Quantitative and qualitative analysis of biodiesel by NMR spectroscopic methods

Doudin, Khalid

doi:10.1016/j.fuel.2020.119114

Cited by 50 publications

(26 citation statements)

References 28 publications

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“…1 H NMR and 13 C NMR spectra of the castor kernel oil obtained by a nonreactive extraction process and castor methyl ester produced by a reactive extraction process obtained at optimum conditions are shown in Figures , , and , respectively. NMR spectra can be used to know the functional groups present in the sample and the conversion status of triglycerides into biodiesel Figure shows the 1 H NMR spectra of virgin castor kernel oil and the final product after transesterification (castor kernel oil FAME) using reactive extraction methods, respectively.…”

Section: Resultssupporting

confidence: 89%

“…This ester group (C–O) was observed at about 1159 cm –1 in the castor seed kernel, but it was shifted to 1170 cm –1 in the case of castor kernel methyl ester. This signature signifies that the oil extracted from the kernel using the reactive extraction process was converted into FAME. ,, Further, the presence of a band at around 1439 cm –1 for the methyl group (−O–CH 3 ) and 1170 cm –1 for the ester group simultaneously indicated the formation of castor kernel oil fatty acid methyl ester (Figure ). …”

Section: Resultsmentioning

confidence: 94%

“…This signature signifies that the oil extracted from the kernel using the reactive extraction process was converted into FAME. 48,72,73 Further, the presence of a band at around 1439 cm −1 for the methyl group (−O−CH 3 ) and 1170 cm −1 for the ester group simultaneously indicated the formation of castor kernel oil fatty acid methyl ester (Figure 7). 54 NMR Analysis.…”

Section: Characterization Of Nonreactive (Cko) and Reactive Extractio...mentioning

confidence: 99%

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Reactive Extraction for Fatty Acid Methyl Ester Production from Castor Seeds Using a Heterogeneous Base Catalyst: Process Parameter Optimization and Characterization

Mamuye

Reshad

2022

ACS Omega

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Fatty acid methyl ester (FAME) from oil seeds is conventionally produced via a two/three-process-step method: extraction of oil and subsequent esterification/transesterification to fatty FAME (biodiesel). However, in the present study, we investigated the production of castor kernel oil (CKO) FAME by reactive extraction for extraction and transesterification in a single process using a heterogeneous catalyst. The content of oil that can be extracted was checked by investigating several nonreactive extraction parameters such as solvent type (polar, nonpolar, and mixture), the solvent to kernel ratio, and extraction time. Maximum oil was extracted using methanol as a solvent with a methanol-to-seed ratio of 6.25:1 for 6 h extraction time. The viscosity of CKO obtained by nonreactive extraction was reduced from 288.83 to 19.04 mm2/s by reactive extraction using a 4.09 wt % catalyst concentration (BaO) and a 330.9:1 methanol-to-oil molar ratio for 6 h reaction time at 64 °C. Reactive extraction for transesterification of CKO was performed using BaO, CaO, and ZnO heterogeneous catalysts. BaO results in the increased yield of CKO FAME compared to other catalysts. Central composite design (CCD) using the response surface methodology (RSM) was implemented to design the experimental matrix, process parameter optimization, maximize the yield of CKO FAME, and investigate interaction effects of parameters such as reactive extraction temperature (55–65 °C), catalyst concentration (3–5 wt %), and methanol-to-oil molar ratio (175:1–350:1) on the yield of CKO FAME. A second-order model equation with a p-value < 0.05 and an R 2 value near 1.0 was obtained to predict the yield using the input parameters. The maximum yield CKO FAME of 96.13 wt % with 94.4% purity of produced CKO FAME was obtained at a catalyst concentration of 4.09 wt % and a methanol-to-oil molar ratio of 330.9:1 for 6 h with a reaction temperature of 64 °C. Therefore, a comparable conversion of castor seed oil triglyceride (96.13 wt %) was obtained in a single step directly from castor seeds. Furthermore, the rheological behavior investigation of castor kernel oil and castor methyl ester revealed that the dynamic viscosity of both samples was found to be dependent on triglyceride content and temperature.

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Section: Resultssupporting

confidence: 89%

Section: Resultsmentioning

confidence: 94%

Section: Characterization Of Nonreactive (Cko) and Reactive Extractio...mentioning

confidence: 99%

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Reactive Extraction for Fatty Acid Methyl Ester Production from Castor Seeds Using a Heterogeneous Base Catalyst: Process Parameter Optimization and Characterization

Mamuye

Reshad

2022

ACS Omega

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“…The signals at 0.8 ppm related to terminal methyl hydrogens (-CH 3 -), a strong signal at 1.2 ppm from the methylene of carbon chain (-CH 2 -), a signal at 1.6 ppm from the β-carbonyl methylene, and signals associated with unsaturation at 2.0, 2.8 and 5.3 ppm, assigned to allylic, bisallylic and olefinic hydrogens, respectively. For instance, a broad peak originated at 5.3 ppm corresponds to hydrogens of unsaturated double bonds due to -CH=CH-and from -CH=CH-CH=CH-protons either from isolated and nonconjugated double bonds [46]. Biodiesel purity was > 96.3% as estimated by 1 H NMR (Table 4) depicts the fuel properties of the Jatropha-derived biodiesel (FAME) with American Society for Testing and Materials standard (ASTM D 6751) and compared with Indian standards (IS 15607) specification for biodiesel.…”

Section: Quantification Of Methyl Estermentioning

confidence: 99%

Synthesis of Ca–Fe-based heterogeneous catalyst from waste shells and their application for transesterification of Jatropha oil

Semwal

Raj

Patel

et al. 2022

Syst Microbiol and Biomanuf

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The depletion of fossil fuel reserves with increased fuel demand and global emissions has increased the search for ecofriendly renewable fuels with a low environmental impact. Biodiesel can be considered as mono-alkyl esters of long-chain fatty acids obtained from the transesterification of vegetable oils and animal fats. Economically low-cost biodiesel production has received considerable interest for blending with fossil-based diesel for a more sustainable future. Therefore, the current study focuses on synthesizing an efficient, low-cost heterogeneous CaO catalyst from waste egg and seashell using a solidstate method and applying it to the transesterification of Jatropha oil. The Ca 2 Fe 2 O 5 solid catalyst was prepared by doping calcined CaO with iron in a 2:1 ratio using ferric oxide (Fe 2 O 3 ). Furthermore, the catalyst was extruded and analytically characterized using XRD, FT IR, BET, and its basic strength was quantified by Hammett indicators. Later on, transesterification of Jatropha oil was optimized by varying reaction parameters, such as the molar ratio of methanol to Jatropha oil, reaction time, and catalyst loading. The maximum conversion yield was 96.3% at a 20:1 methanol-to-oil ratio and 80 bar N 2 pressure using 5% (w/w) catalyst loading. Furthermore, the catalytic recycling study demonstrated that the Ca 2 Fe 2 O 5 catalyst could retain > 70-80% of transesterification efficiency and stability up to 4 cycles under high acid value and moisture conditions.

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“…Nuclear Magnetic Resonance (NMR) spectroscopy and Fourier Transform Infrared (FTIR) spectrometry have lately been employed to monitor biodiesel production. NMR is a powerful method that is currently underutilised in biodiesel analysis [258]. Although FTIR is one of the well-established methods for analysing biodiesel, it is less sensitive for detecting tiny components than Gas Chromatography (GC).…”

Section: Analytical Technique To Determine Chemical Properties Of Biodieselmentioning

confidence: 99%

A Short Review on Catalyst, Feedstock, Modernised Process, Current State and Challenges on Biodiesel Production

et al. 2021

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Biodiesel, comprising mono alkyl fatty acid esters or methyl ethyl esters, is an encouraging option to fossil fuels or diesel produced from petroleum; it has comparable characteristics and its use has the potential to diminish carbon dioxide production and greenhouse gas emissions. Manufactured from recyclable and sustainable feedstocks, e.g., oils originating from vegetation, biodiesel has biodegradable properties and has no toxic impact on ecosystems. The evolution of biodiesel has been precipitated by the continuing environmental damage created by the deployment of fossil fuels. Biodiesel is predominantly synthesised via transesterification and esterification procedures. These involve a number of key constituents, i.e., the feedstock and catalytic agent, the proportion of methanol to oil, the circumstances of the reaction and the product segregation and purification processes. Elements that influence the yield and standard of the obtained biodiesel encompass the form and quantity of the feedstock and reaction catalyst, the proportion of alcohol to feedstock, the temperature of the reaction, and its duration. Contemporary research has evaluated the output of biodiesel reactors in terms of energy production and timely biodiesel manufacture. In order to synthesise biodiesel for industrial use efficaciously, it is essential to acknowledge the technological advances that have significant potential in this sector. The current paper therefore offers a review of contemporary progress, feedstock categorisation, and catalytic agents for the manufacture of biodiesel and production reactors, together with modernised processing techniques. The production reactor, form of catalyst, methods of synthesis, and feedstock standards are additionally subjects of discourse so as to detail a comprehensive setting pertaining to the chemical process. Numerous studies are ongoing in order to develop increasingly efficacious techniques for biodiesel manufacture; these acknowledge the use of solid catalytic agents and non-catalytic supercritical events. This review appraises the contemporary situation with respect to biodiesel production in a range of contexts. The spectrum of techniques for the efficacious manufacture of biodiesel encompasses production catalysed by homogeneous or heterogeneous enzymes or promoted by microwave or ultrasonic technologies. A description of the difficulties to be surmounted going forward in the sector is presented.

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Quantitative and qualitative analysis of biodiesel by NMR spectroscopic methods

Cited by 50 publications

References 28 publications

Reactive Extraction for Fatty Acid Methyl Ester Production from Castor Seeds Using a Heterogeneous Base Catalyst: Process Parameter Optimization and Characterization

Reactive Extraction for Fatty Acid Methyl Ester Production from Castor Seeds Using a Heterogeneous Base Catalyst: Process Parameter Optimization and Characterization

Synthesis of Ca–Fe-based heterogeneous catalyst from waste shells and their application for transesterification of Jatropha oil

A Short Review on Catalyst, Feedstock, Modernised Process, Current State and Challenges on Biodiesel Production

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