Determinação do teor de ésteres graxos em biodiesel metílico de soja por cromatografia gasosa utilizando oleato de etila como padrão interno

Marques, Marcelo Volpatto; Naciuk, Fabrício Fredo; Mello, Ana Maria de Souza; Seibel, Nair Maria; Fontoura, Luiz Antonio Mazzini

doi:10.1590/s0100-40422010000400039

Cited by 19 publications

(18 citation statements)

References 10 publications

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“…Some chromatographic methods have been created and improved to analyze the biodiesel 6 . Among these, thin layer chromatography (TLC), 7 gas chromatography (GC), 8 high-performance liquid chromatography (HPLC), [9][10][11] gel permeation chromatography (GPC), 12 nuclear magnetic resonance (NMR) 13 and near infrared spectroscopy (NIR) 14 are included.…”

Section: Introductionmentioning

confidence: 99%

Chromatographic analyses of fatty acid methyl esters by HPLC-UV and GC-FID

Carvalho¹,

Mendonça

Pinho³

et al. 2012

J. Braz. Chem. Soc.

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Um método analítico por cromatografia líquida de alto rendimento com detecção ultravioleta (HPLC-UV) (método A) foi utilizado na determinação simultânea dos valores totais de triacilglicerídeos, diacilglicerídeos, monoacilglicerídeos e ésteres metílicos de ácidos graxos na alcólise de diferentes óleos (algodão, canola, girassol, milho e soja). As análises foram realizadas a 40 °C por 20 min usando gradiente de metanol (MeOH) e 2-propanol-hexano 5:4 (v/v) (PrHex): 100% de MeOH em 0 min, 50% de MeOH e 50% de PrHex em 10 min mantido com eluição isocrática por 10 min. Outro método por HPLC-UV (método B) com eluição isocrática de acetonitrila por 34 min foi utilizado na determinação da composição de ácidos graxos de óleos analisando seus derivados de éster metílico. Os conteúdos foram analisados com satisfatória repetibilidade (desvio padrão relativo, RSD < 3%), linearidade (r 2 > 0,99) e sensibilidade (limite de quantificação). O método B foi comparado com o método oficial cromatográfico gasoso com detecção através de ionização por chama (GC-FID) da American Oil Chemists' Society (AOCS) na determinação de ésteres metílicos de ácidos graxos (FAME) em amostras reais de biodiesel.An analytical method using high performance liquid chromatography with UV detection (HPLC-UV) (method A) was used for simultaneous determination of total amounts of triacylglycerides, diacylglycerides, monoacylglycerides and fatty acid methyl esters in alcoholysis of different oil (cotton, canola, sunflower, corn and soybean) samples. Analyses were carried out at 40 °C for 20 min using a gradient of methanol (MeOH) and 2-propanol-hexane 5:4 (v/v) (PrHex): 100% of MeOH in 0 min, 50% of MeOH and 50% of PrHex in 10 min maintained with isocratic elution for 10 min. Another HPLC-UV method (method B) with acetonitrile isocratic elution for 34 min was used to determine the fatty acid composition of oils analyzing their methyl ester derivatives. Contents were determined with satisfactory repeatability (relative standard deviation, RSD < 3%), linearity (r 2 > 0.99) and sensitivity (limit of quantification). Method B was compared with an official gas chromatographic method with flame ionization detection (GC-FID) from American Oil Chemists' Society (AOCS) in the determination of fatty acid methyl esters (FAME) in biodiesel real samples.Keywords: biodiesel, triacylglycerides, gas chromatography, liquid chromatography, methyl ester IntroductionThe direct use of fats and oils (mainly composed by triacylglycerides) in diesel engines is problematic and can lead to many problems, such as carbon deposit due to its poor atomization, high viscosity and thickening of lubricating oil as a consequence of its low volatility. 1,2 There are many possible solutions to address the viscosity problem, which are dilution with diesel fuel, microemulsions with short chain alcohols and pyrolysis or transesterification of triacylglycerides. Transesterification is a widespread process used for obtaining biodiesel and involves the catalyzed reaction of triacylglycerides (TAGs) a...

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Section: Introductionmentioning

confidence: 99%

Chromatographic analyses of fatty acid methyl esters by HPLC-UV and GC-FID

Carvalho¹,

Mendonça

Pinho³

et al. 2012

J. Braz. Chem. Soc.

View full text Add to dashboard Cite

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“…This detection system significantly increases the identification power of GC, avoiding ambiguities about the chemical nature of the eluting species [52]. Recent approaches for development of GC-based alternative analytical methods include the use of ethyl oleate as internal standard for glycerol determination [54], the use of ionic liquid as stationary phase for determination of FAME in diesel blends [55] and the determination of polyunsaturated FAMEs with wax capillary column using methyl tricosanoate as internal standard. [56].…”

Section: Biodiesel Quality Controlmentioning

confidence: 99%

Electrochemical Methods in Analysis of Biofuels

Santos¹,

Takeuchi²,

Fenga³

et al. 2011

Applications and Experiences of Quality Control

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“…17 In the literature, many studies have demonstrated that the GC technique can be applied to determine the content of FAME or FAEE in samples of B100 or in mixtures of diesel and biodiesel, 19 and it is also used to quantify other substances like the alcohol used in the reaction and also secondary products such as glycerol, monoacylglycerides, diacylglycerides and triacylglycerides. 1,2,[20][21][22][23][24][25][26][27] However, due to the variety of raw materials 28,29 that can be employed for biodiesel production and the importance of its production in several countries, it is strategic to develop fast 30 and economically attractive methods, through modifications such as applying different column temperatures and lengths and the use of a different internal standard 23 exhibiting similar characteristics, but not present in biodiesel composition.…”

Section: Introductionmentioning

confidence: 99%

Determination of Alkyl Esters Content by Gas Chromatography: Validation of Method Based on Short Column and Response Factor

Silva¹,

Melo²,

Wolf³

et al. 2017

J. Braz. Chem. Soc.

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In this study an analytical method, based on gas chromatography with flame ionization detection, using a short column and response factor (GCSCRF), was validated for the quantification of fatty acid alkyl esters (methylic or ethylic). During the validation process, the proposed method was employed to analyze twenty samples of fatty acid methyl esters and fatty acid ethyl esters. Biodiesel samples were produced from soybean oil and the validated method was found to be selective, being able to separate and identify every ester species present in the samples according to its carbon number. When the method was submitted to some variations in the sample preparation procedure, it remained robust. Limits of detection and quantification were 6.76 and 20.4 mg mL -1 , respectively. The suggested method also showed great precision when successive analyses were carried out for different analysts, with standard deviation (SD) 0.6 for repeatibility and relative standard deviation (RSD) percentage 7.3% for intermediate precision, excellent accuracy when compared to other reference methods (EN 14103 and high-performance liquid chromatography with ultraviolet dection (HPLC-UV)) and recovery studies.Keywords: biodiesel, gas chromatography, chromatografic column, response factor IntroductionThe growing energy crisis, caused by a high consumption of fossil fuels and environmental degradation, has influenced the development of renewable fuels as alternative energy sources. Biodiesel, produced by the transesterification or esterification of vegetable or animal oils and fats or fatty acids, in the presence of an alcohol such as methanol or ethanol, 1-3 is one of the most promising alternative fuels. Besides being renewable, nontoxic and biodegradable, biodiesel can be added to petrodiesel due to its similar physico-chemical properties. 4Pure biodiesel is represented by B100 (100% fatty acid alkyl esters (FAAE)). However, in the case of biodiesel/petrodiesel blends the abbreviation BX indicates the percentage volume of B100 in these blends. 5 Nowadays, a B7 mixture (7% B100 and 93% diesel oil) is marketed in Brazil. 6 Biodiesel is composed of a mixture of fatty acid methyl esters (FAME) or ethyl esters (FAEE). 7 The quantification of these esters is conducted using several analytical techniques, particularly gas chromatography (GC) and high-performance liquid chromatography (HPLC).8-14 GC with flame ionization detection (FID) shows excellent selectivity in biodiesel analysis and is the main technique used for this purpose. 8,11,15,16 In Brazil, the production and use of biodiesel is regulated and supervised by the Brazilian National Petroleum, Natural Gas and Biofuels Regulatory Agency (ANP) through Resolution No. 45/2014, 17 in which the European Standard EN1410318 is adopted for the determination of methyl esters by the GC technique. In this case, the external calibration method is used, based on a comparison of the analyte peak area with the peak area of some external standards, analyzed at different concentrations. 17In the ...

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Determinação do teor de ésteres graxos em biodiesel metílico de soja por cromatografia gasosa utilizando oleato de etila como padrão interno

Cited by 19 publications

References 10 publications

Chromatographic analyses of fatty acid methyl esters by HPLC-UV and GC-FID

Chromatographic analyses of fatty acid methyl esters by HPLC-UV and GC-FID

Electrochemical Methods in Analysis of Biofuels

Determination of Alkyl Esters Content by Gas Chromatography: Validation of Method Based on Short Column and Response Factor

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