GROUP 4

CHANG WEN QI | KHAIRUL ANWAR | SYAHIRA SYAELLA

CONTENTS ACKNOWLEDGEMENT OBJECTIVES INTRODUCTION EQUIPMENT AND INSTRUMENT IN IBD :1. LIQUID CHROMATOGRAPHY- MASS SPECTROMETRY (LC-MS)2. SOXHLET EXTRACTOR3. ROTARY EVAPORATOR4. SPRAY DRYER5. HIGH PRESSURE LOOP REACTOR6. MOLECULAR DISTILLATION7. HIGH PRESSURE REACTOR8. BIOREACTOR9. CENTRIFUGE10. TURBO EXTRACTOR LABORATORIES AND DEPARTMENTS VISIT1. COSMECEUTICAL & FRAGRANCES DEPARTMENT2. FOOD & NUTRACEUTICAL DEPARTMENTS3. FINE CHEMICAL PILOT PLANT CONCLUSION REFERENCE

ACKNOWLEDGEMENT

First of all, with consent from Allah, we were given a good health to attend the industrial trip to IBD, UTM. A special appreciation was expressed to our lecturers which are Mdm Nor Faizah Binti Razali, Dr Mazatusziha Binti Ahmad and Mdm Farhana Binti Mohd Hatta for willing to spend their time attending the trip with us. Furthermore, we would also like to express our special gratitude towards the director of Institute of Bioproduct Development of Universiti Teknologi Malaysia, Prof Ramlan Abdul Aziz who gave us permission to visit the institute. Special thanks goes to the staff involved which were Mr Muhammad Subri Bin Ab. Rahman, Mr Amran Bin Buang , Miss Nurul Liza , Miss Hikmah and other staff of Institute of Bioproduct Development who gave a lot of useful information to us about the machines and its uses. Last but not least, we would like to thank our classmates who involved in this industrial trip to Institute of Bioproduct Development , Universiti Teknologi Malaysia for their support.

OBJECTIVES:The purpose of this industrial visit is:1. To give exposure for the students to know the equipment and instruments use in industry related to Chemical Reaction Engineering, Separation Engineering Technology and other subjects.2. To know the function, operating condition and procedure to use all the equipment and instruments.3. To provide a better understanding of the theory learned in class with practical learning and "hands-on" in the industry. 4. To increase the level of knowledge and interest in the "Research and Development" Chemical Engineering Technology and Bioproduct development.

INTRODUCTION:Institute of Bioproduct Development (IBD) is a Centre of Excellence in University Teknologi Malaysia (UTM) focused on Research, Development and Commercialization of innovative bioproducts. It supports in developing high value components and processing technology for industries such as nutraceuticals, cosmeceuticals, phytochemicals, flavour and fragrance, food ingredients, probiotics, biofertilizers and biopesticides. IBD is equipped with multi-purpose facilities and handled by a group of highly skilled multi-disciplinary experienced personnels. Research is carried out in the laboratories that meet the international standard level and achieve ISO accreditation. IBD also serve its customers to develop bioproduct through a complete process. IBD has been officiated by the Honorable Prime Minister, Dato Seri Abdullah bin Haji Ahmad Badawi on 6 June 2005. The Vision: To be an innovative leader in bioproduct research and development The Mission: To develop innovative market driven bioproduct to promote and enhance wellness and healthy living from natural resources through sustainable process and creating wealth for the nation. Research Theme: Biotechnology for Wellness Industry. Objectives of IBDTo carry out Research & Business Development of bioproduct through innovative processes by:- Focusing on high end fundamental research with novelty and impactful publications. Providing and designing market driven bioproducts that benefits society and economy. Offering consultancy & contract research services through utilization of our Technological Platforms; Bioprocessing, Herbal & Pytochemical and Biovalidation. Utilizing semi industrial scale process equipment with flexibility support for Process & Product Development, Process Scaling Up, Plant Optimization & Troubleshooting.

To produce highly qualified human capital through Life Long Learning by :- Providing an extensive training in the level of Professional Short Courses & Certificate Level Programmes in the scope of Biotechnology, Herbal Industry, Holistic Therapy & Wellness Industry. Organizing courses related to Process & Plant Technology for Engineers and Plant Operators in an in-house mode scheme. Offering postgraduate programme in the level of Masters & PhD for biotechnology and plant technology sector.

EQUIPMENT AND INSTRUMENT IN IBD1. LIQUID CHROMATOGRAPHY- MASS SPECTROMETRY (LC-MS)LC-MS refers to the combination of liquid chromatographic separation (or HPLC) with mass spectrometric detection (MS). Liquid chromatography generally utilizes very small particles packed and operated at high pressure, referred to high performance liquid chromatography (HPLC). Modern LC-MS method used HPLC instrumentation to introduce samples. In HPLC the sample is forced by liquid at high pressure, known as mobile phase, through a column that is packed with stationary phase to accomplish particular types of separations. As for the mass spectrometer, it is a technique to measure the mass-to-charge ratio of charged particles. They work by ionizing chemical compounds to generate molecule fragments and measuring their mass-to-charge ratios. In MS procedure: A sample was introduced into MS instrument and undergoes vaporization. The components of sample are ionized and formed charged particles. The ions are separated according to their mass-to-charge ratio by electromagnetic field. The ions are detected and processed into mass spectra.The MS technique has both quantitative and qualitative uses. The use of LC-MS has been widely developed in pharmacokinetic studies of pharmaceuticals and thus the most frequently used technique in the field of bioanalysis. In IBD, the researchers have profiled lipids in coconut oil using ultra-high performance LC-MS. The lipid profiles of three different technique of processes such as integrated process, wet process (fermentation) and dry process (cold process) have been developed and compared using a software. The use of LC-MS have contributed to cosmeceutical and fragrance field especially in producing hair gel, hair cream, skin nutrient cream and lip balm. According to master students at IBD, LC-MS was used to extract galeic acid from traditional plants (belimbing dayak and kacip fatimah) as the acid can stop the growth of cancer cells. 2. SOXHLET EXTRACTORA soxhlet extractor is a laboratory apparatus for the extraction of lipids and other molecules from a solid sample. A soxhlet extraction apparatus is composed of a condenser, a soxhlet extractor, and round bottomed flask. It is a batch process and solid-liquid extraction process. When solid was introduced into the machine, the solute was extract from the solid. After that, the solute goes through rotary evaporator to obtain our desired product.

Principles of Soxhlet Extractor:A soxhlet extraction method is somewhat opposite from filtration in that the extraction of the sample is for an insoluble organic components in a solvent, unlike complete solubility of an organic component in a sample, which is suitable for just simple filtration. Therefore, a soxhlet extraction procedure allows a compound to be extracted from insoluble material using a chemical solvent. Application of Soxhlet Extractor Food testing Biofuels Environmental analysis of soils, sludge, and wastes.3. ROTARY EVAPORATORThe Rotary Evaporators is used mainly for the continuous distillation under reducing pressure the condition exchanging the volatile solvent in a large amount. Especially to the distillation of receiving the liquid at the time of concentration and chromatographic fractionation of aqueous extract, all right separation and purified reaction product. In this instrument, the process involved is liquid-liquid extraction, where we want to extract our desired product.

The Rotary Evaporators makes the flask under being most suitable for the speed through electronic control; the constant velocity is rotated in order to increase the evaporation area. Enable the evaporation flask under negative pressure through the vacuum pump. Evaporate flask, rotate, put into water bath pan at constant temperature heating at the same time, solution shoulder, depress in rotating flask going on, heating, spreading, and evaporating in the bottle. The evaporator system of the rotation can seal and reduce pressure to 400- 600torrs; Heat the solvent in the distillation flask by heating the bath, the heating temperature can be close to the boiling point of this solvent. In addition, under high-efficient cooler function, can liquefy the hot vapour rapidly, accelerate the evaporation rate. In IBD, the machine was used to extract essential oil. Essential oil was extracted from various herbs obtaining all around Malaysia such as black paper, kacip fatimah, ginger oil, mangosteen and many more. The oil was extracted and manufactured to form variety of useful product such as for medical purpose and cosmetic purpose.4. SPRAY DRYERSpray drying is a method of producing a dry powder from a liquid or slurry by rapidly drying with a hot gas. This is the preferred method of drying of many thermally-sensitive materials such as foods and pharmaceuticals

Capacity: 30 litre/hr 50 litre/hr 100 litre/hr

Operating Temperature: 300 to 450 oC

Firstly, the liquid feed is pumped through an atomiser device that produces fine droplets into the main drying chamber. The spray dryer is equipped with two type atomiser, two fluid nozzle and rotary atomizer. By using two fluid nozzles, compressed air is used to help atomizing where as in rotary atomizer the feed is atomized with the help of spinning wheel which rotate up to 30,000 rpm. Then the hot drying gas can be passed through the chamber meet the fine fed droplet. The water from the droplet wills evaporate and leaving the solid content in the form of powder. The powder and water vapour will then go to a cyclone separator in which the powder will be separated from the water vapour and hot air.

Spray drying is the most widely used industrial process involving particle formation and drying. The spray dryer at IBD is extensively used to process herbal extract. Almost all Malaysian popular herbs have been processed with success. The spray drying operation at IBD is located in clean room area. The procedure and installation meet the requirement of GMP. We can ensure that the products process is clean and hygienic.5. HIGH PRESSURE LOOP REACTORHigh Pressure Loop Reactor can operate either in continuous mode or batch mode. In batch mode the plant capacity is 80 kg/batch where as in continuous mode the capacity is up to 30 l/hr.

Operating Mode: Batch ContinuousCapacity: Batch: 80kg/batch Continuous: 20 to 30 litre/hrOperating Temperature: Up to 250oCOperating Pressure: Up to 40 bar

This high pressure loop reactor provides very rigorous mixing for reaction especially for liquid-gas mixing as well as liquid-liquid mixing. During the reaction gas are introduced via reaction mixer to create a well dispersed mixture that is injected at high velocity into an autoclave. This mixture is rapidly circulated by a special pump at high gas/liquid ratios throughout the volume of the loop and permits the maximum possible mass transfer rates. A heat exchanger in the external loop allows for independent optimisation of heat transfer. For continuous operation, product is separated by an in-line cross-flow filter which retains the suspended solid catalyst within the loop. The plant was design and built to comply with explosion proof environment and suitable to handle. The range of process reactions carried out in these plants include: Hydrogenations, Alkoxylations, Oxidations, Aminations, Reductive Aminations, Alkylations, Reductive Alkylations, Carbonylations, Chlorination, Dehydrogenation, Ethoxylations / Propoxylations, Nitrile synthesis, Phosgenations and many more.6. MOLECULAR DISTILLATION

Capacity: 35 kg/hrOperating Temperature: 210 oCOperating Pressure: 0.001 mbarNumber of stages: 3

Molecular distillation separate volatile from less volatile by utilizing the thin-film wiping action of feed liquid on inside wall of a heated cylindrical vacuum chamber. As the result the volatile will evaporates. The vapour will be condensed in separate condenser and the liquid will be drawn as heavy product or goes to the next stage. This process is an efficient thermal separation technique with minimum product decomposition and maximum product quality. The advantages of molecular distillation process include short residence time of the feed liquid, a significantly lowered temperature due to high vacuum capability, and optimal efficiency in mass and heat transfer. Therefore, this plant is suitable for processing heat sensitive of high value products.

The industries from the following field will benefit from this plant: Pharmaceutical, Biomaterial Concentration Molecular Distillations Of Esters, Fatty Acids, Mono, Di, & Triglycerides Vitamin, Nutraceutical, Essential Oil Isolation Wax Fractionation Oil Deodorization Water Removal ppm Level Food, Flavor Purification Solvent Recovery7. HIGH PRESSURE REACTORHigh pressure is a stirred tank reactor equipped with agitator. The reactor can be heated up to 250 C using thermal oil. The thermal oil unit is equipped with temperature control system to obtain precise operating temperature.

Capacity: 20 litre/hrOperating Pressure: Up to 40 barOperating Temperature: Up to 250 oC

8. BIOREACTORA bioreactor is any manufactured or engineered device that supports a biologically active environment. Bioreactor also vessel in which a chemical process is carried out which involves organisms or biochemically active substances derived from such organisms. This process can either be aerobic or anaerobic. These bioreactors are commonly cylindrical, ranging in size from litres to cubic metres, and are often made of stainless steel. It may also refer to a device or system meant to grow cells or tissues in the context of cell culture. These devices are being developed for use in tissue engineering or biochemical engineering. Biological resources include agriculture, forestry, and biologically-derived waste, and there are many other renewable bioresource examples. Other energy storage chemicals in plants include oils, waxes, fats, etc., and because these other plant compounds have distinct properties, they offer potential for a host of different bioproducts.

The Bioprocess Pilot Facility (BPF) is an integrated multi-purpose facility for fermentation, biotransformation and down-stream processing at Institute of Bioproduct Development (IBD). The facility is highly engineered and bioreactors are built according to cGMP standard. Bioreactors volumes are increased at equal geometry for optimum scale up. The facility has the ability to carry out bacterial fermentation ranging from 16L to 1500L. The facility is run by a skilled multidisciplinary team of engineers and technical support staff.

Bioreactor available in IBD, UTM 1500 L Bioreactor 150 L Bioreactor (2x) 16 L Bioreactor (7x)*come with automatic temperature, pH, CO2 and pO2 controller.Marmalian Cell Culture bioreactor.IBD have two type of cell culture bioreactor which are disposable bag type and CSTR type. All the bioreactors are equipped with all necessary control system and can be run with minimal human supervision. All the data are logged to computer system and can be viewed and manipulated later.All these facility is housed in cleaned room and equipped with all necessary equipment, such as low temperature freezer, bio safety cabinet, inverted microscope with camera and incubators.

9. CENTRIFUGE

A centrifuge is a piece of equipment, generally driven by an electric motor that puts an object in rotation around a fixed axis, applying a force perpendicular to the axis. A centrifuge is also used to separate the components of blood in blood banks. The centrifuge works using the sedimentation principle, where the centripetal acceleration causes denser substances to separate out along the radial direction. By the same token lighter objects will tend to move to the top.Centrifugation is a process by which a centrifuge is used to separate components of a complex mixture. By spinning laboratory samples at very high speeds, the components of a given mixture are subjected to centrifugal force, which causes more dense particles to migrate away from the axis of rotation and lighter ones to move toward it. These particles can sediment at the bottom of the tube into whats known as a pellet, and this isolated specimen, or the remaining solution, the supernatant, can be further processed or analysed.The principle component of a centrifuge is the rotor, which is the moving part that spins at high speeds. Many centrifuges will have a refrigeration unit that allows the internal temperature to be controlled during the spin. They also have knobs or buttons for inputting the parameters for each run, which can include the duration of the spin, the temperature, and the magnitude of the spin in terms of speed or relative force. Spin speed is measured as RPM, or revolutions per minute.

10. TURBO EXTRACTOR

Turbo extractor and distillation plant is useful to can extract essential oil from local herbs with high yield. The plant can utilize either hydro-extraction process or steam distillation extraction process. The plant is equipped with explosion proof motor suitable for solvent extraction process. The plant can accept wide variety or raw materials. Generally leafy raw materials can be processed as it is the other type such as rhizomes, tree root and barks need to be grounded to small size in order to make the process optimized. Special design agitator is installed in order to speed up the process. This two speed agitator can handle even hard raw materials.Capacity:30kg/batchFeed Type:All type of herbs Leaves Rhizomes Tree roots Tree barksExtraction Type: Hydro distillation Steam distillation Solvent distillation

One of the examples in the herbal and various other food preparation industries is when a vegetable matrix necessitates extraction for further processing, it is importance to ensure that a high degree of extraction efficiency is reached, that the extract is not oxidised. Many laboratory procedures require solid-liquid extraction as a preliminary phase of the preparation of a sample, for example as happens in the analysis of environmental contaminants in vegetables. The operation of solid-liquid extraction must guarantee that all the analytes are retrieved completely and that they are in no way degraded during the extraction process. The applications of Turbo Extractor are lycopene extractions from industrial tomato skin waste and the retrieval of essential oil from scraps of orange peel residue from candied peel production.

LABORATORIES & DEPARTMENTS VISIT

1. PICTURES AT COSMECEUTICAL & FRAGRANCES DEPARTMENT Briefing & explanation by Ms. Nurhikmah about research conducted by Cosmeceutical & Fragrances Department.Chemical, Instruments and Equipment in Cosmeceutical & Fragrances Lab.

Product of Cosmeceutical & Fragrances, IBD: Anti-Obesity Cream

Product of Cosmeceutical & Fragrances, IBD: Various of Essential Oils extracted from local flowers, herbs and leaves

Product of Cosmeceutical & Fragrances: Facial, Body & Hand Cosmetic (Lotion, Cleanser, Tonner)Product of Cosmeceutical & Fragrances:Royal Perfumes made by Zaffran Oil & Gaharu Oil

Raw Materials such as spices, herbs and dried flowers use in the research and development of Cosmetics and Perfumes.Among the National & International Award receive by the team of researcher.

2. PICTURES AT FOOD & NUTRACEUTICAL DEPARTMENTRaw materials used in the research to determine its nutrition contents for product developmentRaw materials used in the research to determine its nutrition contents for product development

The equipment used in the laboratory, Tintometer and Mass BalanceThe equipment used in the laboratory, Viscometer

Research product; Cocoa Butter

Research products such as PhytoPlus Tongkat Ali, Herbal Chocolate and others

An Award winning research; COGURT- diary free and highly nutritious yogurt from coconut.Display Rack in the Department to exhibits all the research products with information and the recognition that the researcher receive national and internationally.

3. PICTURES AT FINE CHEMICAL ENGINEERING PILOT PLANTEquipment that available in IBD Pilot PlantEquipment that available in IBD Pilot Plant

Equipment that available in IBD Pilot PlantScale up Rotary Evaporator for higher production

Dried Kaffir Lime leaves, Bark of Gaharu & Cendana to be feed into the extractor. Dried Pineapple powder after the juice being process by the spray dryer

CONCLUSION

IBD has been known as its speciality in contributing idea for research and development field in Malaysia. Through this trip, students had gained a lot of knowledge on analytical method and equipment used in industrial process. Process such as separation, distillation and extraction had been used mainly in extraction of essential oil from herbal plants and students have been exposed to the process itself. Not to forget through this trip students get to know the machine from staffs of IBD and their contribution not only to cosmetic field but also to medical field. The industrial visit also exposed students to learning process during industrial training. Besides, students learned the process or method used to produce large scale production of product such as batch process. In conclusion, the industrial visit has reached its objective to expose students towards machine and process unit works used in separation, biochemistry process and chemical reaction engineering. In addition, students get to observe the working environment in industry and the practical works used in industrial training.

SEPARATIONCHEMICAL REACTION ENGINEERINGANALYTICAL

Soxhlet Extractor Rotary Evaporator Spray Dryer Molecular Distillation Turbo Extractor Centrifuge High Pressure Reactor High Pressure Loop reactor Bioreactor Liquid Chromatography-Mass Spectrometry (LCMS)

REFERENCES1. Principle of rotary evaporatorFrom: http://ietinfo.com/info/201210/use-and-principle-of-the-rotary-evaporators.html (Retrieve on: 29 March 2014)

2. High Performance Liquid Chromatography (HPLC) From: http://www.chemguide.co.uk/analysis/chromatography/hplc.html (Retrieve on: 29 March 2014)

3. Liquid Chromatography Mass SpectrometryFrom: http://www.pharmacelsus.de/lcms/ (Retrieve on: 3 April 2014)

4. Liquid Chromatography Mass SpectrometryFrom: https://www.jic.ac.uk/services/metabolomics/topics/lcms/why.htm(Retrieve on: 3 April 2014)

5. About Institute of Bioproduct Development UTM From: http://www.newibd.utm.my/about/about-ibd/ (Retrieve on 3 April 2014)

6. Fine Chemical Engineering Pilot PlantFrom: http://www.newibd.utm.my/gallery/fine-chemical-pilot-plant-equiptment/ (Retrieve on: 3 April 2014)

7. Bioprocessing Pilot FacilityFrom: http://www.newibd.utm.my/rnd/bioprocessing-pilot-facility/ (Retrieve on 4 April 2014)

8. Food & Nutraceutical From: http://www.newibd.utm.my/rnd/department-of-research-inovation/food-nutraceuticals/ (Retrieve on 4 April 2014)

9. Gary D. Christian; Analytical Chemistry 6th Edition. Wiley International Publication, United State of America.

10. Christie J. Geankoplis Transport Process and Separation Process Principles. 4th Edition. Pearson-Prentice Hall Education Inc. New Jersey USA.

11. H. Scott Fogler. Elements of Chemical Reaction Engineering 4th Edition. Prentice Hall International Series. USA