Abstract
Methods for thermochemical conversion of biomass into renewable energy and materials rapidly increase in range and outreach. A focus on the target product streams for valorization is natural, yet several pretreatment steps and conversion methods also result in an aqueous byproduct, which has been given less attention. This paper aims to fill this knowledge gap in the existing literature on identification and quantification of organic components in such aqueous phases by reporting a fast and direct workup protocol combined with application of quantitative analytical nuclear magnetic resonance (NMR) spectroscopy. Laboratory workup procedures combined with subsequent proton NMR spectroscopy with water signal suppression using presaturation pulses during relaxation delay, noesygppr1d, have been established, evaluated, and approved by testing on three different Bruker BioSpin NMR spectrometers; an 850 MHz AVANCE III HD with a 5 mm TCI CryoProbe, a 600 MHz AVANCE NEO with a QCI CryoProbe, and a 500 MHz AVANCE with a 5 mm BBO room-temperature probe additionally confirmed the quantification method to be applicable. The analytical procedure identified furfural, methanol, acetic acid, and formic acid as the dominating compounds in the analyzed aqueous samples, which were process effluents generated by the patented Arbacore pellet production process using steam explosion of wood shavings. A selected range of quantitative results in the aqueous phase from large-scale steam explosion is included in the study. The described procedure provides excellent quantitative reproducibility with experimental series standard deviations of <1% (mM), is nondestructive, and can be automated on demand.
Highlights
Pretreatment and conversion of biomass into renewable energy and materials are a continuously expanding field of interest and research
A great variety of HPLC procedures for aqueous-phase identification and quantification has been reported, using a refractive index detector (RID), an ultraviolet detector (UVD), and a diode array detector (DAD), coupled with mass spectrometry (MS) and two-dimensional comprehensive liquid chromatography coupled with DAD and MS (LC×LC/DAD-MS).[5−10] Disadvantages of using analytical procedures involving HPLC involve their general dependency on previous information on sample content and extensive calibration curve preparations to identify and quantify sample compounds
This paper describes and reports on direct application of quantitative analytical nuclear magnetic resonance (NMR) spectroscopy to investigate aqueous product streams, targeting biorefinery byproducts
Summary
Pretreatment and conversion of biomass into renewable energy and materials are a continuously expanding field of interest and research. Extensive research was performed, and literature studies were published addressing a great variety of conversion methods targeting biomass thermal liquefaction, pyrolysis, carbonization, and gasification.[1−4] In general, the conversion methods and the resulting published papers have in common a focus on the target product stream for valorization, typically bio-oil or biochar, yet several pretreatment steps and conversion methods result in an aqueous phase containing a significant proportion of biomassderived products These byproducts have been given only limited attention, and there is a knowledge gap in the existing literature. A great variety of HPLC procedures for aqueous-phase identification and quantification has been reported, using a refractive index detector (RID), an ultraviolet detector (UVD), and a diode array detector (DAD), coupled with mass spectrometry (MS) and two-dimensional comprehensive liquid chromatography coupled with DAD and MS (LC×LC/DAD-MS).[5−10] Disadvantages of using analytical procedures involving HPLC involve their general dependency on previous information on sample content and extensive calibration curve preparations to identify and quantify sample compounds
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