Free and Total Glycerin Analyses in Biodiesel–Diesel Blends

Pisarello, María Laura; Maquirriain, Maira Alejandra; Querini, C.A.

doi:10.1021/acs.energyfuels.8b00896

Cited by 8 publications

(8 citation statements)

References 24 publications

(50 reference statements)

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“…The volumetric procedure for the determination of the total and free glycerol was a simple and low-cost alternative for quality control laboratories. 10 Although there was no need to convert the sample to acylglycerides, several extraction steps were required prior to titration, which lasted at least 1 h. In addition, the procedure consumed large amounts of sample ( ca. 300 g per determination).…”

Section: Resultsmentioning

confidence: 99%

“…The use of an internal standard is also recurrent and adds another step to the analysis. Alternative procedures without chromatographic separations have been proposed exploiting amperometry, 9 volumetry, 10 and spectrophotometry. 11 A volumetric procedure was proposed to quantify glycerol in biodiesel.…”

Section: Introductionmentioning

confidence: 99%

“…The analyte was oxidized by sodium metaperiodate to produce formic acid, which was titrated with standardized sodium hydroxide solution. 10 Despite the simplicity of the proposed determination, the extraction of glycerol took 15 min, and required 300 g of sample per determination. It also required the adjustment of the sample acidity to minimize errors.…”

Section: Introductionmentioning

confidence: 99%

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A novel online dispersive liquid–liquid microextraction for the spectrophotometric determination of free glycerol in biodiesel

2023

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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A novel online dispersive liquid–liquid microextraction for the spectrophotometric determination of free glycerol in biodiesel

2023

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“…20 However, to attend several legislations around the world, alternative methods have being proposed to determinate the amount of biodiesel in fuels, as 1 H-NMR and ATR-FTIR. [21][22][23] Determination of free glycerol by visible absorption spectrophotometry was proposed by Bondioli and Bella. 24 Glycerol was extracted from the biodiesel and reacted with sodium metaperiodate.…”

Section: Free Glycerol In Biodieselmentioning

confidence: 99%

Determination of Free Glycerol in Biodiesel Using UV-Visible Spectroscopy: a Validation Study

Nogueira¹,

Gomes²,

Sartori³

et al. 2019

Rev. Virtual Quim.

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Resumo: Concentrações elevadas de glicerina livre em biodiesel causam danos em motores. Pela legislação brasileira, (ANP Resolução 45/2014), o limite máximo permitido para glicerina livre em biodiesel é 0,02 % em massa. A norma ASTM D6584 estabelece que o método padrão para se determinar glicerina livre em biodiesel é cromatografia gasosa, uma técnica demorada e cara. Como alternativa, a glicerina livre pode ser quantificada, após derivatização, por espectroscopia de absorção na região do UV-Visível (410 nm). No presente trabalho usamos o protocolo de validação para o método espectroscópico. Resultados indicam que o método é linear (r 2 = 0.995) para o intervalo de concentrações estudado e possui exatidão e precisão aceitáveis. O método apresentou valores de desvio padrão relativos para repetibilidade e exatidão abaixo de 5,0 %. Para o cálculo dos valores de limite de detecção e quantificação foram empregados três diferentes métodos. Dois deles apresentaram limites de quantificação apropriados para glicerina. Entretanto, o método proposto pelo INMETRO forneceu um valor maior para o limite de quantificação. Considerando que o método é baseado em reação química de derivatização, com parâmetro colorimétrico, a robustez do método foi analisada para pequenas alterações na reação em função da temperatura, do comprimento de onda e do material da cubeta. Os resultados mostraram que o método é robusto para pequenas variações na temperatura de reação, mas não é robusto para mudanças no comprimento de onda e para mudança de material da cubeta (plástico ou vidro).

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“…There are numerous analytical methods to determine FGL in biodiesel samples. Volumetric methods have been proposed, , as well as other methods based on the use of dynamic separation with different detectors (FID, MS, PAD, DAD), such as chromatography − and capillary electrophoresis . Also, NIR, fluorescence, and UV–vis spectroscopic methods − were used, avoiding a separation step.…”

Section: Introductionmentioning

confidence: 99%

Free Glycerol Sensing in Biodiesel: Automatic System Based on Sequential Enzymatic Reactions Using a Fit-for-Purpose Chemiluminescence Detection Chamber

et al. 2019

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The transesterification reaction to produce biodiesel generates a residual content of free glycerol, which may cause several problems to the engines. According to the international specification, the free glycerol determination involves a derivatization step followed by chromatographic analysis, which is done by advanced laboratories. Argentina is one of the largest biodiesel producers in the world, and part of this production is carried out by small and medium-sized producers. For those producers, this analysis is expensive and requires a considerable amount of time because there are few laboratories and they are localized far from the production site. This work proposes an alternative method for free glycerol determination in biodiesel samples taking advantage of automation, the use of an economic and available kit of enzymes, and a rapid and simple detection which was improved by the use of a fit-for-purpose chemiluminescence detection chamber designed in our laboratory. Quantification of free glycerol was performed by chemiluminescence at 425 nm after the reaction of hydrogen peroxide and luminol in the presence of Co2+. The hydrogen peroxide was generated by sequential enzymatic reactions based on the catalytic effect of glycerol kinase and glycerol phosphate oxidase. The calibration curve was linear in the 0.0045–0.0200% (w/w) range (r = 0.9910), and the sample throughput of the automatic system was 8 h–1. The geometrical configuration of the designed chemiluminescence detection chamber allowed an appropriate mixture of the reagents, due to a coupled efficient mixing system, and a highly sensitive detection (LOD value: 0.0013% (w/w)). The enzymatic method was applied for the determination of glycerol in commercial (soybean) and laboratory syntethized biodiesel samples (corn and sunflower). The trueness of the method was evaluated by comparison with the reference method (EN 14105), and a nonsignificative difference between them was observed (n = 6; P = 0.05).

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Free and Total Glycerin Analyses in Biodiesel–Diesel Blends

Cited by 8 publications

References 24 publications

A novel online dispersive liquid–liquid microextraction for the spectrophotometric determination of free glycerol in biodiesel

A novel online dispersive liquid–liquid microextraction for the spectrophotometric determination of free glycerol in biodiesel

Determination of Free Glycerol in Biodiesel Using UV-Visible Spectroscopy: a Validation Study

Free Glycerol Sensing in Biodiesel: Automatic System Based on Sequential Enzymatic Reactions Using a Fit-for-Purpose Chemiluminescence Detection Chamber

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