• International Journal of Technology (IJTech)
  • Vol 10, No 3 (2019)

Comparative Study of Batchwise Solvent Extraction and the Microwave Assisted Extraction Method for the Purification of Triglyceride for Biodiesel Feedstock from Crude Calophyllum Inophyllum Oil (CCIO)

Hakun Wirawasista Aparamarta, Setiyo Gunawan, Badril Azhar, Hanggoro T. Aditya, Arief Widjaja, Yi Hsu Ju

Corresponding email: hakun2397@gmail.com

Cite this article as:
Aparamarta, H.W., Gunawan, S., Azhar, B., Aditya, H.T., Widjaja, A., Ju, Y.H., 2019. Comparative Study of Batchwise Solvent Extraction and the Microwave Assisted Extraction Method for the Purification of Triglyceride for Biodiesel Feedstock from Crude Calophyllum Inophyllum Oil (CCIO). International Journal of Technology. Volume 10(3), pp. 551-560

Hakun Wirawasista Aparamarta Department of Chemical Engineering, Institut Teknologi Sepuluh Nopember, Surabaya 60111, Indonesia
Setiyo Gunawan Department of Chemical Engineering, Institut Teknologi Sepuluh Nopember, Surabaya 60111, Indonesia
Badril Azhar Department of Chemical Engineering, Institut Teknologi Sepuluh Nopember, Surabaya 60111, Indonesia
Hanggoro T. Aditya Department of Chemical Engineering, Institut Teknologi Sepuluh Nopember, Surabaya 60111, Indonesia
Arief Widjaja Department of Chemical Engineering, Institut Teknologi Sepuluh Nopember, Surabaya 60111, Indonesia
Yi Hsu Ju Department of Chemical Engineering, National Taiwan University of Science and Technology, Taipei 106-07, Taiwan
Email to Corresponding Author


Recently, edible oil has been employed for biodiesel feedstocks.  However, the use of such oil to fulfil energy demand raises certain problems, such as the sustainability of the practice due to its competition with food. Therefore, it is necessary to obtain alternative resources from non-edible oil. One promising biodiesel feedstock from a non-edible oil source is crude Calophyllum inophyllum oil (CCIO) because of its high oil content. The highest oil content in CCIO is triglyceride (TG), which influences biodiesel production. The higher content of TG results in a higher yield of biodiesel. Previous research on the conversion of CCIO into biodiesel with an environmentally friendly purification method and fast separation of compounds is limited. In this work, batchwise solvent extraction (BSE) and microwave-assisted extraction (MAE) were compared to achieve an effective and efficient method for TG purification.  By using the microwave method with 450 watts of power for 30 minutes, a high content of TG was obtained.  It was found that TG content increased significantly, from 75.99% to 83.46%. Using the BSE method with a mixture of petroleum ether?methanol (methanol 25%), a solvent-to-oil mass ratio of 5:1, time for the first 2 stages  (48 hours),  the TG content obtained was 82.02%. The data obtained for the microwave method are almost equivalent to the first 2 stages of BSE with regard to TG content (83.46% compared to 82.02%) and almost 0.01 times shorter than BSE (30 minutes compared to 48 hours).

Batchwise solvent extraction; Biodiesel; Free fatty acid; Microwave-assisted extraction; Triglycerides


Along with annual economic growth, population and regional development, the need for energy is also increasing. Fuel consumption increased rapidly from 2009 to 2015, from around 1,297,000 barrels/day (bpd) to 1,628,000 bpd, or an increase of 20.3%. In six years, there was an increase in fuel consumption of 331,000 bpd. Indonesia's oil consumption is showing an increasing trend due to its growing population and economy. As domestic production cannot meet domestic demand, Indonesia  imports 350,000  to 500,000  barrels of fuel per day  from  several  countries. The country needs more fuel oil to meet domestic demand, so an alternative source of renewable energy is needed.

Biodiesel is one of the solutions to fulfil domestic demand in Indonesia. Recently, biodiesel feedstock has used used edible oil, such as palm, soy bean, sunflower and rapeseed. The use of edible oil to meet energy demand poses many problems, such as the sustainability of the practice due to its competition with food, land and water (Kansedo et al., 2009). This competition will increase the price of raw materials, and almost 80% of the cost of biodiesel production is that of the raw materials (Saraf & Thomas 2007). The selection of the underlying raw material is based on the oil content and yield of the plant used as biodiesel feedstock, so that production costs can be lower (Gui et al., 2008). This oil content is usually determined by establishing the triglyceride (TG) levels which are mostly found in oil; on this basis, C. Inophyllum is one of the best feedstocks for biodiesel production. Aparamarta et al. (2018) report that the oil content of C. inophyllum is 70.38%.

The biggest challenge in using crude C. inophyllum oil as biodiesel feedstock is the large amount of free fatty acids (FFA) it contains. The level of these in oil should be below 3% for alkaline-catalyzed transesteri?cation (Ribeiro et al., 2011) and lower than 0.3% for edible oil (SNI, 2002). A high level of FFA will cause a saponification reaction, which can decrease biodiesel yields, hinder the separation of ester from glycerin, and reduce the formation rate of biodiesel (Thiruvengadaravi et al., 2012). Therefore, methods for TG purification are applied to achieve an optimal yield of biodiesel. Existing methods are chemical purification, which involves chemicals that can be hazardous in handling and which can damage the environment. Therefore, it is necessary to find a solution comprising an easy method to provide better separation of FFA and TG and which does not damage the environment. One approach is the batchwise solvent extraction (BSE) method, as used by Aparamarta et al. (2016), who succeeded in separating TG and FFA with purity and recovery of TG as the indicator for the effective separation of nonpolar lipid fraction from crude C. inophyllum seed oil. The resulting product had a TG content of 98.53% and FFA of 0.35%. However, this method requires a long separation time process.

Therefore, this study involved the addition of the microwave-assisted extraction (MAE) method to the TG purification process. MAE is an extraction process that utilizes the energy generated by microwaves with a frequency of 0.30-300 GHz in the form of electromagnetic non-ionization radiation. The advantages of the MAE method are that it has a lower solvent consumption, and a significantly reduced extraction time compared to conventional methods (Cercado et al., 2018). In addition, it has a better heating process, less energy consumption and increased yields (Liu et al., 2013). The heating process acts as the driving force to extract the triglyceride compound from the biological matrix in a shorter period of time (Patil et al., 2011). The method was used by Leong et al. (2016), who used microwave heating to obtain pyrolyzed oil from crude glycerol.

The purpose of this research is to study an effective method for TG purification as a biodiesel feedstock. The alternative raw material selected was Calophyllum inophyllum, on the basis of oil content and yield. The technology selected was batchwise solvent extraction (BSE) and microwave-assisted extraction (MAE). 


High purification of triglyceride (TG) was successfully obtained from crude Calophyllum inophyllum via batchwise solvent extraction (BSE) and microwave assisted extraction (MAE). The data obtained for the MAE method are almost equivalent to the first two stages BSE for TG content (83.46% compared to 82.02%) and almost 0.01 times shorter than BSE (30 minutes compared to 48 hours). The optimum conditions using the BSE method were achieved at stage 9, with percentages of TG of 94.67% and of FFA of 0.63%.  For MAE, the optimum conditions were obtained at 450 watts and 30 minutes, resulting in corresponding figures of 83.46% and 7.5%. The power and extraction time variables had a significant influence on the percentages of TG compound in the C. inophyllum oil.


This work was supported by a grant (138/Addendum/ITS/2019) provided by the Institute of Research and Public Services (LPPM), Institut Teknologi Sepuluh Nopember (ITS), Surabaya, Indonesia.The author would like to thank Mr. Gunawan, Mr. Rayhan, and Mr. Adya for their excellent technical support.

Supplementary Material
R1-CE-2920-20190404112722.png Fig 1 MAE method
R1-CE-2920-20190404112812.jpg Fig 2 GC and TLC result for BSE method
R1-CE-2920-20190404112851.jpg Fig 3 GC and TLC result for MAE method
R1-CE-2920-20190404112934.jpg Fig 4 Time effect for BSE method
R1-CE-2920-20190404113013.png Fig 5a time effect for TG
R1-CE-2920-20190404113110.png Fig 5b Time effect for FFA
R1-CE-2920-20190404113203.png Fig 6a Power Effect for TG
R1-CE-2920-20190404113242.png Fig 6b Power effect for FFA

Purification of Triacylglycerols from Nyamplung (Calophyllum inophyllum) Oil by Batchwise Solvent Extraction. Industrial Engineering Chemistry Research, Volume 55(11), pp. 3113–3119

Aparamarta, H.W., Anggraini, D., Istianingsih, D., Susanto, D.F., Widjaja, A., Ju, Y.H., Gunawan, S., 2017. Fatty Acid Fragmentation of Triacyglycerol Isolated from Crude Nyamplung Oil. In: AIP Conference Proceedings, Volume 1840(1), pp. 060004

Aparamarta, H.W., Qadariyah, L., Gunawan S., Ju Y.H., 2018. Separation and Identification of Fatty Acid in Triacyglycerol Isolated from Calophyllum inophyllum Oil. Asia Research Publishing Network, Volume 13(2), pp. 442-451

Atabani, A.E., César, A.D. 2014. Calophyllum Inophyllum L. –A Prospective Non Edible Biodiesel Feedstock. Study of Biodiesel Production, Properties, Fatty Acid Composition, Blending and Engine Performance. Renewable and Sustainable Energy Reviews, Volume 37, pp. 644655

Azam, M.M., Waris, A., Nahar, N.M., 2005. Prospects and Potential of Fatty Acid Methyl Esters of Some Non-traditional Seed Oils for Use as Biodiesel in India. Biomass and Bioenergy, Volume 29(4), pp. 293–302

Cercado, A.P.I., Ballesteros, F.C., Capareda, S.C., 2018. Biodiesel from Three Microalgae Transesterification Processes using Different Homogenous Catalysts. International Journal of Technology, Volume 9(4), pp. 645–651

Du, W., Xu, Y.Y., Liu, D., Zeng, H., 2004. Comparative Study on Lipase-catalyzed Transformation of Soybean Oil for Biodiesel Production with Different Acyl Acceptors. Journal of Molecular Catalysis B: Enzymatic, Volume 30(3-4), pp. 125–129

Erliyanti, N.K., Rosyidah, E., 2017. Pengaruh Daya Microwave terhadap Yield pada Ekstraksi Minyak Atsiri dari Bunga Kamboja (Plumeria alba) Menggunakan Metode Microwave Hydrodistillation (The Effect of Microwave Power on Extraction Yield of Essential Oil from Cambodian Flowers (Plumeria alba) using Microwave Hydrodistillation Method). Jurnal Rekayasa Mesin (Journal of Machine Engineering), Volume 8(3), pp. 175–178

Ferhat, M.A., Meklati, B.Y., Smadja, J., Chemat, F., 2006. An Improved Microwave Clevenger Apparatus for Distillation of Essential Oils from Orange Peel. Journal of Chromatography A, Volume 1112(1-2), pp. 121–126

Gui, M.M., Lee, K.T., Bhatia S., 2008. Feasibility of Edible Oil vs Non Edible Oil vs Waste Edible Oil as Biodiesel Feedstock. Energy, Volume 33(11), pp. 1646–1653

Gunawan, S., Fabian, C. Ju, Y. H., 2008a. Isolation and Purification of Fatty Acid Steryl Esters from Soybean Oil Deodorizer Distillate. Industrial Engineering Chemistry Research, Volume 47(18), pp. 7013–7018

Gunawan, S., Kasim, N.S., Ju, Y.H., 2008b. Separation and Purification of Squalene from Soybean Oil Deodorizer Distillate. Separation and Purification Technology, Volume 60(2), pp. 128–135

Kansedo, J., Lee K.T., Bhatia S., 2009. Cerbera Odollam (Sea Mango) Oil as A Promising Non-edible Feedstock for Biodiesel Production. Fuel, Volume 88(6), pp. 1148–1150

Karakaya, S., El S.N., Karagozlu, N., Sahin, S., Sumnu, G., Bayramoglu, B., 2014. Microwave-Assisted Hydrodistillation of Essential Oil from Rosemary. Journal of Food Science and Technology, Volume 51(6), pp. 1056–1065

Leong, S.K., Lam, S.S., Ani, F.N., Ng, J-H., Chong, C.T., 2016. Production of Pyrolyzed Oil from Crude Glycerol using a Microwave Heating Technique. International Journal of Technology, Volume 7(2), pp. 323–331

Liu, W., Yin, P., Liu, X., Chen, W., Chen, H., Liu, C., Qu, R., Xu, Q., 2013. Microwave Assisted Esterification of Free Fatty Acid Over a Heterogeneous Catalyst for Biodiesel Production. Energy Conversion and Management, Volume 76, pp. 10091014

Patil, P.D., Gude, V.G., Mannarswamy, A., Cooke, P., Munson-McGee, S., Nirmalakhandan, N., Lammers, P., Deng, S., 2011. Optimization of Microwave Assisted Transesterification of Dry Algal Biomass using Response Surface Methodology. Bioresource Technology, Volume 102(2), pp. 1399–1405

Ribeiro, A., Castro, F., Carvalho, J., 2011. In?uence of Free Fatty Acid Content in Biodisel Production on Non-edible Oils. In: Wastes: Solutions, Treatments and Opportunities 1st International Conference, Guimara?es Portugal, pp. 12?14

Saraf, S., Thomas, B., 2007. Influence of Feedstock and Process Chemistry on Biodiesel Quality. Process Safety and Environmental Protection, Volume 85(5), pp. 360–367

Sahoo, P.K., Das, L.M., Babu, M.K.G., Naik, S.N., 2007. Biodiesel Development from High Acid Value Polanga Seed Oil and Performance Evaluation in a CI Engine. Fuel, Volume 86(3), pp. 448–454

Sengar, G., Sharma, H.K., Kumar, N., 2015. Effect of Microwave Heating on Physico-chemical and Thermal Behavior of Blended Fat. International Food Research Journal, Volume 22(1), pp. 295–303

Singh, S.P., Singh, D., 2010. Biodiesel Production through the Use of Different Sources and Characterization of Oils and Their Esters as the Substitute of Diesel: A Review. Renewable and Sustainable Energy Reviews, Volume 14(1), pp. 200–216

SNI 01-3741, 2002. Indonesian Standart of Cooking Oil

Thiruvengadaravi, K.V., Nandagopal, J., Baskaralingam, P., Sathya Selva Bala, V., Sivanesan, S., 2012. Acid-catalyzed Esterification of Karanja (Pongamia pinnata) Oil with High Free Fatty Acids for Biodiesel Production. Fuel, Volume 98, pp. 1–4

Zhang, H., Yang, X., Wang, Y., 2011. Microwave Assisted Extraction of Secondary Metabolites from Plants: Current Status and Future Directions. Trends in Food Science & Technology, Volume 22(12), pp. 672–688