Validation of a GC–IDMS method for the metrologically traceable quantification of selected FAMEs in biodiesel

Morales, Valle; Goren, Ahmet C.; Held, Andrea; Bílsel, Mine; Gündüz, Simay; Yilmaz, Hasibe

doi:10.1007/s00769-015-1144-1

Cited by 4 publications

(5 citation statements)

References 4 publications

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“…The critical interpretation of the spectrum has revealed the presence of mostly I-MG and 1,2-DG whose nature were found to be similar to residual glycerides identified in case of transesterified products of different vegetable oils. 3,4) were confirmed from the appearance of their characteristic signals. The concentration of these residual glycerides is higher compared to those observed in the CRM NIST2772 b as evident from the intensities of these components shown in the same (Figure 15b).…”

Section: Monitoring Development Standardization and Quality Aspects Of Crm Of Soya Based Biodiesel During Their Production Processmentioning

confidence: 84%

“…Quality control and assessment of biodiesel (B100) production are related to determination of 22 parameters of physical and chemical characteristics such as total ester content, free fatty acid value, glycerides (mono, di, tri), free glycerin and total glycerin contents, iodine value, calorific value, cetane number, flash point, ash content, refractive index, viscosity, density, fatty acid profile, linolenic ester content (C18:3), PUFA content etc. as specified in the standards ASTM D6751 and EN14214 (European Committee for Standardization (CEN) [1][2][3][4][5][6][7][8][9][10]. These standards define product specifications and measurement methods for biodiesel to be used as automotive and aviation fuels.…”

Section: Introductionmentioning

confidence: 99%

“…These materials consist of pure organic compounds to be used for calibration as well as wide range of complex matrix materials for validation or development of analytical techniques and methods for numerous products [9]. Certified reference materials are needed to give laboratories the possibility to demonstrate their method proficiency, proper working of their instruments, and check the performance and validation of their own developed or standard analytical methods [1][2][3][4][5][6][7][8][9][10].…”

Section: Introductionmentioning

confidence: 99%

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Monitoring of Development of Certified Reference Material of Biodiesel by High Field NMR Spectroscopic Techniques

Sarpal¹,

Silva²,

Monteiro³

et al. 2016

JMT

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Analytical strategies based on Nuclear Magnetic Resonance (NMR) (500 MHz and 800 MHz) spectroscopic techniques ( 1 H, 13 C, 13 C-DEPT) have been presented for monitoring the development of Certified Reference Material (CRM) of biodiesel meeting ASTM D 6751/EN 14214 specifications. The protocol includes the analyses of feedstocks of oil and biodiesel, and impurities generated during transesterification reaction by NMR methods duly validated by standard methods based on GC-MS. The quality parameters such as contents of ester (B100), linolenic acid (C18:3), poly unsaturated fatty acids (PUFA), residual acyl glycerides (mono, di, tri), free glycerin and fatty acid profile, and iodine values have been determined directly by newly developed methods based on NMR techniques in samples of biodiesel produced by transesterification reaction of soybean, sunflower, cotton, canola and corn (maize) oils drawn at different interval of times. The systematic 1H and 13C NMR spectral interpretation has revealed the presence of five types of residual glycerides (AGs) namely 1 or 2 mono glycerides (1-MG, 2-MG); 1,2 and 1,3 di glycerides (1,2-DG; 1,3-DG) and triglycerides (1,2,3-TG) in the biodiesel as well as transesterified products independent of types and nature of vegetable oils. The spectral analyses of samples at 800 MHz NMR instrument has provided enhanced sensitivity and resolution of signals of interest, which enabled identification of very low levels of various AGs. The repeatability standard Deviation (%SD) of quality parameters show that the NMR methods provide results with acceptable precision. The accurate and rapid profiling of residual impurities generated during transesterification reaction without any further chemical treatment will be an effective guide for the catalyst developer for the syntheses of novel catalysts required for quality control of biodiesel. A rapid and convenient approach has been described for the analyses and quantification of bound and free glycerin in the biodiesel and transesterified products, which will enable rapid quality assessment and certification of CRMs.

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Section: Monitoring Development Standardization and Quality Aspects Of Crm Of Soya Based Biodiesel During Their Production Processmentioning

confidence: 84%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Monitoring of Development of Certified Reference Material of Biodiesel by High Field NMR Spectroscopic Techniques

Sarpal¹,

Silva²,

Monteiro³

et al. 2016

JMT

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“…16 Biodiesel must be in accordance with a set of quality parameters to be employed, that includes purity and impurities contents; performance characteristics, as cetane number, oxidative stability; and physical properties, as viscosity, and specific mass. 19 The purity of biodiesel is expressed as esters content, and can be estimated by several instrumental techniques, as gas chromatography-flame ionization detector (GC-FID), [20][21][22][23][24][25][26][27][28][29][30][31][32][33][34][35][36][37][38][39] gas chromatography-mass selective detector (GC-MSD), 22,38,[40][41][42][43][44][45][46] high performance liquid chromatography--evaporative light scattering detector (HPLC-ELSD), [22][23][24][25]47,48 high performance liquid chromatography-refractive index detector (HPLC-RID), 49 high performance liquid chromatography-variable wavelength detector (HPLC-VWD), 23,32,34 gel permeation chromatography (GPC), 23 high performance thin layer chromatography (HPTLC), 50 nuclear magnetic resonance (NMR), …”

Section: Introductionmentioning

confidence: 99%

GC-FID methodology validation for the fatty esters content determination in biodiesel with hexadecyl acetate as the internal standard

et al. 2017

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Biodiesel purity expressed as fatty esters content is one of its most important quality parameters. Although several instrumental methods have been employed, gas chromatography with internal standard calibration has been the most used. Biodiesel is a very complex matrix, therefore finding a suitable internal standard (IS) is not straightforward. EN14103:2003 standard established methyl heptadecanoate (C17:0) as IS. Since this fatty ester is naturally present in some biodiesel feedstock as tallow, that standard was reviewed in 2011, and methyl nonadecanoate (C19:0) became the new IS. In turn, C19:0 produces a peak on the chromatogram that is difficult to resolve from methyl linoeate (C18:2) and metyl linolenate (C18:3) ones. In this paper, a GC-FID method for the determination of the esters content in methyl and ethyl biodiesel from canola and soy oils, using hexadecyl acetate as a new internal standard was validated. EN14103:2003 was used as reference method. Method selectivity, accuracy (t student parameter < 2.18 from both methods), repeatability (0.1 -0.4%), intermediate precision (0.2 -1.8%), and robustness (0.1 -1.6%) were investigated and considered appropriate for the scope.

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“…The results were evaluated statistically, and the distribution of fatty acid composition in sunflower oil was determined. The composition of fatty acids (as methyl ester derivatives) in sunflower oil was also investigated in TÜBİTAK UME laboratories by gas chromatography-mass spectrometry (GC-MS) [9,10].…”

Section: Introductionmentioning

confidence: 99%

Proficiency testing performance of Turkish laboratories on determination of relative composition of fatty acids in sunflower oil

Yilmaz¹,

Gündüz²,

Akcadag³

2017

J.Chem.Metrol.

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Proficiency testing of laboratories in Turkey to compare and evaluate their performances on analysis of fatty acids in sunflower oil was performed. Analysis of the quality control test material allows the laboratory to compare the analytical results with other laboratories. In order to increase the quality of chemical analysis and awareness of metrology, TÜBİTAK UME have been organizing Proficiency Testing Schemes in the field of determination of fatty acids in sunflower oil since 2005. In this study, an overview of the proficiency test for the determination of fatty acids in sunflower oil in Turkey is presented.

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Validation of a GC–IDMS method for the metrologically traceable quantification of selected FAMEs in biodiesel

Cited by 4 publications

References 4 publications

Monitoring of Development of Certified Reference Material of Biodiesel by High Field NMR Spectroscopic Techniques

Monitoring of Development of Certified Reference Material of Biodiesel by High Field NMR Spectroscopic Techniques

GC-FID methodology validation for the fatty esters content determination in biodiesel with hexadecyl acetate as the internal standard

Proficiency testing performance of Turkish laboratories on determination of relative composition of fatty acids in sunflower oil

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