Using design of experiments to optimize derivatization with methyl chloroformate for quantitative analysis of the aqueous phase from hydrothermal liquefaction of biomass
| Autor: | Marianne Glasius, René B. Madsen, Maika Klemmer, Bo B. Iversen, Mads Mørk Jensen, Jacob Becker, Per Sigaard Christensen, Kasper Houlberg, Anders Juul Mørup |
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| Jazyk: | angličtina |
| Rok vydání: | 2016 |
| Předmět: |
Formates
Central composite design 020209 energy GAS-CHROMATOGRAPHY Methyl chloroformate derivatization 02 engineering and technology 01 natural sciences Biochemistry Gas Chromatography-Mass Spectrometry Analytical Chemistry MICROALGAE Hydrothermal liquefaction aqueous phase chemistry.chemical_compound Bioreactors 0202 electrical engineering electronic engineering information engineering Biomass SOLUBLES Derivatization Distillation Chromatography CHLORELLA-PYRENOIDOSA TECHNOECONOMIC ANALYSIS 010401 analytical chemistry Temperature Aqueous two-phase system Water DRIED DISTILLERS GRAINS 0104 chemical sciences Hydrothermal liquefaction chemistry Aqueous phase recirculation SPECTROMETRY Methyl chloroformate Biofuels Reagent TECHNOLOGIES Gas chromatography Gas chromatography–mass spectrometry Edible Grain Design of experiments SUPERCRITICAL WATER FRACTIONS |
| Zdroj: | Madsen, R B, Jensen, M M, Mørup, A, Houlberg, K, Sigaard Christensen, P, Klemmer, M, Becker, J, Iversen, B B & Glasius, M 2016, ' Using design of experiments to optimize derivatization with methyl chloroformate for quantitative analysis of the aqueous phase from hydrothermal liquefaction of biomass ', Analytical and Bioanalytical Chemistry, vol. 408, no. 8, pp. 2171-2183 . https://doi.org/10.1007/s00216-016-9321-6 |
| Popis: | Hydrothermal liquefaction is a promising technique for the production of bio-oil. The process produces an oil phase, a gas phase, a solid residue, and an aqueous phase. Gas chromatography coupled with mass spectrometry is used to analyze the complex aqueous phase. Especially small organic acids and nitrogen-containing compounds are of interest. The efficient derivatization reagent methyl chloroformate was used to make analysis of the complex aqueous phase from hydrothermal liquefaction of dried distillers grains with solubles possible. A circumscribed central composite design was used to optimize the responses of both derivatized and nonderivatized analytes, which included small organic acids, pyrazines, phenol, and cyclic ketones. Response surface methodology was used to visualize significant factors and identify optimized derivatization conditions (volumes of methyl chloroformate, NaOH solution, methanol, and pyridine). Twenty-nine analytes of small organic acids, pyrazines, phenol, and cyclic ketones were quantified. An additional three analytes were pseudoquantified with use of standards with similar mass spectra. Calibration curves with high correlation coefficients were obtained, in most cases R 2 > 0.991. Method validation was evaluated with repeatability, and spike recoveries of all 29 analytes were obtained. The 32 analytes were quantified in samples from the commissioning of a continuous flow reactor and in samples from recirculation experiments involving the aqueous phase. The results indicated when the steady-state condition of the flow reactor was obtained and the effects of recirculation. The validated method will be especially useful for investigations of the effect of small organic acids on the hydrothermal liquefaction process. |
| Databáze: | OpenAIRE |
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