Pyrolysis−GC−MS Analysis of the Formation and Degradation Stages of Charred Residues from Lignocellulosic Biomass

Vila, Francisco Javier González; Tinoco, Pilar; Almendros, G.; Martı́n, Francisco

doi:10.1021/jf0006325

Cited by 102 publications

(55 citation statements)

References 25 publications

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“…The weight reduction in charcoal during heating has been widely recognised (Bustin and Guo 1999;Czimczik et al 2002;Gonzales-Vila et al 2001;Hammes et al 2006;McParland et al 2007). In our laboratory study, the higher the temperature of formation or the longer the duration of charring, the more weight was lost from the sample (Fig.…”

Section: Discussionmentioning

confidence: 99%

The use of reflectance values for the interpretation of natural and anthropogenic charcoal assemblages

McParland

Collinson

Scott

et al. 2009

Archaeol Anthropol Sci

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Charcoal assemblages occur in both natural and archaeological settings. Cell wall reflectance values of charcoal in polished blocks under oil provide a proxy for temperature of formation. This paper aims to (1) determine whether wildfire charcoals and anthropological charcoals from various pyrotechnical activities can be distinguished using reflectance data and (2) establish if re-charring (i.e. use of charcoal fuel) can be recognised in the archaeological record through analysis of laboratory-produced re-charred charcoals and charcoals from an experimental iron smelt and traditional bronze casting which utilised charcoal fuel. Reflectance frequency data from assemblages representing burning of charcoal, in this case of iron smelting and bronze casting, indicates temperatures from above the mean value of charcoal production (>475°C) up to the maximum temperature reached in the subsequent process (i.e. >475 to >1,100°C). In contrast, wildfire charcoals showed a range of values including material with barely measurable reflectance (minimum values from 0.06% to 0.56%Ro) to maximum reflectance values varying from 1.65%Ro (Tilford) to 3.8%Ro (Zacca). The mean wildfire reflectance indicated temperatures in the range 325-400°C, which can therefore clearly be distinguished from that of the charcoal burning processes. The laboratory-produced re-charred charcoals take on the reflectance value of the highest temperatures experienced; reflectance values were not constrained by the original temperature of formation. High temperatures are most easily achievable by the burning of charcoal fuel, and hence high reflectance charcoals are likely to represent re-charred charcoal. Therefore, this quantitative reflectance method can be used in archaeology to determine the minimum temperature of formation of charcoals in anthropological processes which involve fire, can indicate the likelihood of use of charcoal or wood as fuel and can distinguish between an assemblage of high temperature anthropogenic charcoals and charcoals formed from natural wildfire.

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Section: Discussionmentioning

confidence: 99%

The use of reflectance values for the interpretation of natural and anthropogenic charcoal assemblages

McParland

Collinson

Scott

et al. 2009

Archaeol Anthropol Sci

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“…Another method that has been successfully used to determine yields and chemical composition of steam-treated lignocellulosics is the Py-GC-MS (Courier-point pyrolysis-gas chromatography-mass spectrometry) 110 . This method is based upon the GC-MS analysis of molecular markers that are released from biomass by controlled pyrolysis and can be unequivocally used to quantify cellulose, hemicellulose and lignin, with the advantage of giving further structural information on each of these biopolymers.…”

Section: Methods To Determine Pretreatment Recovery Yieldsmentioning

confidence: 99%

The chemistry involved in the steam treatment of lignocellulosic materials

Ramos¹

2003

Quím. Nova

546

217

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Recebido em 16/8/02; aceito em 15/5/03Pretreatment of lignocellulosic materials is essential for bioconversion because of the various physical and chemical barriers that greatly inhibit their susceptibility to bioprocesses such as hydrolysis and fermentation. The aim of this article is to review some of the most important pretreatment methods developed to date to enhance the conversion of lignocellulosics. Steam explosion, which precludes the treatment of biomass with high-pressure steam under optimal conditions, is presented as the pretreatment method of choice and its mode of action on lignocellulosics is discussed. The optimal pretreatment conditions for a given plant biomass are defined as those in which the best substrate for hydrolysis is obtained with the least amount of soluble sugars lost to side reactions such as dehydration. Therefore, pretreatment optimization results from a compromise between two opposite trends because hemicellulose recovery in acid hydrolysates can only be maximized at lower pretreatment severities, whereas the development of substrate accessibility requires more drastic pretreatment conditions in which sugar losses are inevitable. To account for this heterogeneity, the importance of several process-oriented parameters is discussed in detail, such as the pretreatment temperature, residence time into the steam reactor, use of an acid catalyst, susceptibility of the pretreated biomass to bioconversion, and process design.

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“…In the present study, signal intensity is controlled by the pyrolysability of the material analysed [45]. Because the signal intensity of the chestnut wood chars obtained at T CHAR ≥ 600 ºC and rice straw chars at T CHAR ≥ 800 ºC was too low for meaningful quantification, in combination with poor reproducibility, we report only the results for chars obtained at T CHAR ≤ 500 ºC and ≤ 700 ºC for chestnut wood and rice straw, respectively.…”

Section: Total Quantified Peak Area (Tqpa)mentioning

confidence: 99%

Rapid molecular screening of black carbon (biochar) thermosequences obtained from chestnut wood and rice straw: A pyrolysis-GC/MS study

Kaal

Schneider

Schmidt

2012

Biomass and Bioenergy

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Rice straw and chestnut wood were heated between 200 and 1000 °C (T CHAR ) to produce Black C 'thermosequences'. The molecular properties of the charred residues were assessed by pyrolysis-GC/MS to investigate the relation between charring intensity and pyrolysis fingerprint. Samples obtained at T CHAR > 500 ºC (wood) or > 700 ºC (straw) gave low quality pyrograms and poor reproducibility because of high thermal stability, but pyrolysis-GC/MS allowed to track the thermal degradation of the main biocomponents (polysaccharides, lignin, methylene chain-based aliphatics, triterpenoids, chlorophyll and proteins) in the lower temperature range, mostly occurring between T CHAR 250 and 500 ºC. With increasing T CHAR , the charred residues of these biocomponents lose characteristic functional groups, aromatise and finally condense into non-pyrolysable biomass. The proportions of the pyrolysis products of unspecific origin (benzene, toluene, PAHs, etc.), increase with charring intensity, while the ratios that reflect the abundance of alkyl cross-linkages between aromatic moieties (e.g. benzene/toluene, naphthalene/alkylnaphthalene) decrease. These results provide the guidelines to using pyrolysis-GC/MS for the molecular characterisation of different components in Black C and biochar, which is an important parameter for predicting Black C/biochar behaviour in soil. Results are consistent with earlier studies of these samples using the BPCA (benzenepolycarboxylic acid) method and the ring current-induced 13 Cbenzene chemical shift NMR (Nuclear Magnetic Resonance) approach. Pyrolysis-GC/MS provides more information on molecular structures in the low temperature range (T CHAR ≤ 500 ºC) while the BPCA and NMR ring current methods provide more reliable estimations of charring intensity, especially at higher temperatures (T CHAR ≥ 500 ºC).3

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Pyrolysis−GC−MS Analysis of the Formation and Degradation Stages of Charred Residues from Lignocellulosic Biomass

Cited by 102 publications

References 25 publications

The use of reflectance values for the interpretation of natural and anthropogenic charcoal assemblages

The use of reflectance values for the interpretation of natural and anthropogenic charcoal assemblages

The chemistry involved in the steam treatment of lignocellulosic materials

Rapid molecular screening of black carbon (biochar) thermosequences obtained from chestnut wood and rice straw: A pyrolysis-GC/MS study

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