ASTM E1821-08
(Test Method)Standard Test Method for Determination of Carbohydrates in Biomass by Gas Chromatography
Standard Test Method for Determination of Carbohydrates in Biomass by Gas Chromatography
SIGNIFICANCE AND USE
The structural carbohydrate content is used in conjunction with other assays to determine the total composition of biomass samples.
SCOPE
1.1 This test method describes the determination of structural carbohydrates present in a biomass sample, expressed as the percent mass of an oven-dried sample basis of each anhydrosugar.
1.2 Sample materials suitable for this procedure include hard and softwoods, herbaceous materials, such as sericea and switchgrass, agricultural residues, such as corn stover, wheat straw, and bagasse, wastepaper, such as boxboard, office waste, and newsprint, acid or alkaline-pretreated biomass, washed free of any residual acid or alkali, and the solid fraction of fermentation residues.
1.3 The options for the types of samples to be analyzed in this procedure are:
1.3.1 Prepared Biomass Samples:
1.3.1.1 Air Dried Material—Results are reported as the percent by mass, based on the oven-dried mass of the air-dried sample.
1.3.1.2 45°C Dried Material—Results are reported as the percent by mass, based on the oven-dried mass of the 45°C dried sample.
1.3.1.3 Freeze Dried Material—Results are reported as the percent by mass, based on the oven-dried mass of the freeze dried sample.
1.3.2 Extractives-Free Sample—Results are reported as the percent by mass, based on the oven-dried mass of the extracted sample.
1.4 This standard method is generally not suitable for samples that contain soluble, nonstructural carbohydrates unless they are removed prior to analysis.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. See Section 8 for specific hazards statements.
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Designation: E1821 − 08
StandardTest Method for
Determination of Carbohydrates in Biomass by Gas
1
Chromatography
This standard is issued under the fixed designation E1821; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
INTRODUCTION
This test method gives a reproducible way to quantitatively determine in lignocellulosic materials
thekindandamountofthestructuralcarbohydratesmadefromarabinose,xylose,mannose,galactose,
and glucose. This way is accomplished by first hydrolyzing the carbohydrates to their constituent
monosaccharides. Subsequent derivatization produces the corresponding alditol acetates that are
quantified using capillary gas chromatography.
1. Scope 1.4 This standard method is generally not suitable for
samples that contain soluble, nonstructural carbohydrates un-
1.1 This test method describes the determination of struc-
less they are removed prior to analysis.
tural carbohydrates present in a biomass sample, expressed as
the percent mass of an oven-dried sample basis of each 1.5 The values stated in SI units are to be regarded as
anhydrosugar. standard. No other units of measurement are included in this
standard.
1.2 Sample materials suitable for this procedure include
1.6 This standard does not purport to address all of the
hard and softwoods, herbaceous materials, such as sericea and
safety concerns, if any, associated with its use. It is the
switchgrass, agricultural residues, such as corn stover, wheat
responsibility of the user of this standard to establish appro-
straw,andbagasse,wastepaper,suchasboxboard,officewaste,
priate safety and health practices and determine the applica-
and newsprint, acid or alkaline-pretreated biomass, washed
bility of regulatory limitations prior to use. See Section 8 for
free of any residual acid or alkali, and the solid fraction of
specific hazards statements.
fermentation residues.
1.3 The options for the types of samples to be analyzed in
2. Referenced Documents
this procedure are:
2
2.1 ASTM Standards:
1.3.1 Prepared Biomass Samples:
D1193Specification for Reagent Water
1.3.1.1 Air Dried Material—Results are reported as the
E1690Test Method for Determination of Ethanol Extrac-
percent by mass, based on the oven-dried mass of the air-dried
tives in Biomass
sample.
E1721Test Method for Determination of Acid-Insoluble
1.3.1.2 45°C Dried Material—Results are reported as the
Residue in Biomass
percent by mass, based on the oven-dried mass of the 45°C
E1756Test Method for Determination of Total Solids in
dried sample.
Biomass
1.3.1.3 Freeze Dried Material—Results are reported as the
E1757Practice for Preparation of Biomass for Composi-
percent by mass, based on the oven-dried mass of the freeze
tional Analysis
dried sample.
1.3.2 Extractives-Free Sample—Results are reported as the
3. Terminology
percentbymass,basedontheoven-driedmassoftheextracted
3.1 Definitions of Terms Specific to This Standard:
sample.
3.1.1 anhydrosugars, n—the nominal repeating unit of a
polysaccharide. When polysaccharides undergo acid
1
This test method is under the jurisdiction of ASTM Committee E48 on
BioenergyandIndustrialChemicalsfromBiomassandisthedirectresponsibilityof
2
Subcommittee E48.05 on Biomass Conversion. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 1, 2008. Published May 2008. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approvedin1996.Lastpreviouseditionapprovedin2007asE1821-01(2007).DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E1821-08. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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E1821 − 08
hydrolysis,eachrepeatingunitaddsasinglemoleculeofwater arabinose and xylose, k =0.88 (m/z 132/150); for mannose,
to form the free monosaccharide that is analyzed. The extra galactose and glucose, k=0.90 (m/z 162/180).
weight from this water of hydrolysis must be taken in to
3.2.14 LF—loss factor for monosaccharide c. Used to cor-
account whencalculating the actual mass percent of the poly-
rect for the amount of monosaccharide lost through degrada-
saccharide in the original biomass sample.
tion during acid hydrolysis of biomass.
3.1.2 as received biomass, n—materialasitisreceivedinits
3.2.15 m —initial mass of the biomass specimen, in mg.
I
field or process collected state.
3.2.16 m —mass of monosaccharide in solution, cor-
corr
3.1.3 extractives-free biomass—air-dried solids left after
rected
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:E1821–01 (Reapproved 2007) Designation:E1821–08
Standard Test Method for
Determination of Carbohydrates in Biomass by Gas
1
Chromatography
This standard is issued under the fixed designation E1821; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
INTRODUCTION
This test method gives a reproducible way to quantitatively determine in lignocellulosic materials
thekindandamountofthestructuralcarbohydratesmadefromarabinose,xylose,mannose,galactose,
and glucose. This way is accomplished by first hydrolyzing the carbohydrates to their constituent
monosaccharides. Subsequent derivatization produces the corresponding alditol acetates that are
quantified using capillary gas chromatography.
1. Scope
1.1 This test method describes the determination of structural carbohydrates present in a biomass sample, expressed as the
percent mass of an oven-dried sample basis of each anhydrosugar.
1.2 Sample materials suitable for this procedure include hard and softwoods, herbaceous materials, such as sericea and
switchgrass, agricultural residues, such as corn stover, wheat straw, and bagasse, wastepaper, such as boxboard, office waste, and
newsprint, acid or alkaline-pretreated biomass, washed free of any residual acid or alkali, and the solid fraction of fermentation
residues.
1.3 The options for the types of samples to be analyzed in this procedure are:
1.3.1 Prepared Biomass Samples:
1.3.1.1 Air Dried Material—Results are reported as the percent by mass, based on the oven-dried mass of the air-dried sample.
1.3.1.2 45°C Dried Material—Results are reported as the percent by mass, based on the oven-dried mass of the 45°C dried
sample.
1.3.1.3 Freeze Dried Material—Results are reported as the percent by mass, based on the oven-dried mass of the freeze dried
sample.
1.3.2 Extractives-Free Sample—Results are reported as the percent by mass, based on the oven-dried mass of the extracted
sample.
1.4 This standard method is generally not suitable for samples that contain soluble, nonstructural carbohydrates unless they are
removed prior to analysis.
1.5
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use. See Section 8 for specific hazards statements.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
E1690 Test Method for Determination of Ethanol Extractives in Biomass
E1721 Test Method for Determination of Acid-Insoluble Residue in Biomass
E1756 Test Method for Determination of Total Solids in Biomass
E1757 Practice for Preparation of Biomass for Compositional Analysis
1
This test method is under the jurisdiction ofASTM Committee E48 on Biotechnology and is the direct responsibility of Subcommittee E48.05 on Biomass Conversion.
Current edition approved Nov. 15, 2007.May 1, 2008. Published JanuaryMay 2008. Originally approved in 1996. Last previous edition approved in 20012007 as
E1821-01(2007).
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
E1821–08
3. Terminology
3.1 Descriptions of Terms Specific to This Standard:
3.1.1 anhydrosugars, n—the nominal repeating unit of a polysaccharide. When polysaccharides undergo acid hydrolysis, each
repeating unit adds a single molecule of water to form the free monosaccharide that is analyzed.The extra weight from this water
of hydrolysis must be taken in to account whencalculating the actual mass percent of the polysaccharide in the original biomass
sample.
3.1.2 as received biomass, n—material as it is received in its field or process collected state.
3.1.3 extractives-free biomass—air-dried solids left after biomass has been treated according to Test Method E1690.
3.1.4 o
...
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