Method development for the characterization of biofuel intermediate products using gas chromatography with simultaneous mass spectrometric and flame ionization detections

► A GC–FID/MS method for biofuels and their intermediate products was developed. ► The method was based on parallel identification using MS and quantification with FID. ► The quantification accounted for unidentified, unresolved, and acidic species. ► The PTV injection conditions were optimized to m...

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Veröffentlicht in:Journal of Chromatography A 2012-02, Vol.1224, p.79-88
Hauptverfasser: Šťávová, Jana, Stahl, Danese C., Seames, Wayne S., Kubátová, Alena
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container_start_page 79
container_title Journal of Chromatography A
container_volume 1224
creator Šťávová, Jana
Stahl, Danese C.
Seames, Wayne S.
Kubátová, Alena
description ► A GC–FID/MS method for biofuels and their intermediate products was developed. ► The method was based on parallel identification using MS and quantification with FID. ► The quantification accounted for unidentified, unresolved, and acidic species. ► The PTV injection conditions were optimized to minimize discrimination. Accurate analytical methods are required to develop and evaluate the quality of new renewable transportation fuels and intermediate organic liquid products (OLPs). Unfortunately, existing methods developed for the detailed characterization of petroleum products, are not accurate for many of the OLPs generated from non-petroleum feedstocks. In this study, a method was developed and applied to the detailed characterization of complex OLPs formed during triacylglyceride (TG) pyrolysis which is the basis for generating one class of emerging biofuels. This method uses gas chromatography coupled simultaneously with flame ionization and mass spectrometry detectors (GC–FID/MS). The FID provided accurate quantification of carbonaceous species while MS enabled identification of unknown compounds. A programed temperature vaporizer using a 25 °C, 0.1 min, 720 °C min −1, 350 °C, 5 min temperature program is employed which minimizes compound discrimination better than the more commonly utilized split/splitless injector, as verified with injections at 250 and 350 °C. Two standard mixtures featuring over 150 components are used for accurate identification and a designed calibration standard accounts for compound discrimination at the injector and differing FID responses of various classes of compounds. This new method was used to identify and quantify over 250 species in OLPs generated from canola oil, soybean oil, and canola methyl ester (CME). In addition to hydrocarbons, the method was used to quantify polar (upon derivatization) and unidentified species, plus the unresolved complex mixture that has not typically been determined in previous studies. Repeatability of the analytical method was below 5% RSD for all individual components. Using this method, the mass balance was closed for samples derived from canola and soybean oil but only ca. 77 wt% of the OLP generated from CME could be characterized. The ability to close the mass balance depended on sample origin, demonstrating the need for an accurate quantification method for biofuels at various stages of production.
doi_str_mv 10.1016/j.chroma.2011.12.013
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Accurate analytical methods are required to develop and evaluate the quality of new renewable transportation fuels and intermediate organic liquid products (OLPs). Unfortunately, existing methods developed for the detailed characterization of petroleum products, are not accurate for many of the OLPs generated from non-petroleum feedstocks. In this study, a method was developed and applied to the detailed characterization of complex OLPs formed during triacylglyceride (TG) pyrolysis which is the basis for generating one class of emerging biofuels. This method uses gas chromatography coupled simultaneously with flame ionization and mass spectrometry detectors (GC–FID/MS). The FID provided accurate quantification of carbonaceous species while MS enabled identification of unknown compounds. A programed temperature vaporizer using a 25 °C, 0.1 min, 720 °C min −1, 350 °C, 5 min temperature program is employed which minimizes compound discrimination better than the more commonly utilized split/splitless injector, as verified with injections at 250 and 350 °C. Two standard mixtures featuring over 150 components are used for accurate identification and a designed calibration standard accounts for compound discrimination at the injector and differing FID responses of various classes of compounds. This new method was used to identify and quantify over 250 species in OLPs generated from canola oil, soybean oil, and canola methyl ester (CME). In addition to hydrocarbons, the method was used to quantify polar (upon derivatization) and unidentified species, plus the unresolved complex mixture that has not typically been determined in previous studies. Repeatability of the analytical method was below 5% RSD for all individual components. Using this method, the mass balance was closed for samples derived from canola and soybean oil but only ca. 77 wt% of the OLP generated from CME could be characterized. 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A programed temperature vaporizer using a 25 °C, 0.1 min, 720 °C min −1, 350 °C, 5 min temperature program is employed which minimizes compound discrimination better than the more commonly utilized split/splitless injector, as verified with injections at 250 and 350 °C. Two standard mixtures featuring over 150 components are used for accurate identification and a designed calibration standard accounts for compound discrimination at the injector and differing FID responses of various classes of compounds. This new method was used to identify and quantify over 250 species in OLPs generated from canola oil, soybean oil, and canola methyl ester (CME). In addition to hydrocarbons, the method was used to quantify polar (upon derivatization) and unidentified species, plus the unresolved complex mixture that has not typically been determined in previous studies. Repeatability of the analytical method was below 5% RSD for all individual components. Using this method, the mass balance was closed for samples derived from canola and soybean oil but only ca. 77 wt% of the OLP generated from CME could be characterized. 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Accurate analytical methods are required to develop and evaluate the quality of new renewable transportation fuels and intermediate organic liquid products (OLPs). Unfortunately, existing methods developed for the detailed characterization of petroleum products, are not accurate for many of the OLPs generated from non-petroleum feedstocks. In this study, a method was developed and applied to the detailed characterization of complex OLPs formed during triacylglyceride (TG) pyrolysis which is the basis for generating one class of emerging biofuels. This method uses gas chromatography coupled simultaneously with flame ionization and mass spectrometry detectors (GC–FID/MS). The FID provided accurate quantification of carbonaceous species while MS enabled identification of unknown compounds. A programed temperature vaporizer using a 25 °C, 0.1 min, 720 °C min −1, 350 °C, 5 min temperature program is employed which minimizes compound discrimination better than the more commonly utilized split/splitless injector, as verified with injections at 250 and 350 °C. Two standard mixtures featuring over 150 components are used for accurate identification and a designed calibration standard accounts for compound discrimination at the injector and differing FID responses of various classes of compounds. This new method was used to identify and quantify over 250 species in OLPs generated from canola oil, soybean oil, and canola methyl ester (CME). In addition to hydrocarbons, the method was used to quantify polar (upon derivatization) and unidentified species, plus the unresolved complex mixture that has not typically been determined in previous studies. Repeatability of the analytical method was below 5% RSD for all individual components. Using this method, the mass balance was closed for samples derived from canola and soybean oil but only ca. 77 wt% of the OLP generated from CME could be characterized. The ability to close the mass balance depended on sample origin, demonstrating the need for an accurate quantification method for biofuels at various stages of production.</abstract><cop>Netherlands</cop><pub>Elsevier B.V</pub><pmid>22245174</pmid><doi>10.1016/j.chroma.2011.12.013</doi><tpages>10</tpages></addata></record>
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subjects Biofuel
Biofuels - analysis
C (programming language)
Canola Oil
Canola oil methyl ester
Carboxylic Acids - analysis
Carboxylic Acids - chemistry
Coronal mass ejection
Fatty Acids, Monounsaturated - chemistry
Flame Ionization - methods
Fuels
Gas chromatography
Gas Chromatography-Mass Spectrometry - methods
GC–FID
GC–MS
Glycerides - analysis
Glycerides - chemistry
Hot Temperature
Hydrocarbons, Acyclic - analysis
Hydrocarbons, Acyclic - chemistry
Injectors
Least-Squares Analysis
Mathematical analysis
Pyrolysis
Reproducibility of Results
Soybean Oil - chemistry
Soybeans
Triacylglycerides
title Method development for the characterization of biofuel intermediate products using gas chromatography with simultaneous mass spectrometric and flame ionization detections
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