Thin Layer chromatography as innovative technique for qualitative characterization of Biodiesel produced by esterification

Marcelo Paulo Stracke, Antonio Vanderlei dos Santos, Mauro Cesar Marchetti, Caroline Barlette da Cunha, Michel Brondani, João Henrique Cabral Wancura, Flávio Dias Mayer, Ronaldo Hoffmann


The objective of this work was to evaluate the use of TLC, using the iodine vapor visualization method, for identification and preliminary characterization of biodiesel produced by esterification. The esterification reaction was performed at constant temperature of 65 °C for 2 hours, using dimethyl sulfate as alkylating agent and dodecanoic acid as oleaginous raw material. The chromatographic plate was subjected to the method of revelation after adding 5 µL of a sample of fatty acid and biodiesel on the chromatographic vessel. The indication of biodiesel formation was obtained by calculating the retention factor (Rf) and validated by hydrogen nuclear magnetic resonance (H1NMR). The Rf values and of the region of peaks of chemical functions were identical to those found in other studies, which allowed to confirm the formation of biodiesel. It can be concluded that TLC can be used as a innovative technique for preliminary qualitative characterization of biodiesel formation by esterification.

Texto completo:



Baskar G, Aiswarya R (2016) Trends in catalytic production of biodiesel from various feedstocks. Renew Sustain Energy Rev 57:496–504.

Halek F, Delavari A, Kavousi-rahim A (2013) Production of biodiesel as a renewable energy source from castor oil. CLEAN - Soil, Air, Water 15:1063–1068.

Ollis DL, Liu BJ, Stevenson BJ (2012) Engineering Enzymes for Energy Production. Aust J Chem 65:652–655.

Canesin EA, de Oliveira CC, Matsushita M, et al. (2014) Characterization of residual oils for biodiesel production. Electron J Biotechnol 17:39–45.

Xue F, Zhang X, Luo H, Tan T (2006) Short communication. A new method for preparing raw material for biodiesel production. Process Biochem 41:1699–1702.

Özener O, Yüksek L, Ergenç AT, Özkan M (2012) Effects of soybean biodiesel on a DI diesel engine performance, emission and combustion characteristics. Fuel 115:875–883.

Qi DH, Geng LM, Chen H, et al. (2009) Combustion and performance evaluation of a diesel engine fueled with biodiesel produced from soybean crude oil. Renew Energy 34:2706–2713.

Buyukkaya E (2010) Effects of biodiesel on a di diesel engine performance, emission and combustion characteristics. Fuel 89:3099–3105.

Xue J, Grift TE, Hansen AC (2011) Effect of biodiesel on engine performances and emissions. Renew Sustain Energy Rev 15:1098–1116.

Demirbas A (2009) Progress and recent trends in biodiesel fuels. Energy Convers Manag 50:14–34.

Coggon R, Vasudevan PT, Sanchez F (2007) Enzymatic transesterification of olive oil and its precursors. Biocatal Biotransform 25:135–143.

Datta A, Mandal BK (2016) A comprehensive review of biodiesel as an alternative fuel for compression ignition engine. Renew Sustain Energy Rev 57:799–821.

Atadashi IM, Aroua MK, Aziz AA (2010) High quality biodiesel and its diesel engine application: A review. Renew Sustain Energy Rev 14:1999–2008.

Gautam K, Gupta NC, Sharma DK (2014) Physical characterization and comparison of biodiesel produced from edible and non-edible oils of Madhuca indica (mahua), Pongamia pinnata (karanja), and Sesamum indicum (til) plant oilseeds. Biomass Convers Biorefinery 4:193–200.

Aransiola EF, Ojumu TV, Oyekola OO, et al. (2014) A review of current technology for biodiesel production: State of the art. Biomass and Bioenergy 61:276–297.

Ng J, Hoon KN, Gan S (2010) Advances in biodiesel fuel for application in compression ignition engines. Clean Technol Environ Policy 12:459–493.

Bharathiraja B, Chakravarthy M, Kumar RR, et al. (2014) Biodiesel production using chemical and biological methods - A review of process, catalyst, acyl acceptor, source and process variables. Renew Sustain Energy Rev 38:368–382.

Elms RD, El-Halwagi MM (2010) The effect of greenhouse gas policy on the design and scheduling of biodiesel plants with multiple feedstocks. Clean Technol Environ Policy 12:547–560.

Beltrán-Prieto JC, Kolomazník K, Pecha J (2013) A review of catalytic systems for glycerol oxidation: Alternatives for waste valorization. Aust J Chem 66:511–521.

Meira M, Quintella CM, Ribeiro EMO, et al. (2015) Overview of the challenges in the production of biodiesel. Biomass Convers Biorefinery 1–9.

Ma F, Hanna MA (1999) Biodiesel production : a review 1. Bioresour Technol 70:1–15.

Leung DYC, Wu X, Leung MKH (2010) A review on biodiesel production using catalyzed transesterification. Appl Energy 87:1083–1095.

Cai ZZ, Wang Y, Teng YL, et al. (2015) A two-step biodiesel production process from waste cooking oil via recycling crude glycerol esterification catalyzed by alkali catalyst. Fuel Process Technol 137:186–193.

Freedman B, Pryde EH, Mounts TL (1984) Variables

Affecting the Yields of Fatty Esters from Transesterified Vegetable Oils1. JAOCS 61:1638–1643.

Freedman B, Butterfield RO, Pryde EH (1986) Transesterification Kinetics of Soybean Oil1. JAOCS 63:1375–1380.

Moreira F, Badenes SM, Cabral JMS (2013) Biocatalytic transesterification of triglycerides and alcohols for the production of biodiesel using cutinase in organic media. Biocatal Biotransformation 31:246–254.

Tiwari P, Garg S (2016) Study of reversible kinetic models for alkali-catalyzed Jatropha curcas transesterification. Biomass Convers Biorefinery 6:61–70.

Rezende MJC, Pinto AC (2016) Esterification of fatty acids using acid-activated Brazilian smectite natural clay as a catalyst. Renew Energy 92:171–177.

Yu H, Niu S, Lu C, et al. (2016) Preparation and esterification performance of sulfonated coal-based heterogeneous acid catalyst for methyl oleate production. Energy Convers Manag 126:488–496.

Saravanan K, Tyagi B, Shukla RS, Bajaj HC (2015) Esterification of palmitic acid with methanol over template-assisted mesoporous sulfated zirconia solid acid catalyst. Appl Catal B Environ 172-173:108–115.

Alegría A, Cuellar J (2015) Esterification of oleic acid for biodiesel production catalyzed by 4-dodecylbenzenesulfonic acid. Appl Catal B Environ 179:530–541.

Neumann K, Werth K, Martín A, Górak A (2016) Biodiesel production from waste cooking oils through esterification: Catalyst screening, chemical equilibrium and reaction kinetics. Chem Eng Res Des 107:52–62.

Phan AN, Phan TM (2008) Biodiesel production from waste cooking oils. Fuel 87:3490–3496.

Urrutia C, Sangaletti-Gerhard N, Cea M, et al. (2016) Two step esterification-transesterification process of wet greasy sewage sludge for biodiesel production. Bioresour Technol 200:1044–1049.

Mazumdar P, Dasari SR, Borugadda VB, et al. (2013) Biodiesel production from high free fatty acids content Jatropha curcas L. oil using dual step process. Biomass Convers Biorefinery 3:361–369.

Adewuyi A, Oderinde RA, Ojo DFK (2012) Biodiesel from the seed oil of Treculia africana with high free fatty acid content. Biomass Convers Biorefinery 2:305–308.

National Agency of Petroleum Natural Gas and, Biofuels (2008) Resolution ANP no 7.

Fernando S, Karra P, Hernandez R, Jha SK (2007) Effect of incompletely converted soybean oil on biodiesel quality. Energy 32:844–851.

Tariq M, Ali S, Khalid N (2012) Activity of homogeneous and heterogeneous catalysts, spectroscopic and chromatographic characterization of biodiesel: A review. Renew Sustain Energy Rev 16:6303–6316.

Monteiro MR, Ambrozin ARP, Lião LM, Ferreira AG (2008) Critical review on analytical methods for biodiesel characterization. Talanta 77:593–605.

Zhang WB (2012) Review on analysis of biodiesel with infrared spectroscopy. Renew Sustain Energy Rev 16:6048–6058.

Fedosov SN, Brask J, Xu X (2011) Analysis of biodiesel conversion using thin layer chromatography and nonlinear calibration curves. J Chromatogr A 1218:2785–2792.

Martelanc M, Vovk I, Simonovska B (2009) Separation and identification of some common isomeric plant triterpenoids by thin-layer chromatography and high-performance liquid chromatography. J Chromatogr A 1216:6662–6670.

Ilbeigi V, Sabo M, Valadbeigi Y, et al. (2016) Laser desorption-ion mobility spectrometry as a useful tool for imaging of thin layer chromatography surface. J Chromatogr A 1459:145–151.

Mroczek T, Ndjoko-Ioset K, Głowniak K, et al. (2006) Investigation of Symphytum cordatum alkaloids by liquid-liquid partitioning, thin-layer chromatography and liquid chromatography-ion-trap mass spectrometry. Anal Chim Acta 566:157–166.

Ristivojević P, Trifković J, Vovk I, Milojković-Opsenica D (2017) Comparative study of different approaches for multivariate image analysis in HPTLC fingerprinting of natural products such as plant resin. Talanta 162:72–79.

Dawan P, Satarpai T, Tuchinda P, et al. (2017) A simple analytical platform based on thin-layer chromatography coupled with paper-based analytical device for determination of total capsaicinoids in chilli samples. Talanta 162:460–465.

Collins CH, Braga GL, Bonato PS (2006) Fundamentos da cromatografia, 1st ed. Ed. Unicamp, Campinas, São Paulo.

Machado SA (2013) Estudo da produção de biodiesel a partir do óleo de macaúba (Acrocomia aculeata) pela rota etílica. Universidade de São Paulo

Froehner S, Leithold J, Lima LF (2007) Transesterification Of Vegetable Oils: Characterization by Thin-layer Cromatography and Density. Quim Nova 30:2016–2019.

Ferrari RA, Oliveira VS, Scabio A (2005) Biodiesel from soybean: characterization and consumption in an energy generator. Quim Nova 28:19–23.

Souza WL, Ferrari RA, Scabio A (2006) Biodiesel de óleo de de girassol e etanol. Biomassa Energ 2:1–5.

Cubas AL V, Machado MM, Pinto CRSC, et al. (2016) Biodiesel production using fatty acids from food industry waste using corona discharge plasma technology. Waste Manag 47:149–154.

Satyarthi JK, Srinivas D, Ratnasamy P (2009) Estimation of Free Fatty Acid Content in Oils, Fats, and Biodiesel by 1HNMR Spectroscopy. Energy and Fuels 23:2273–2277.

Kollar SRM (2012) Desenvolvimento de Metodologias Analíticas para Análise de Biodiesel por RMN - 1H 1,40 T.

Shimamoto GG, Tubino M (2016) Quantification of methanol in biodiesel through 1H nuclear magnetic resonance spectroscopy. Fuel 175:99–104.



  • Não há apontamentos.

Direitos autorais 2019 Revista GEINTEC - Gestão, Inovação e Tecnologias

Licença Creative Commons
Esta obra está licenciada sob uma licença Creative Commons Atribuição - NãoComercial 4.0 Internacional.


ISSN: 2237-0722

A REVISTA GEINTEC possui D.O.I e está cadastrada nos sistemas:

Os trabalhos da Revista GEINTEC - Gestão, Inovação e Tecnologias de está licenciado com uma Licença Creative Commons - Atribuição-NãoComercial 4.0 Internacional.

Licença Creative Commons

Associação Acadêmica de Propriedade Intelectual - Aracaju/SE. Universidade Federal de Sergipe. Cidade Universitária Prof. "José Aloísio de Campos" 

Av. Marechal Rondon, s/n Jardim Rosa Elze - Pólo de Pós-Graduação - Sala 8 - CEP 49100-000 - São Cristóvão/SE. [email protected]