitres per litre, that will settle out of suspension within a specified period of time. 3.3.2 Procedure 3.3.2.1 TSVS analysis 1) Weigh the empty crucibles. 2) Transfer a volume of sample into the crucible. 3) Place the sample in a drying oven at 103oC overnight. 4) Collect the samples and transfer into desiccator 45 minutes. 5) Weight the crucible and regards them as dried crucibles. 6) Place the crucible into furnace overnight. 7) Collect the samples and transfer into desiccator for 45 minutes. 8) Weigh the crucible and regards them as ash crucibles. 9) Records all the data and analyse. 3.3.2.2 TSSVSS analysis 1) Weigh the empty crucibles. 2) Pipette the samples onto the microfibre filter. 3) Transfer the filter into the empty crucible. 4) Place the sample in a drying oven at 103oC overnight. 5) Collect the samples and transfer into desiccator 45 minutes. 6) Weight the crucible and regards them as dried crucibles. 7) Place the crucible into furnace overnight. 8) Collect the samples and transfer into desiccator for 45 minutes. 9) Weigh the crucible and regards them as ash crucibles. 10) Records all the data and analyse. 9|Page 3.3.3 Lab analysis 3.3.3.1 TSVS analysis FIGURE 4: Experimental procedure 3.3.3.2 TSSVSS analysis FIGURE 5: Experimental procedure 10 | P a g e 4.0 WEEKLY ACTIVITY 4.1 Week 1 Date: 15th February 2021 until 19th February 2021 ❖ General briefing on rules and regulations by (Mdm.) Rumaizah binti Pathi, CRAUN Research’s Administrative Officer ❖ Briefing on Downstream Technology Division by Dr. Nurleyna Yunus, Head of DTD. ❖ Explanation on scope of work by supervisor, (Ms.) Rafiqqah binti Sabri ❖ Conduct an initial theoretical studies on Gas-Chromatography Mass Spectrometry (GC-MS). ❖ Present current findings on GC-MS to the supervisor. 4.2 Week 2 Date: 22nd February 2021 until 26th February 2021 ❖ Study on the theoretical serial dilution and its application on preparing new solution with distinct concentration. ❖ Record and analyse previous data on Total Solid Volatile Solid (TSVS) and Total Suspended Solid and Volatile Suspended Solid (TSSVSS). ❖ Study the correct steps for GC-MS records and documentation at software and logbook. ❖ Prepare the stock solutions. ❖ Prepare all levels (Level 1 to Level 7). ❖ Run samples and solutions for calibration analysis. 4.3 Week 3 Date: 1st March 2021 until 5th March 2021 ❖ Conduct research studies on mixer tank’s possible arrangement and dimension. ❖ Present the proposed design to supervisor. ❖ Conduct sample preparation for GC-MS calibration. ❖ Analyse the sample by GC-MS on the chromatogram produced. ❖ Replace a component in the GC-MS equipment. 11 | P a g e 4.4 Week 4 Date: 8th March 2021 until 12th March 2021 ❖ Learn on the fundamentals of Chemical Oxygen Demand (COD) preparation. ❖ Conduct experimental Chemical Oxygen Demand (COD) analysis. ❖ Prepare all levels (Level 1 to Level 7). ❖ Conduct GC-MS experimental analysis on the said prepared solution. 4.5 Week 5 Date: 15th March 2021 until 19th March 2021 ❖ Perform calibration for VFA analysis on all chemical component from previous stock preparation. ❖ From the VFA calibration, record and conclude the parameter necessary for improvement of re-calibration. ❖ Perform new calibration for COD analysis. ❖ Prepare new sample for VFA calibration. ❖ Conduct GC-MS experimental analysis on the said preparation. ❖ Record and analyse chromatogram generated from GC-MS. 4.6 Week 6 Date: 22nd March 2021 until 26th March 2021 ❖ Conduct an experiment to TSVS and TSSVSS at different samples ❖ Collect pH readings for each of the sample. ❖ Record all data pertaining to the samples’ readings for analysis. ❖ Conduct GC-MS experimental analysis on the said preparation. 4.7 Week 7 Date: 29th March 2021 until 2nd April 2021 ❖ Perform Chemical Oxygen Demand (COD) analysis on new sample ❖ Record and analyse the absorbance value for each of the sample ❖ Weigh dried TSVS and TSSVSS by using a laboratory weighing machine. ❖ Record the weigh and calculate the Volatile Solid (VS) and Volatile Suspended Solid (VSS). ❖ Prepare new 20% Sulphuric Acid solution. 12 | P a g e 4.8 Week 8 Date: 5th April 2021 until 9th April 2021 ❖ Learn and perform Total Starch Analysis on various samples. ❖ Prepare presentation slides for industrial training evaluator. ❖ Seek for supervisor’s approval on prepared presentation slides. 4.9 Week 9 Date: 12th April 2021 until 16th April 2021 ❖ Prepare empty crucible by placing them in a furnace before weigh. ❖ Prepare slides for presentation. ❖ Internship presentation with respective supervisor in mini conference room. ❖ Perform calibration on pH meter. ❖ Perform calibration on GC-MS from level 1 to level 7. ❖ Perform COD analysis. ❖ Record and analyse the absorbance value. 4.10 Week 10 Date: 19th April 2021 until 23rd April 2021 ❖ Prepare standard calibration for COD. ❖ Prepare buffer solutions for Total Starch (TS) content analysis. ❖ Prepare sulphuric acid reagent for COD analysis. ❖ Run COD analysis on new calibrated reagent solutions. ❖ Record and analyse readings of absorbance. ❖ Perform VFA analysis on two level. 13 | P a g e 5.0 CONCLUSION In total, this internship has been an excellent and rewarding experience. I can conclude that there have been a lot I’ve learnt from my work at CRAUN Research Sdn Bhd. Asides from analytical procedure and critical thinking, I have definitely gained several values that could enhance me to be a better individual. Throughout the industrial training, I found that several things are crucial: Discipline Discipline is important for smooth and trouble-free operation in all workplaces. However, in laboratory, it is highly significant considering the presence of toxic and hazardous materials and nature of operations that are routinely carried out. Safety in the laboratory is an important concern. Carelessness is often the cause of questionable results and accidents in laboratories but there is a clear demarcation between careless and discipline. All in all, disciplined conduct is an essential requirement in laboratories. Time management Time management is the strategy of planning out available time and controlling the amount of time spend on specific tasks in order to work more efficiently. Without strong time management, works and lab analysis can lead to poor quality of work, missing deadlines, increase personal stress levels, ruining work-life balance and harming professional reputations. I am able to have a glimpse of idea of every analysis that need to be accomplish while determining the duration needed for each of them. It can also help me focus on just the essential task and avoid time-consuming distractions. Monotasking The ability to juggle multiple projects or tasks at one time has long been considered a virtue. While multitasking can be a key skill at times, it also can result in substantial inefficiency. Given that most tasks in the clinical lab require focus and concentration, switching from task to task often necessitates significantly more time to refocus and engage with new tasks. Alternatively, monotasking, or creating focused blocks of time for a single task or project, can be more efficient. Interpersonal communication Interpersonal communication is the process of exchange of information, ideas and feelings between two or more people through verbal or non-verbal methods. Interpersonal communication is crucial for career development and productivity in the workplace. On the other hand, it allows me and other respected supervisor to discuss problems and weigh the pros and cons of alternatives before coming up with final solution. 14 | P a g e