Abstract
The present study is focused on the quantification of glycerides and free fatty acid in oils extracted from various seeds for biodiesel production from Indian territory. A new method based on 1H- and 13C-NMR spectroscopic techniques was developed in order to estimate triglycerides (TG), diglycerides, monoglycerides, free fatty acids (FFA) and various other components such as para-substituted phenols, silylated methyl esters, aromatic acids, naphthalenes, etc. Iodine values of the extracted oils were estimated using the developed 1H-NMR spectroscopic method, which was correlated with the TG content present in the sample. Results by the NMR method were validated by the blend preparation, fatty acid composition determined by the GC and from the iodine value of the samples. The developed method is direct, rapid and no sample treatment is required. The results from these comprehensive studies indicated that NMR spectroscopic technique is useful for the quantification of extracted oils and can be used effectively for the development and monitoring of biodiesel production and determining the fuel quality.
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References
Knothe G (2001) Historical perspectives on vegetable oil-based diesel fuels. Ind Oils 12:1103–1107
Pinto AC, Guarieiro LLN, Rezende MJC, Ribeiro NM, Torres EA, Lopes WA (2005) Biodiesel: an overview. J Braz Chem Soc 16:1313–1330
Di Serio M, Tesser R, Pengmei L, Santacesaria E (2008) Heterogeneous catalysts for biodiesel production. Energy Fuels 22:207–217
Ballesteros E, Gallego M, Valeareel M (1993) Automatic method for on-line preparation of fatty acid methyl esters from olive oil and other types of oil prior to their GC determination. Anal Chim Acta 282:581–588
Fuse T, Kusu F, Takamura K (1997) Determination of higher fatty acids in oils by high-performance liquid chromatography with electrochemical detection. J Chromatogr A 764:177–182
Lam S, Grushka E (1978) Labeling of fatty acids with 4-Bromomethyl-7-methoxycoumarin via crown ether catalyst for fluorimetric detection in high-performance liquid chromatography. J Chromatogr 158:207–224
Saad B, Ling CW, Jab MS, Lim BP, Mohamad Ali AS, Wai WT, Saleh MI (2007) Determination of free fatty acids in palm oil samples using non-aqueous flow injection titrimetric method. Food Chem 102:1407–1414
Al-Alawi A, van de Voort FR, Sedman J, Ghetler A (2006) Automated FTIR analysis of free fatty acids or moisture in edible oils. JALA 11:23–29
Sherazi STH, Mahesar SA, Bhanger MI, Van de Voort FR, Sedman J (2007) Rapid determination of free fatty acids in poultry feed lipid extracts by SB-ATR FTIR spectroscopy. J Agric Food Chem 55:4928–4932
Knothe G (2001) Monitoring a progressing transesterification reaction by fiber-optic near-infrared spectroscopy with correlation to 1H Nuclear Magnetic Resonance spectroscopy. J Am Oil Chem Soc 77:489–493
Knothe G (2001) Determining the blend level of mixtures of biodiesel with conventional diesel fuel by fiber-optic near-infrared spectroscopy and 1H Nuclear Magnetic Resonance spectroscopy. J Am Oil Chem Soc 78:1025–1028
Knothe G, Kenar JA (2004) Determination of the fatty acid profile by 1H NMR spectroscopy. Eur J Lipid Sci Tech 106:88–96
Miyake Y, Yokomizo K, Matsuzaki N (1998) Determination of unsaturated fatty acid composition by high-resolution Nuclear Magnetic Resonance spectroscopy. J Am Oil Chem Soc 75:1091–1094
Miyake Y, Yokomizo K, Matsuzaki N (1998) Rapid determination of iodine value by 1H Nuclear Magnetic Resonance spectroscopy. J Am Oil Chem Soc 75:15–19
Sarpal AS, Kapur GS, Mukherjee S, Jayaparkash KC, Jain SK (1994) Determination of iodine value of lubricating oils by nuclear magnetic resonance (NMR) spectroscopy. Lubric Eng 51(3):209–214
Van Duynhoven J, Goudappel GJ, Gribnau MCM, Shukla VKS (1999) Solid fat content determination by NMR. INFORM 10:479–484
Satyarthi JK, Srinivas D, Ratnasamy P (2009) Estimation of free fatty acid content in oils, fats, and biodiesel by 1H NMR spectroscopy. Energy Fuels 23(4):2273–2277
Wollenberg KF (1990) Quantitative high resolution 13C NMR of the olefinic and carbonyl carbons of edible vegetable oils. J Am Oil Chem Soc 67:487–492
Shiao TY, Shiao MS (1989) Determination of fatty acid compositions of triacylglycerols by high resolution NMR spectroscopy. Bot Bull Academia Sinica 30:191–194
Wollenberg KF (1991) Quantitative triacylglycerol analyses of whole vegetable seeds by 1H and 13C magic angle sample spinning NMR spectroscopy. J Am Oil Chem Soc 68:391–395
Ajiwe VIE, Obika AE (2000) African pear seed oil: potential alternative source to diesel oil. Energy Fuels 14:112–116
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The authors wish to acknowledge the Management of IOC, R&D Faridabad for allowing them to publish the present work.
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Kumar, R., Bansal, V., Tiwari, A.K. et al. Estimation of Glycerides and Free Fatty Acid in Oils Extracted From Various Seeds from the Indian Region by NMR Spectroscopy. J Am Oil Chem Soc 88, 1675–1685 (2011). https://doi.org/10.1007/s11746-011-1846-4
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DOI: https://doi.org/10.1007/s11746-011-1846-4