Characterization of milling effects on the physical and chemical nature of herbaceous biomass with comparison of fast pyrolysis product distributions using Py-GC/MS

Murillo, Jessica D.; Ware, Elizabeth A.; Biernacki, Joseph J.

doi:10.1016/j.jaap.2014.04.010

Cited by 22 publications

(4 citation statements)

References 32 publications

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“…Figure illustrates a timeline of experimental techniques that have been used to study pyrolysis beginning in the mid-20th century to present. A broad range of works has been published on biomass pyrolysis (especially cellulose) using bulk, batch, slow pyrolysis since the beginning of the 20th century. − Likely, the most used method have been thermogravimetric analysis (TGA), which became widely applied by about 1960. − Py-GC/MS was introduced shortly after and has been a major tool used in the elucidation of reaction pathways. − Techniques such as the free fall reactor (drop tube), radiant flash pyrolysis, wire-mesh heating and other laboratory-scale micropyrolyzers are less frequently cited among others. Gravimetric-based bulk, slow pyrolysis methods provide information only about the amount of oil, gas, and char produced, whereas real-time gravimetric analysis (i.e., TGA) provides some, yet lumped, kinetic information.…”

Section: Introductionmentioning

confidence: 99%

Biomass Fast Pyrolysis Using a Novel Microparticle Microreactor Approach: Effect of Particles Size, Biomass Type, and Temperature

2018

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Biomass fast pyrolysis is emerging as a front-running approach for the generation of renewable chemical and fuel resources. The pyrolysis temperature, solid-and gas-phase residence times, and biomass particle size and type have a substantial impact on char, oil, and gas yields. A laboratory-scale fast pyrolysis technique was demonstrated using manufactured biomass microspheres. A unique single-particle (∼10 μg) microreactor technology coupled to a millisecond response flame ionization detector was used to investigate the effects of relevant particle and process parameters and to capture the dynamics of real-time microscale single-particle pyrolysis for the first time. The manufactured biomass microspheres were produced by spray-drying finely milled microcrystalline cellulose, switchgrass (Panicum virgatum), and tall fescue straw (Festuca arundinacea) flour.

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Section: Introductionmentioning

confidence: 99%

Biomass Fast Pyrolysis Using a Novel Microparticle Microreactor Approach: Effect of Particles Size, Biomass Type, and Temperature

2018

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“…The most common method for compositional analysis of biomass is acid digestion followed by HPLC determination of solubilized sugars . Biomass polymers can also be pyrolyzed to generate small molecules that can be identified using gas chromatography (GC) in combination with mass spectrometry (MS). − GC/MS characterization studies of biomass pyrolysates and pyrolysis oils are numerous, and pyrolysis (Py)-GC-MS has been applied to corn stalks and food waste, switchgrass, alfalfa, and tall fescue, birch, Bermuda grass, , and Miscanthus , which is the subject of this study. A large number of cellulose-, hemicellulose-, and lignin-derived compounds have been identified using mass spectral library searching. − The dominant cellulose-derived product is anhydro-α-glucopyranose (levoglucosan); however, smaller organic oxygenates are also seen, including furfural, 5-(hydroxymethyl)furfural, acetol, acetic acid, and many others. ,− The pyrolysis process also converts some of the lignin into hydroxy, methoxy-phenylpropane derivatives, for example, p -coumaryl alcohol, coniferyl alcohol, and sinapyl alcohol; these compounds, and other related aromatics, are derived from the p -hydroxyphenyl (H), guaiacyl (G), and syringyl (S) classes of lignin. ,,, Thermogravimetry coupled with different measurement instruments, specifically FTIR, , has also been used to investigate biomass pyrolysis, and significant differences in the decomposition temperatures of the polymer classes were noted: hemicellulose degrades at lower temperatures (220–300 °C), ,, cellulose at 350–400 °C, ,− while lignin tends to have a broadened thermogravimetric profile, stretching from ∼250 to 500 °C. ,, …”

Section: Introductionmentioning

confidence: 99%

“…7 Biomass polymers can also be pyrolyzed to generate small molecules that can be identified using gas chromatography (GC) in combination with mass spectrometry (MS). 8−13 GC/MS characterization studies of biomass pyrolysates and pyrolysis oils are numerous, and pyrolysis (Py)-GC-MS has been applied to corn stalks and food waste, 14 switchgrass, alfalfa, and tall fescue, 15 birch, 16 Bermuda grass, 17,18 and Miscanthus, 19 which is the subject of this study. A large number of cellulose-, hemicellulose-, and lignin-derived compounds have been identified using mass spectral library searching.…”

Section: ■ Introductionmentioning

confidence: 99%

Pyrolysis Two-Dimensional GC-MS of Miscanthus Biomass: Quantitative Measurement Using an Internal Standard Method

et al. 2017

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Accurate measurement of biomass pyrolysis products can provide valuable guidance for thermal processing. However, pyrolysis generates large numbers of compounds in varying concentrations, factors that can make compound identification and quantitation difficult. In this study, Miscanthus biomass samples were analyzed using pyrolysis/two-dimensional gas chromatography/mass spectrometry (Py-GCxGC-MS), which provided a more comprehensive chromatographic separation and mass spectral compound identification. Quantitative measurement was performed for 34 calibrated pyrolysis compounds using an internal standard method. Pyrolysis efficiency was measured as a function of sample mass, pyrolysis temperature, and pyrolysis temperature ramp rate. For most of the calibrated pyrolysis products, production efficiency decreased with sample mass, increased with pyrolysis temperature, and decreased with pyrolysis temperature ramp rate. Significantly, the temperature profiles of the different pyrolysis products were variable, notably acetic acid and the vinyl and formyl derivatives of phenol and guaiacol, which were produced at lower temperatures compared to other compounds such as the syringyl derivatives and levoglucosan. Lignol ratios were compared with those generated using 1H/13C heteronuclear single quantum coherence (HSQC) nuclear magnetic resonance spectroscopy (NMR). Lower fractions of syringyl- and guaiacyl-lignols and higher fractions of the phenol-lignols were generated by Py-GCxGC-MS compared to HSQC-NMR.

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“…For example, the most abundant pyrolysis products formed from NR are isoprene and dipentene, corresponding to the monomer and dimer, respectively ( Scheme 1 ) [ 31 , 32 ]. Sample size affects pyrolysis behavior, such as pyrolysis rate and kinds and abundances of pyrolysis products [ 31 , 33 , 34 , 35 ]. Determination of TWP content in an environmental sample using pyrolysis analysis is performed by the calibration curve [ 36 ].…”

Section: Introductionmentioning

confidence: 99%

Variation in Abundance Ratio of Isoprene and Dipentene Produced from Wear Particles Composed of Natural Rubber by Pyrolysis Depending on the Particle Size and Thermal Aging

Jung

Choi

2023

Polymers

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Tire wear particles (TWPs) are generated by friction between the road and the tire. TWPs are one of the major microplastics found in environmental samples, such as road dust, particulate matter (PM), and sediment. TWP contents in environmental samples are generally analyzed using the pyrolysis technique. Tire tread compounds of heavy vehicles are usually composed of natural rubber (NR). Isoprene and dipentene are the principal pyrolysis products of NR, and dipentene is employed as the key marker for the determination of the TWP contents. In this study, an NR abrasion specimen was thermally aged, and an abrasion test was performed to obtain the wear particles. The influence of the wear particle size and thermal aging on the pyrolysis behavior of NR was investigated. The isoprene/dipentene ratio exponentially increased as the wear particle size decreased, and it was also increased by the thermal aging of the abrasion specimen. The increased isoprene/dipentene ratio by thermal aging was explained by increasing the crosslink density. Using the relationship between the wear particle size and the isoprene/dipentene ratio, it is possible to estimate the isoprene/dipentene ratio for very small TWP such as PM. The experimental results concluded that the wear particle size and thermal aging affect the formation of the key pyrogenic products, and the influencing factors should be considered for the quantification of TWP contents in the environmental samples.

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Characterization of milling effects on the physical and chemical nature of herbaceous biomass with comparison of fast pyrolysis product distributions using Py-GC/MS

Cited by 22 publications

References 32 publications

Biomass Fast Pyrolysis Using a Novel Microparticle Microreactor Approach: Effect of Particles Size, Biomass Type, and Temperature

Biomass Fast Pyrolysis Using a Novel Microparticle Microreactor Approach: Effect of Particles Size, Biomass Type, and Temperature

Pyrolysis Two-Dimensional GC-MS of Miscanthus Biomass: Quantitative Measurement Using an Internal Standard Method

Variation in Abundance Ratio of Isoprene and Dipentene Produced from Wear Particles Composed of Natural Rubber by Pyrolysis Depending on the Particle Size and Thermal Aging

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