Determination of the iodine value of biodiesel using 1H NMR with 1,4-dioxane as an internal standard

Oromí-Farrús, Mireia; Villorbina, Gemma; Eras, Jordi; Gatius, Ferran; Torres, Mercè; Canela, Ramón

doi:10.1016/j.fuel.2010.06.016

Cited by 20 publications

(13 citation statements)

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“…To study the effect of relaxation delay on the quantitative analyses, the spectra of two extracts (SNDWCSPS, CHLW CSPS) and soybean oil were recorded under relaxation delays of 5, 10, and 15 s, and the integral areas of functional groups were measured. The results did not show any variation in the integral intensities of protons of functional groups of esters, unsaturations, methyls, etc., at relaxation delays of 10 and 15 s. Similar observations were reported in our earlier work on the analysis of yeast extracts [26] and also by Oromí-Farrús et al [13] in their work on the analysis of biodiesels. The following parameters were used for each recording: relaxation delay 10 s; acquisition time 3.4 s, 90°pulse width 8.13-8.64 μs; number of scans 16 or 32, chemical shift range 0-12 ppm.…”

Section: Nmr Recordingssupporting

confidence: 90%

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Determination of lipid content of oleaginous microalgal biomass by NMR spectroscopic and GC–MS techniques

et al. 2015

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Direct methods based on (1)H NMR spectroscopic techniques have been developed for the determination of neutral lipids (triglycerides and free fatty acids) and polar lipids (glyceroglycolipids/phospholipids) in the solvent extracts of oleaginous microalgal biomasses cultivated on a laboratory scale with two species in different media. The chemical shift assignments observed in the (1)H and (13)C NMR spectra corresponding to unsaturated (C18:N, N = 1-3, C20:3, C20:5, C22:6, epoxy) and saturated (C14-C18) fatty acid ester components in a complex matrix involving overlapped resonances have been unambiguously confirmed by the application of 2D NMR spectroscopy (total correlation spectroscopy and heteronuclear single quantum coherence-total correlation spectroscopy). The study of the effect of a polar lipid matrix on the determination of neutral lipids by an internal reference blending process by a systematic designed experimental protocol has provided absolute quantification. The fatty acid composition of algal extracts was found to be similar to that of vegetable oils containing saturated (C16-C18:0) and unsaturated (C18:N, N = 1-3, C20:N, N = 3-4, C22:6) fatty acids as confirmed by NMR spectroscopy and gas chromatography-mass spectrometry analyses. The NMR methods developed offer great potential for rapid screening of algal strains for generation of algal biomass with the desired lipid content, quality, and potential for biodiesel and value-added polyunsaturated fatty acids in view of the cost economics of the overall cost of generation of the biomass.

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Section: Nmr Recordingssupporting

confidence: 90%

“…PUFA polyunsaturated fatty acid a Terminal methyls of saturated (C14-C18) and unsaturated (C18:1, C18:2) fatty components Table 5 for peak assignment 13 C NMR chemical shifts of the characteristic signals due to different components of various algal extracts are summarized in Table 5.…”

Section: H Nmr Spectral Features Of Algal Extractsmentioning

confidence: 99%

Determination of lipid content of oleaginous microalgal biomass by NMR spectroscopic and GC–MS techniques

et al. 2015

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“…D content(%) was calculated by the internal standard method and obtained from relative proton ( 1 H) integration ratio between deuterated compounds ( 1 and 2 ) and 1,4‐dioxane as an internal standard . D content(%) of deuterated compound can be calculated using the following formula:

Starting material yield (%) = \frac{^{1} H NMR Integral of starting material}{^{1} H NMR Integral of internal standard} \times n

n : The ratio of the internal standard to the initial amount of starting material.

normalD content (() %) = 100 % - starting material yield (() %)

…”

Section: Methodsmentioning

confidence: 99%

Microwave‐assisted Efficient H/D Exchange Method of 9H‐Carbazole and 2‐Phenylpyridine as Organic Light‐emitting Materials

Kim

Lim

2019

Bulletin Korean Chem Soc

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“…[168][169][170] Given that the fatty acid composition of the base oil principally affects the CN of biodiesel, prediction of this parameter was also proposed by employing ANN, 171,172 with the possibility of obtaining a model with an accuracy >92%. 174 Furthermore, structural data for biodiesel samples derived from 1 H NMR spectra combined with multivariate techniques also allowed inference of CN. 1 H NMR was also employed for the determination of the iodine value using 1,4-dioxane as an internal standard, allowing analysis with smaller samples than required for the iodometric method.…”

Section: Other Alternativesmentioning

confidence: 99%

Greener procedures for biodiesel quality control

2015

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Biodiesel analysis often requires large amounts of chemicals and organic solvents with consequent generation of large waste volumes. However, several environmentally friendly alternatives have been presented for assay of biodiesel quality control parameters. These approaches include direct analysis with reagentless procedures, improved sample preparation by dilution or analyte extraction with nontoxic solvents, preparation of emulsions or microemulsions, and sample mineralisation under mild conditions as well as strategies for minimization of reagent consumption and waste generation. These greener alternatives are critically reviewed, highlighting the advantages and limitations of each approach in biodiesel analysis. Alternative analytical techniques (e.g. flow analysis and electrochemical detection), predictive studies, and measurement of physicochemical parameters are also discussed. A two-nozzle FBMN for nebulisation of biodiesel samples and water, avoiding acid digestion Ca, K, Mg, Na, and P: 0.005-0.5; minor components: 0.001-3 45 4400 | Anal. Methods, 2015, 7, 4396-4418 This journal is

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Determination of the iodine value of biodiesel using 1H NMR with 1,4-dioxane as an internal standard

Cited by 20 publications

References 14 publications

Determination of lipid content of oleaginous microalgal biomass by NMR spectroscopic and GC–MS techniques

Determination of lipid content of oleaginous microalgal biomass by NMR spectroscopic and GC–MS techniques

Microwave‐assisted Efficient H/D Exchange Method of 9H‐Carbazole and 2‐Phenylpyridine as Organic Light‐emitting Materials

Greener procedures for biodiesel quality control

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