Determination of Iodine Value Using Alternative Solvent to Carbon Tetrachloride

High-resolution 1 H nuclear magnetic resonance ( 1 H NMR) has been found to be an effective tool for the direct, rapid, and automated determination of the iodine value (IV) of vegetable oils, including hydrogenated oils (IV = 45.9-140.2). The total time required to obtain the 1 H NMR data is about 3 min per sample. The IV is calculated from the number of double-bonded protons and the average molecular weight derived directly from the spectrum. The average of olefinic protons and allylic plus divinyl protons area was used to calculate the absolute number of double-bonded protons. The 1 H NMR results were compared with those obtained by the traditional Wijs-cyclohexane methods. The correlation coefficient between traditional IV and the novel 1 H NMR method was r 2 = 0.9994 for the regression equation Y = 0.9885X + 2.8084, where X was the result given by the traditional method. With the proposed regression equation, IV calculated by the 1 H NMR method was within an error of ±1 unit of the result obtained by the traditional method. The proposed method is practically viable if one can afford to have the NMR system. JAOCS 75, 15-19 (1998).

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“…Traditional IV was measured according to AOCS Method Cd 1-25 with slight modification. Cyclohexane was used instead of carbon tetrachloride (10).…”

Section: Methodsmentioning

confidence: 99%

Rapid determination of iodine value by ¹H nuclear magnetic resonance spectroscopy

Miyake

Yokomizo

Matsuzaki

1998

J Americ Oil Chem Soc

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“…1,2 It is measured by the standard method EN 14111 based on iodometry−potentiometry. 3,4 Analytical techniques such as chromatography (GC and GC-MS) 5−10 and spectroscopy (NMR and IR) 11−31 are being used extensively for neutral lipid content, fatty acid profiling, reaction monitoring, and quality control of biodiesel produced from diverse sources of vegetable oils and microbial oils (algae and yeast). High-resolution nuclear magnetic resonance (NMR) spectroscopic techniques (1D, 2D, and 3D) offer many advantages over existing analytical methods due to ease of direct, rapid, simultaneous, and nondestructive analysis in the multicomponent systems of oils and biodiesel from various sources.…”

Section: Introductionmentioning

confidence: 99%

“…These specifications are intended to produce B100 biodiesel suitable for blending with conventional diesel to ensure that the product meets the technical requirements of modern diesel engines . The iodine value (IV; g of I 2 /(100 g)), which determines the degree of the unsaturation of oils and biodiesels, is one of the most important quality parameters responsible for deciding the oxidation stability, combustion, pour point, and cetane number characteristics. , It is measured by the standard method EN 14111 based on iodometry–potentiometry. , …”

Section: Introductionmentioning

confidence: 99%

Direct Method for the Determination of the Iodine Value of Biodiesel by Quantitative Nuclear Magnetic Resonance (q¹H NMR) Spectroscopy

Sarpal

Silva

et al. 2015

Energy Fuels

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A direct, rapid, and convenient method for the determination of iodine value (IV) of biodiesels from vegetable oils has been developed by the application of nuclear magnetic resonance (500 and 600 MHz 1 H NMR) techniques. The method is based on the correlation of integrated intensities (I us ) of unsaturated hydrogen in the 1 H NMR spectra of biodiesels with (1) the predetermined iodine values by the standard iodometry based method (EN 14111), ( 2) iodine values determined from the fatty acid profile by GC-MS method, and (3) iodine values from the absolute number of double bonds (ADB) determined by 1 H NMR. The simple mathematical equation, IV = K(I us ) (K = 15.78), derived from the correlations, provides a direct method for the determination of iodine value in the range of 5−140 g of I 2 /(100 g). The constant "K" has been found to be independent of the nature and source of vegetable oils. It is equally applicable to blends of biodiesels, blends of biodiesel and oils in all proportions, and biodiesel samples containing glyceride impurities. The statistical comparison between NMR, EN 14111, and GC-MS methods indicates that NMR method provides equivalent results with acceptable precision. The quantitative NMR (q 1 H NMR) protocol for the optimization of acquisition and processing parameters have been established for achieving better precision on 500 and 600 MHz instruments.

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Determination of Iodine Value Using Alternative Solvent to Carbon Tetrachloride

Cited by 2 publications

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Rapid determination of iodine value by ¹H nuclear magnetic resonance spectroscopy

Rapid determination of iodine value by ¹H nuclear magnetic resonance spectroscopy

Direct Method for the Determination of the Iodine Value of Biodiesel by Quantitative Nuclear Magnetic Resonance (q¹H NMR) Spectroscopy

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Determination of Iodine Value Using Alternative Solvent to Carbon Tetrachloride

Cited by 2 publications

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Rapid determination of iodine value by 1H nuclear magnetic resonance spectroscopy

Rapid determination of iodine value by 1H nuclear magnetic resonance spectroscopy

Direct Method for the Determination of the Iodine Value of Biodiesel by Quantitative Nuclear Magnetic Resonance (q1H NMR) Spectroscopy

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Product

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Rapid determination of iodine value by ¹H nuclear magnetic resonance spectroscopy

Rapid determination of iodine value by ¹H nuclear magnetic resonance spectroscopy

Direct Method for the Determination of the Iodine Value of Biodiesel by Quantitative Nuclear Magnetic Resonance (q¹H NMR) Spectroscopy