Simultaneous high-temperature gas chromatography with flame ionization and mass spectrometric analysis of monocarboxylic acids and acylglycerols in biofuels and biofuel intermediate products

Flanagan, Ganna; Andrianova, Anastasia A.; Casey, Jana; Hellrung, Eric; Diep, Bonnie A.; Seames, Wayne; Kubátová, Alena

doi:10.1016/j.chroma.2018.11.044

Cited by 8 publications

(8 citation statements)

References 41 publications

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“…Gas chromatography (GC) analytical techniques have been widely used in modern analysis for more than half a century [1]. Since the 1980s, with the ever-increasing demands of the petroleum industry, environmental chemistry, and catalyst chemistry, high-temperature GC analysis operated at elevated temperatures over 300 °C has been highly desired [2,3]. As one of the most important components of the GC apparatus, capillary chromatographic columns (CCs) are widely used nowadays because of their high separation efficiency.…”

Section: Introductionmentioning

confidence: 99%

Preparation and Thermal Evaluation of Novel Polyimide Protective Coatings for Quartz Capillary Chromatographic Columns Operated over 320 °C for High-Temperature Gas Chromatography Analysis

Huangfu

Zhang

et al. 2019

Polymers

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Protection of intrinsically brittle quartz chromatographic columns (CCs) from breakage or property deterioration in gas chromatography (GC) analysis has become an important research topic regarding high-temperature GC techniques. Polyimide (PI) has proved to be the most suitable protective coating for quartz CCs. In the current research, a series of novel high-temperature-resistant PI coatings for quartz CCs operated over 320 °C have been successfully prepared. For this purpose, the aromatic diamine with a rigid skeleton structure 2-(4-aminophenyl)-5-aminobenzimidazole (APBI) was copolymerized with two aromatic dianhydrides—3,3’,4,4’-benzophenotetracarboxylic acid dianhydride (BTDA) and 4,4’-oxydiphthalic anhydride (ODPA)—and an aromatic diamine with flexible ether linkages—4,4’-oxydianiline (ODA)—by a two-step polymerization procedure via soluble poly(amic acid) (PAA) precursors, followed by thermal imidization at elevated temperatures. The developed PI coatings exhibited good comprehensive properties, including glass transition temperatures (Tg) as high as 346.9 °C, measured by dynamic mechanical analysis (DMA), and coefficients of linear thermal expansion (CTEs) as low as 24.6 × 10−6/K in the range of 50–300 °C. In addition, the PI coatings exhibited good adhesion to the fused quartz capillary columns. No cracking, delamination, warpage, or other failures occurred during the 100-cycle thermal shock test in the range of 25–320 °C.

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Section: Introductionmentioning

confidence: 99%

Preparation and Thermal Evaluation of Novel Polyimide Protective Coatings for Quartz Capillary Chromatographic Columns Operated over 320 °C for High-Temperature Gas Chromatography Analysis

Huangfu

Zhang

et al. 2019

Polymers

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“…Do kluczowych, powtarzających się elementów stanowisk badawczych należy zaliczyć kolumnę z niepolarną fazą stacjonarną typu metylopolisiloksan, typu wysokotemperaturowego, dozownik on-column lub PTV oraz detektor płomieniowo-jonizacyjny FID. Podobny zestaw zastosowano w pracy Flanagan et al (2019) z tą różnicą, że dodatkowo na wylocie kolumny chromatograficznej wykorzystano splitter, umożliwiający podłączenie do spektrometru mas celem dokładniejszej identyfikacji poszczególnych acylogliceroli. Uzyskano wysoką czułość dla oznaczania acylogliceroli poniżej 1 mg/kg przy zastosowaniu reaktora krakingu dla próbki oleju sojowego.…”

Section: Rys 2 Budowa Strukturalna 13-dioleinianu Gliceroluunclassified

Badania hydrorafinatów z procesu współuwodornienia w zakresie oznaczania zawartości mono- i diacylogliceroli

Burnus

Badawczy

Wieczorek

2021

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In this work, the possibilities of using the GC-FID gas chromatography technique for determination of mono- and diacylglycerols content in the stream from the co-hydrogenation of rapeseed oil and middle distillates were investigated. Products from this process are planned to be increasingly used in the future as a new biocomponent of fuel for diesel engines. Before introducing new types of fuel components, it is necessary to test them in detail, especially in terms of residues of the fat raw material. The Regulation of the Minister of Climate of June 24, 2020 on the content of biocomponents formed as a result of co-hydrogenation indicates that the level of biomass conversion is determined on the basis of the content of triacylglycerols in the hydro-raffinate. Hence, on the basis of this determination, it is possible to assess the correctness of the co-hydrogenation process. However, other fatty components may be present in the product of this process in the form of unreacted residues. Therefore, it seems justified to carry out studies on other trace components of fatty origin in the hydro-treating material, due to the introduction of various plant materials together with petroleum hydrocarbons into the co-hydrogenation process. Due to the lack of available standardized methodologies for testing this type of products, a review of the literature was made regarding the possibility of using analytical techniques including gas and liquid chromatography to determine content of the so-called mono- and dicylglycerols, being residues of the fatty raw material, in various types of matrices, including vegetable oils and fatty acid methyl esters. In the case of examining the content of mono- and diacylglycerols in the product from the co-hydrogenation process, it was necessary to use the technique of liquid chromatography for the first-step concentration of the substances of interest. This technique made it possible to separate the sample matrix and concentrate the components to be determined prior to gas chromatographic analysis. Due to the complicated matrix of samples and the low required level of quantification, it was necessary to select appropriate conditions for removing the matrix using the classical liquid chromatography technique. A proprietary methodology for testing the content of mono- and diacylglycerols in the hydro-raffinate was developed, which was used to test selected samples of real hydro-raffinates from the co-HVO and HVO co-hydrogenation process. The ability to detect these trace fat components at a low level was indicated – as low as 2 mg/kg. The obtained sensitivity of the method allowed for additional qualitative assessment of this type of co-hydrogenation products, which are gradually gaining importance on the European market of liquid fuels.

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“…There are several methods for the analysis of free glycerol. Among these are chromatographic (the standard method ASTM D6584 [9]), amperometric, spectrophotometric, and enzymatic [7,8,[10][11][12][13][14] methods. However, the most widely and currently studied method is electrochemical, due to its analysis being less laborious, less expensive, and at the same time sensitive and fast.…”

Section: Introductionmentioning

confidence: 99%

Electrochemical Analysis of Free Glycerol in Biodiesel Using Reduced Graphene Oxide and Gold/Palladium Core-Shell Nanoparticles Modified Glassy Carbon Electrode

et al. 2021

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Glycerol is a major byproduct obtained in the production of biodiesel, an important renewable fuel. The presence of free glycerol in fuel can have structural and performance consequences with respect to the engine, making fuel quality control important. The standard method to analyze glycerol in biodiesel is gas chromatography, a time-consuming and expensive technique. In this context, an electrode based on glassy carbon electrodes (GCEs) modified with reduced graphene oxide and core-shell gold@palladium nanoparticles was developed for the determination of glycerol in biodiesel. The free glycerol analysis was performed in the aqueous phase obtained by liquid–liquid extraction from a biodiesel sample. Cyclic voltammetry was chosen as the method for glycerol electrochemical analysis to regenerate active sites and promote greater sensor stability. The modified Au@Pd/rGO/GCE electrode showed an excellent performance, obtaining a linear range of 18.2 to 109 µmol L−1 with a correlation coefficient of 0.9895, limits of detection and quantification of 5.33 and 17.6 µmol L−1, respectively, high stability during 1000 cycles, and recovery values of 86% and 87% in the quantification of glycerol in biodiesel samples. The proposed method proved to be a great alternative for the analysis of glycerol in biodiesel, being a fast, sensitive, and low-cost technique due to its high stability and the use of small quantities of reagents.

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Simultaneous high-temperature gas chromatography with flame ionization and mass spectrometric analysis of monocarboxylic acids and acylglycerols in biofuels and biofuel intermediate products

Cited by 8 publications

References 41 publications

Preparation and Thermal Evaluation of Novel Polyimide Protective Coatings for Quartz Capillary Chromatographic Columns Operated over 320 °C for High-Temperature Gas Chromatography Analysis

Preparation and Thermal Evaluation of Novel Polyimide Protective Coatings for Quartz Capillary Chromatographic Columns Operated over 320 °C for High-Temperature Gas Chromatography Analysis

Badania hydrorafinatów z procesu współuwodornienia w zakresie oznaczania zawartości mono- i diacylogliceroli

Electrochemical Analysis of Free Glycerol in Biodiesel Using Reduced Graphene Oxide and Gold/Palladium Core-Shell Nanoparticles Modified Glassy Carbon Electrode

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