Analytical monitoring of the production of biodiesel by high-performance liquid chromatography with various detection methods

Holčapek, Michal; Jandera, Pavel; Fischer, Jan; Prokeš, B.

doi:10.1016/s0021-9673(99)00790-6

Cited by 277 publications

(193 citation statements)

References 61 publications

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“…It is also worth to mention, that trans 18:1 isomer has a higher slope than the cis form due to its higher absorption of energy for π-π* transitions. 9 Despite a hard work performed in order to find a chromatographic resolution for 18:1 cis and 16:0, it was impossible to avoid the co-elution of these compounds. It was only possible to quantify 18:1 cis and 16:0 after hydrogenation of biodiesel using Pd/C as catalysts (conditions: temperature of 80 °C and hydrogen pressure of 100 atm).…”

Section: Hplc Separation and Quantitave Analysis: Methods Bmentioning

confidence: 99%

“…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%

“…9,18 Many workers, however, may find that HPLC offers some advantage and indicate some critical points of GC: (i) the presence of heat-labile compounds affects the quantification of FAME (fatty acid methyl esters), (ii) the carbon chain polyunsaturated of the fatty acids may undergo structural changes, isomerization and decomposition under high temperatures, (iii) it is not possible to collect fractions of the separated fatty acid esters for further analysis, (iv) baseline drift, and (v) GC analysis frequently requires derivatization step by saponification furthered to methylation, consuming reagents as hexane, BF 3 and NaCl, being time-consuming and labor-intensive. 11,17 In this work, HPLC (called method B) and GC techniques are compared with respect to the determination of FAMEs in biodiesel.…”

Section: Introductionmentioning

confidence: 99%

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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: Hplc Separation and Quantitave Analysis: Methods Bmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

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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show abstract

“…Each sample analysis was performed in at least duplicate and the relative error between consecutive measurements was evaluated at 5%. This method has previously been developed and successfully applied for the rapid quantitative determination of the yield of the transesterification reaction (Holčapek et al, 1999). The HPLC chromatograms of the raw canola oil, the methyl, and ethyl esters obtained from the transesterification of canola oil using a homogeneous catalyst are shown in Figure S1A in Supplementary Material.…”

Section: Hplc Instrument and Methodsmentioning

confidence: 99%

“…The canola oil conversion is typically determined by HPLC analysis based on a method which was developed for the quantification of MEs in biodiesel produced from transesterification reactions with a homogeneous catalyst in a water-free environment (Holčapek et al, 1999). The electro-catalytic process without the addition of a cosolvent occurred in a two-phase reaction mixture and in the presence of large quantity of water and salts.…”

Section: Conversion Of Canola Oil In Methanolic and Ethanolic Reactiomentioning

confidence: 99%

Electro-Catalytic Biodiesel Production from Canola Oil in Methanolic and Ethanolic Solutions with Low-Cost Stainless Steel and Hybrid Ion-Exchange Resin Grafted Electrodes

et al. 2017

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Biodiesel is a growing alternative to petroleum fuels and is produced by the catalyzed transesterification of fats in presence of an alcohol base. Transesterification processes using homogeneous catalysts are considered to be among the most efficient methods but rely on the feedstock quality and low water content in order to avoid undesirable saponification reactions. In this work, the electro-catalytic conversion of canola oil to biodiesel in a 1% aqueous methanolic and ethanolic reaction mixture was performed without the addition of external catalyst or cosolvent. An inexpensive stainless steel (SS) electrode and a hybrid SS electrode coated with an ion-exchange resin catalyst were used as cathode materials while the anode was composed of a plain carbon paper. The cell voltages were varied from 10 to 40 V and the reaction temperature maintained at 20 or 40°C. The canola oil conversion rates were found to be superior at 40°C without saponification reactions for cell voltages below 30 V. The conversion rates were as high as 87% for the hybrid electrode and 81% for the plain SS electrode. This work could inspire new process development for the conversion of high water content feedstock for the production of second-generation biodiesel.

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Biodiesel from rapeseed oil, methanol and KOH. 3. Analysis of composition of actual reaction mixture

Komers

Stloukal

Machek

et al. 2001

Eur. J. Lipid Sci. Technol.

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Biodiesel from rapeseed oil, methanol and KOH 3. Analysis of composition of actual reaction mixtureDetailed analysis is described of the samples taken after suitable reaction times from the actual reaction mixture during the production of biodiesel fuel using methanolysis of rapeseed oil catalyzed by KOH. Three methods for stoppage of reaction (neutralisation of catalyst, dilution by two suitable solvents) in the sample are used. The contents of mono-, di-and triacylglycerols, methylesters of fatty acids (biodiesel) and potassium salts of fatty acids of rapeseed oil, glycerol (by HPLC method), basicity (by potentiometric titration) and water (by GC and Karl-Fischer method) in the samples are determined. An example of these determinations is described.

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Analytical monitoring of the production of biodiesel by high-performance liquid chromatography with various detection methods

Cited by 277 publications

References 61 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

Electro-Catalytic Biodiesel Production from Canola Oil in Methanolic and Ethanolic Solutions with Low-Cost Stainless Steel and Hybrid Ion-Exchange Resin Grafted Electrodes

Biodiesel from rapeseed oil, methanol and KOH. 3. Analysis of composition of actual reaction mixture

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