Laboratory of biofuels

Contact:
Timo Kikas
Tel.: +372 731 3163
e-mail: timo.kikas@emu.ee

Address:
Chair of Biosystems Engineering

Institute of Forestry and Engineering

Estonian University of Life Sciences
56 Fr. R. Kreutzwald Str.
51006 Tartu, ESTONIA

Our People:

Timo Kikas, PhD Chair Professor, Biosystems Engineering	Merlin Raud, PhD Researcher, Bioenergy and Biofuels	Lisandra Meneses, PhD Senior Researcher	Tharaka Rama Krishna Chowdary Doddapaneni, PhD Marie Curie Research Fellow

Sabarathinam Shanmugam, PhD Postdoctoral Fellow	Renu Geetha Bai, PhD Postdoctoral Fellow	Vahur Rooni, PhD Research Fellow	' Lara Podkuiko, MSc Doctoral student

Margareta Novian Cahyanti, MSc Doctoral Student, Junior Research Fellow	Nikki Sjulander, MSc Doctoral student, Junior Research Fellow	Sharib Khan, MSc Doctoral Student, Junior Research Fellow	Salini Chandrasekharan Nair, MSc Doctoral Student, Junior Research Fellow

Anjana Hari, MSc Doctoral Student,	Damaris Okafor, MSc Doctoral student	Kaie Ritslaid, BSc (science) Lecturer/Analyst

Main Research Fields: Process and production technology of bioethanol production, incl. pretreatment methodology Effective utilisation of biomass for production of different biofuels Utilisation of waste from wood and paper industries for production of biofuels Cultivation of microalgae and design and construction of photobioreactors Study of biosensors and sensor arrays for fast measurements of biochemical oxygen demand (BOD) Development of nanomaterials and nanocomposites for water remediation, sustainable energy and biomedical applications
Reсent Publications: (last 5 years) Rocha-Meneses, Lisandra; Zannerni, Rawan; Inayat, Abrar; Abdallah, Mohamed; Shanableh, Abdallah; Ghenai, Chaouki; Kamil, Mohammed; Kikas, Timo (2022). Current progress in anaerobic digestion reactors and parameters optimization. Biomass Conversion and Biorefinery. DOI: 10.1007/s13399-021-02224-z. Hasanov, Isa; Shanmugam, Sabarathinam; Kikas, Timo (2022). Extraction and isolation of lignin from ash tree (Fraxinus exselsior) with protic ionic liquids (PILs). Chemosphere, 290, 133297. DOI: 10.1016/j.chemosphere.2021.133297. Doddapaneni, Tharaka Rama Krishna C.; Ahmad; Fiaz; Valgepea, Kaspar; Kikas, Timo (2022). Integrated thermochemical and biochemical processes for the production of biofuels and biochemicals. In: Biomass, Biofuels, Biochemicals (67−105). Elsevier. DOI: 10.1016/B978-0-323-89855-3.00025-X. Krishna C. Doddapaneni, Tharaka Rama; Kikas, Timo (2021). Chapter 39 - Thermochemical and biochemical treatment strategies for resource recovery from agri-food industry wastes. In: Bhat, Rajeev (Ed.). Valorization of Agri-Food Wastes and By-Products. Recent Trends, Innovations and Sustainability Challenges (787−807). Academic Press. DOI: 10.1016/B978-0-12-824044-1.00007-6. Cahyanti, Margareta Novian; Doddapaneni, Tharaka Rama Krishna C.; Madissoo, Marten; Pärn, Linnar; Virro, Indrek; Kikas, Timo (2021). Torrefaction of Agricultural and Wood Waste: Comparative Analysis of Selected Fuel Characteristics. Energies, 14 (10), 2774. DOI: 10.3390/en14102774. Aghmashhadi, O.Y.; Rocha-Meneses, L.; Bonturi, N.; Orupõld, K.; Asadpour, G.; Garmaroody, E.R.; Zabihzadeh, M.; Kikas, T. Effect of Ink and Pretreatment Conditions on Bioethanol and Biomethane Yields from Waste Banknote Paper. Polymers 2021, 13, 239. https://doi.org/10.3390/polym13020239. Rooni, V.; Sjulander, N.; Cristobal-Sarramian, A.; Raud, M.; Rocha-Meneses, Lisandra; Kikas, T. (2021). The efficiency of nitrogen explosion pretreatment on common aspen – Populus tremula: N2- VS steam explosion. Energy, Art No 119741. DOI: 10.1016/j.energy.2020.119741. Aghmashhadi, Omid Yazdani; Asadpour, Ghasem; Garmaroody, Esmaeil Rasooly; Zabihzadeh, Majid; Rocha-Meneses, Lisandra; Kikas, Timo (2020). The Effect of Deinking Process on Bioethanol Production from Waste Banknote Paper. Processes, 8 (12), 1563. DOI: 10.3390/pr8121563. Podkuiko, Lara; Kasemets, Mari-Liis; Lips, Inga; Kikas, Timo (2020). Cultivation of Algae Polyculture in Municipal Wastewater with CO2 Supply. Environmental and Climate Technologies , 24 (3), 188−200. DOI: 10.2478/rtuect-2020-0096. Pitman, Kätlin; Nerut, Jaak; Raud, Merlin; Kikas, Timo (2020). Characterisation of Electrochemical Sensor-Array for Utilisation in Construction of BOD Bioelectronic Tongue. Environmental and Climate Technologies , 24 (3), 39−54. DOI: 10.2478/rtuect-2020-0084. Doddapaneni, Tharaka Rama Krishna Chowdary; Kikas, Timo (2020). Integrating Biomass Pyrolysis with Microbial Conversion Processes to Produce Biofuels and Biochemicals. In: Fang, Zhen; Smith, Richard L.; Xu, Lujiang (Ed.). Production of Biofuels and Chemicals with Pyrolysis (1−447). Singapore: Springer Singapore. (Biofuels and Biorefineries; 10).10.1007/978-981-15-2732-6_9 Raud, M.; Orupõld, K.; Rocha-Meneses, L.; Rooni, V.; Träss, O.; Kikas, T (2020). Biomass Pretreatment with the Szego Mill™ for Bioethanol and Biogas Production. Processes, 8, 1327.10.3390/pr8101327. Sjulander, Nikki; Kikas, Timo (2020). Origin, Impact and Control of Lignocellulosic Inhibitors in Bioethanol Production—A Review. Energies, 13 (18), 4751.10.3390/en13184751 Hasanov, Isa; Raud, Merlin; Kikas, Timo (2020). The Role of Ionic Liquids in the Lignin Separation from Lignocellulosic Biomass. Energies, 13 (4864), 1−24.10.3390/en13184864 Raud, Merlin; Kikas, Timo (2020). Perennial Grasses as a Substrate for Bioethanol Production. Environmental and Climate Technologies , 24 (2), 32−40.10.2478/rtuect-2020-0052 Rocha-Meneses, Lisandra; Harris, Peter; Tait, Stephan; Antille, Diogenes L.; Kikas, Timo; McCabe, Bernadette K. (2020). Bioresource recovery in the Australian red meat processing industry: a technical review of strategies for increased circularity. 2020 ASABE Annual International Virtual Meeting, July 13-15, 2020. American Society of Agricultural and Biological Engineers (ASABE), 3−30.10.13031/aim.202000690 Rocha-Meneses, Lisandra; A. Ferreira, Jorge; Mushtaq, Maryam; Karimi, Sajjad; Orupõld, Kaja; Kikas, Timo (2020). Genetic modification of cereal plants: A strategy to enhance bioethanol yields from agricultural waste. Industrial Crops and Products, 150 (C), 112408.10.1016/j.indcrop.2020.112408 Cahyanti, Margareta Novian; Doddapaneni, Tharaka Rama Krishna C.; Kikas, Timo (2020). Biomass torrefaction: An overview on process parameters, economic and environmental aspects and recent advancements. Bioresource Technology, 122737.10.1016/j.biortech.2020.122737 Rocha-Meneses, Lisandra; Otor, Oghenetejiri Frances; Bonturi, Nemailla; Orupõld, Kaja; Kikas, Timo (2020). Bioenergy Yields from Sequential Bioethanol and Biomethane Production: An Optimized Process Flow. Sustainability, 12 (1), 272.10.3390/su12010272 Rauwel, Erwan; Al-Arag; Siham; Salehi, Hamideh; Amorim, Carlos O.; Cuisinier, Frédéric; Guha, Mihu; S. Rosario, Maria; Rauwel, Protima (2020). Assessing Cobalt Metal Nanoparticles uptake by Cancer Cells using Live Raman Spectroscopy. International Journal of Nanomedicine, 15, 7051−7062.10.2147/IJN.S258060 Rauwel, Protima; Rauwel, Erwan (2019). Towards the extraction of radioactive Cesium-137 from water via graphene/CNT and nanostructured Prussian blue hybrid nanocomposites: A Review. Nanomaterials, 9 (6), 682.10.3390/nano9050682 Rauwel, Protima; Ducroquet, Frédérique; Galeckas, Augustinas; Rauwel, Erwan (2019). Selective photocurrent generation in HfO2 and carbon nanotube hybrid nanocomposites under Ultra-Violet and visible photoexcitations. Materials Letters, 1.10.1016/j.matlet.2019.03.030 Raud, M.; Kikas, T.; Sippula, O.; Shurpali, N. J. (2019). Potentials and challenges in lignocellulosic biofuel production technology Renewable and Sustainable Energy Reviews, 111, 44−56.10.1016/j.rser.2019.05.020. Raud, M.; Krennhuber, K.; Jäger, A.; Kikas, T. (2019). Nitrogen explosive decompression pre-treatment: an alternative to steam explosion. Energy, 177, 175−182.10.1016/j.energy.2019.04.071. Rocha-Meneses, Lisandra; Raud, Merlin; Orupõld, Kaja; Kikas, Timo (2019). Potential of bioethanol production-waste for methane recovery. Energy, 173, 133−139.10.1016/j.energy.2019.02.073. Rocha-Meneses, Lisandra; Ferreira, Jorge A; Bonturi, Nemailla; Orupõld, Kaja; Kikas, Timo (2019). Enhancing Bioenergy Yields from Sequential Bioethanol and Biomethane Production by Means of Solid–Liquid Separation of the Substrates. Energies, 12 (19), 3683.10.3390/en12193683. Rocha-Meneses, Lisandra; Bergamo, Thaísa Fernandes; Kikas, Timo (2019). Potential of cereal-based agricultural residues available for bioenergy production. Data in Brief, 23, 103829.10.1016/j.dib.2019.103829. Rocha-Meneses, Lisandra; Silva, Jose Carlos; Cota, Sandra; Kikas, Timo (2019). Thermodynamic, Environmental and Economic Simulation of an Organic Rankine Cycle (ORC) for Waste Heat Recovery: Terceira Island Case Study. Environmental and Climate Technologies, 23 (2), 347−365.10.2478/rtuect-2019-0073. Raud, Merlin; Rooni, Vahur; Kikas, Timo; (2018). Explosive decompression pretreatment - nitrogen or flue gas? European Biomass Conference and Exhibition Proceedings, 2018: 26th European Biomass Conference, 14-17 May 2018, Copenhagen, Denmark. ETA-Florence Renewable Energies, 973 −978.10.5071/26thEUBCE2018-3CO.7.1. Raud, Merlin; Rooni, Vahur; Kikas, Timo (2018). The Efficiency of Nitrogen and Flue Gas as Operating Gases in Explosive Decompression Pretreatment. Energies, 11 (2074).10.3390/en11082074. Rocha-Meneses, Lisandra; Ivanova, Anastasia; Atouguia, Guilherme; Ávila, Isaac; Raud, Merlin; Orupõld, Kaja; Kikas, Timo (2019). The effect of flue gas explosive decompression pretreatment on methane recovery from bioethanol production waste. Industrial Crops And Products, 127, 66−72.10.1016/j.indcrop.2018.10.057. Raud, Merlin; Kikas, Timo; Sippula, Olli; Shurpali, Narasinha (2018). Potential and challenges in lignocellulosic biofuel production technology. Renewable and Sustainable Energy Developments Beyond 2030. Proceedings of the 11th International Conference on Sustainable Energy & Environmental Protection, 2, 115−120. Podkuiko, L.; Olt, J.; Kikas, T. (2017). Growth of Scenedesmus obliquus under artificial flue gas with a high sulphur concentration neutralized with oil shale ash. Proceedings of the Estonian Academy of Sciences, 66(2), 151−158.10.3176/proc.2017.2.03. Rooni, Vahur; Raud, Merlin; Kikas, Timo (2017). The Freezing Pre-Treatment of Lignocellulosic Material: A Cheap Alternative for Nordic Countries. Energy, 139, 1−7.10.1016/j.energy.2017.07.146. Raud, Merlin; Mitt, Marion; Oja, Tõnu; Olt, Jüri; Orupõld, Kaja; Kikas, Timo (2017). Utilization potential of urban greening waste: Tartu case-study. Urban Forestry and Urban Greening, 21, 96−101.10.1016/j.ufug.2016.11.014. Pitman, Kätlin; Raud, Merlin; Scotti, Gianmario; Jokinen, Ville P.; Franssila, Sami; Nerut, Jaak; Lust, Enn; Kikas, Timo (2017). Electrochemical Characterization of the Microfabricated Electrochemical Sensor-Array system. Electroanalysis, 29, 249−258.10.1002/elan.201600559. Pitman, K.; Nerut, J.; Lust, E.; Franssila, S.; Raud, M.; Kikas, T. (2017). Electrooxidation of Hexacyanoferrate(II) Anions and Electroreduction of Oxygen in the Microfabricated Electrochemical Sensor-Array System. ECS Transactions, 77(11), 1771−1782.10.1149/07711.1771ecst. Rocha-Meneses, Lisandra; Raud, Merlin; Orupõld, Kaja; Kikas, Timo (2017). Second-generation bioethanol production: A review of strategies for waste valorisation. Agronomy Research, 15(3), 830−847. Rooni, Vahur; Raud, Merlin; Kikas, Timo (2017). Technical solutions used in different pretreatments of lignocellulosic biomass: a review. Agronomy Research, 15(3), 848−858.
Lectures on Topic: In order to prepare specialists in the field of bioenergy and biofuels who have knowledge and experience in the topics of biofuel production, technology involved, regulations, standards and analysis, we are offering following lectures: TE.0940 Industrial processes and machines in bioenergetics, TE.0941 Characterization of biofuels: legislation and analysis, TE.0942 Biomass as an energy source, TE.0943 Biofuels, TE.0466 Fuels and greases.
Analytical Capability In the Biofuels laboratory we are able to perform following analysis:
	Density measurements with petroleum density meter; hydrometric method Standard Test Method for Density, Relative Density (Specific Gravity), or API Gravity of Crude Petroleum and Liquid Petroleum Products by Hydrometer Method. EN ISO 3675; ASTM D1298 Coefficient for Biodiesel (FAME) r q(15) = q(T) + 0,7243(T-15). Density measurements with digital density meter Standard Test Method for Density and Relative Density of Liquids by Digital Density Meter. EN ISO 12185; ASTM D 4052, ASTM D5002. Analysis of Active Sulphur Species Doctor test Standard Test Method for Qualitative Analysis for Active Sulfur Species in Fuel and Solvents (Doctor Test). ASTM D 4952. Analysis of Fractional composition Standard Test Method for Distillation of Gasolineeum Products Manual method. EN ISO 3405; ASTMD 86.
Measurements of Kinematic viscosity Standard Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and the Calculation of Dynamic Viscosity). EN ISO 3104; ASTMD 445. Measurements of Vapour Pressure Standard Test Method for Vapour Pressure of Petroleum. EN 13016-1; EN 13016-2; ASTM D5191. Measurements of Vapour Lock Index, VLI (VLI=10VP+7E70) Vapour Lock Index VLI (VLI = 10VP + 7E70) Products (Mini Method). EVS-EN 228:2002. Arvutuslik metoodika. Measurements of Existent Gum in Fuels Standard Test Method for Existent Gum in Fuels by Jet Evaporation. EN ISO 6246; ASTMD 381. Measurements of Corrosion Standard Method for Detection of Copper Corrosion from Petroleum Products by the Copper Strip Tarnish Test.; EN ISO 2160; ASTMD 130.
Measurements of Water and Particulates Standard method for Free Water and Partiulate Contamination in Distillate Fuels (Fuels Inspection Procedures). ASTMD1319. Measurements of Cetane Index Standard Test Method for Calculated Cetane Index by Four Variable Equation. EN ISO 4264; ASTMD 4737. Measurements of Cetane Index of distillate fuels. Standard Test Method for Calculated Cetane Index of Distillate Fuels. (Fuels Inspection Procedures). ASTMD 4176.
	Measurements of Flash Point. Cleveland Open cuvette Standard Test Method for Flash and Fire Points by Cleveland Open Cu. EN 22592; ASTMD 92. Measurements of Flash Point. Pensky-Martens method Standard Test Method for Flash Point by Pensky-Martens Closed Tester. EN ISO 2719; ASTM D93. Measruements of carbon residue* Standard Test Method for Conradson Carbon Residue of Gasolineeum Products (on 10% distillation), Micro Method. EN ISO 10370; ASTM D4530.
Analysis of Acid and Base number. Titration Standard Test Method for Acid and Base Number and pH by Color-Indicator Titration. EN ISO 6618; ASTM D974. Determination of water Coulometric Karl Fischer titration method EN ISO 12937; ASTM D4928. Determination of water Volumetric Karl Fischer titration method ASTM D4377. Determination of contamination in middle distillates. EN 12662; ASTM D4807.
Determination of Carbon Residue by Conradson Determination of carbon residue – Conradson method. ASTM D189; EN ISO 6615. Determination of Water and Sediment Standard Method of Test for Water and Sediment in Fuel Oil and Crude Oil by Centrifuge Method. ISO 3734. ASTM D1796. Determination of Water Standard Method of Test for Water in Petroleum Products, and Bituminous Materials by Distillation. ISO 3733; ASTM D 95.
	Determination of Water Standard Method of Test for Water in Petroleum Products, and Bituminous Materials by Distillation. ISO 3733; ASTM D 95. Water Reaction (Water Reaction Interface; Water Reaction separation). Metoodika ASTM D 1094- Water Reaction of Aviation Fuels. Determination of water soluble acids and bases Standard Test Method for Acidity of Hydrocarbon Liquids and their Distillation Residues. ASTM D1093.
Calculation of Viscosity Index Standard Practice for Calculating Viscosity Index From Kinematic viscosity at 100 °C and at 4°^oC. ISO 2909; ASTM D2270.
Determination of acid value of FAME’s Oil and fat derivates.Fatty Acid Methyl Esters(FAME). Determination acid value. EVS-EN 14104. Determination of iodine value of FAME’s Oil and fat derivates.Fatty Acid Methyl Esters(FAME). Determination iodine value. EVS EN 14111. Fibre analysis Fibre analysis from biomass (Crude Fiber, ADF and NDF determinations). Measurements of glucose and ethanol content in liquids Determination of glucose and ethanol concentration with Analox GL6 device.
Determination of structural sugars from the biomass Determination of Structural Carbohydrates and Lignin in Biomass by HPLC – NREL/TP-510-42618.
Intellectual Property: 1. Double walled cylindrical rotating photobioreactor with inner light source (link)
Double walled cylindrical rotating biophotoreactor with inner light source, that includes closed vessel, which is formed by two horizontal double walled cylinders on the common rotational axes with a potential to rotate, outer and inner walls, endplates, and the fixed section that joins both rotating cylinders and is filled with microalgal solution. In the middle of the double walled cylinders inner light source is placed. The excess heat produced by the light source is dissipated using ventilator. Turning the light source on and off the switching mechanism is used. To the upper part of the fixed section the outtake of residual gases and input of nutrient solution with filters and valves are fixed. To the lower part of the fixed section the outtake of excess biomass and input of carbon dioxide (CO₂) and/or air with filters and valves are fixed. The open ends of rotating cylinders are furnished with seals that make contact with the sliding surfaces of the fixed section. The closed ends are furnished with rolling-braces that prevent axial displacement.
2. Nitrogen explosion pretreatment method for disruption of biomass structure (link)
	The invention belongs to the field of instrumentation for production of non-fossil biofuels, more specifically instrumentation for production of bioethanol, biobuthanol and biodiesel and is applicable in biofuel production process from lignocellulosic biomass. In nitrogen explosion method for disrupting cell structure, dry milled biomass is mixed with water to achieve creamy consistency (biomass to water ration from 1:5 to 1:15), pressure is increased using nitrogen gas (N2) to a range of 10 to 60 bars, temperature in the pressure vessel is raised to a range of 125 to 190 degrees of Celsius and is kept thus for the incubation period of 10 to 120 minutes. The mixture is then cooled to a temperature range of 25 to 90 degrees of Celsius, while the total time of biomass heating, incubation and cooling is in the range of 1 to 4 hours. After reaching the final temperature, the pressure is suddenly released to achieve explosive decompression and the pretreated biomass is used in further processing.
3. Integrated flow-through apparatus for ethanol production from lignocellulosic biomass (link)
	The invention falls in the category of non-fossil fuel production technology, bioethanol production in particular, and is applicable in the production of bioethanol from lignocellulosic biomass. Integrated flow-through apparatus for ethanol production from lignocellulosic biomass contains of interconnected pre-treatment, hydrolysis, fermentation, and distillation units. The pre-treatment, hydrolysis, and distillation units are incorporated into a single integrated reactor, where pre-treatment and hydrolysis units are made of two-levelled coil of tubing that is wound around the distillation unit. The tube size in both levels is different and the reactor has a heat exchange system. The pre-treatment unit is placed in the inner part of the two-levelled tubing and the hydrolysis unit in the outer part. The tube size decreases from inner part to outer. Different parts of the tubing are immersed in the heat carrier and separated from each other by insulating walls. The fermentation unit of the apparatus is an upright container that includes an upright winding channel. The inlet of the channel is at the bottom and outlet at the top of the container. Apparatus is furnished with sensors and a control panel to control the processes in the apparatus.