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ASTM E1821-01

(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 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.

General Information

Status
Historical
Publication Date
09-Nov-2001
ICS
65.040.20 - Buildings and installations for processing and storage of agricultural produce
Technical Committee
E48 - Bioenergy and Industrial Chemicals from Biomass
Drafting Committee
E48.05 - Biomass Conversion
Current Stage
Ref Project

Relations

Replaces
ASTM E1821-96 - Standard Test Method for Determination of Carbohydrates in Biomass by Gas Chromatography
Effective Date
10-Nov-2001
Replaced By
ASTM E1821-01(2007) - Standard Test Method for Determination of Carbohydrates in Biomass by Gas Chromatography
Effective Date
15-Nov-2007

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ASTM E1821-01 - Standard Test Method for Determination of Carbohydrates in Biomass by Gas Chromatography
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:E1821–01
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 1.4 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
1.5 This standard does not purport to address all of the
the percent mass of an oven-dried sample basis of each
safety concerns, if any, associated with its use. It is the
anhydrosugar.
responsibility of the user of this standard to establish appro-
1.2 Sample materials suitable for this procedure include
priate safety and health practices and determine the applica-
hard and softwoods, herbaceous materials, such as sericea and
bility of regulatory limitations prior to use. See Section 8 for
switchgrass, agricultural residues, such as corn stover, wheat
specific hazards statements.
straw,andbagasse,wastepaper,suchasboxboard,officewaste,
and newsprint, acid or alkaline-pretreated biomass, washed
2. Referenced Documents
free of any residual acid or alkali, and the solid fraction of
2
2.1 ASTM Standards:
fermentation residues.
D1193 Specification for Reagent Water
1.3 The options for the types of samples to be analyzed in
E1690 Test Method for Determination of Ethanol Extrac-
this procedure are:
tives in Biomass
1.3.1 Prepared Biomass Samples:
E1721 Test Method for Determination of Acid-Insoluble
1.3.1.1 Air Dried Material—Results are reported as the
Residue in Biomass
percent by mass, based on the oven-dried mass of the air-dried
E1756 Test Method for Determination of Total Solids in
sample.
Biomass
1.3.1.2 45°C Dried Material—Results are reported as the
E1757 Practice for Preparation of Biomass for Composi-
percent by mass, based on the oven-dried mass of the 45°C
tional Analysis
dried sample.
1.3.1.3 Freeze Dried Material—Results are reported as the
3. Terminology
percent by mass, based on the oven-dried mass of the freeze
3.1 Descriptions of Terms Specific to This Standard:
dried sample.
3.1.1 anhydrosugars, n—the nominal repeating unit of a
1.3.2 Extractives-Free Sample—Results are reported as the
polysaccharide. When polysaccharides undergo acid hydroly-
percentbymass,basedontheoven-driedmassoftheextracted
sis,eachrepeatingunitaddsasinglemoleculeofwatertoform
sample.
the free monosaccharide that is analyzed. The extra weight
from this water of hydrolysis must be taken in to account
1
This test method is under the jurisdiction of ASTM Committee E48 on
2
Biotechnology and is the direct responsibility of Subcommittee E48.05 on Biomass For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Conversion. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved Nov. 10, 2001. Published February 2002. Originally Standards volume information, refer to the standard’s Document Summary page on
published as E 1821-96. Last previous edition E1821-96. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E1821–01
whencalculating the actual mass percent of the polysaccharide 3.2.17 RR —averagedresponseratioofmonosaccharide c
avg
in the original biomass sample. to the internal standard (inositol) in the calibration standard.
Derived from multiple injections of the same calibration
3.1.2 as received biomass, n—materialasitisreceivedinits
field or process collected state. standard.
3.2.18 RR —response ratio of monosaccharide c to the
3.1.3 extractives-free biomass—air-dried solids left after
s
internal standard (inositol) in the specimen.
biomass has been treated according to Test Method E1690.
3.2.19 RR —response ratio of monosaccharide c to the
3.1.4 oven-dried mass, n—the moisture-free mass of any
STD
internal standard (inositol) in the calibration standard.
biomass sample (as received, prepared
...

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4.1 Ethanol extractives are any materials found in biomass that are soluble in ethanol. They are not considered to be part of the structural components of biomass and should be removed prior to any chemical analysis of the sample. The prolonged extraction removes nonstructural materials that can include waxes, fats, resins, tannins, gums, sugars, starches, and pigments. Removing hydrophobic materials from the biomass makes it easier to wet the material for the analysis of structural components in the biomass.  
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4.1 The ash content is an approximate measure of the mineral content and other inorganic matter in biomass.  
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4.1 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:  
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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.  
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4.1 The acid-insoluble residue content is used in conjunction with other assays to determine the total composition of biomass samples.
SCOPE
1.1 This test method covers determination of the acid-insoluble residue of hard and soft woods, herbaceous materials (such as switchgrass and sericea), agricultural residues (such as corn stover, wheat straw, and bagasse), wastepaper (such as office waste, boxboard, and newsprint), acid and alkaline pretreated biomass, and the solid fraction of fermentation residues. All results are reported relative to the 105 °C oven-dried weight of the sample.  
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4.2 This procedure is not suitable for biomass samples that visibly change on heating to 105 °C, for example, unwashed acid-pretreated biomass still containing free acid.  
4.3 Some materials that contain large amount of free sugars or proteins will caramelize or brown under direct infrared heating elements used in Test Method B. Total solids in these materials should be done by Test Method A.
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1.1 This test method covers the determination of the amount of total solids remaining after drying a sample. Materials suitable for this procedure include samples prepared in accordance with Practice E1757 and extractive-free material prepared in accordance with Test Method E1690. For particulate wood fuels, Test Method E871 should be used.  
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4.1 The percentage, by mass, of sugar content is used in conjunction with other assays to determine the total composition of biomass samples.
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ASTM E1757-19(Practice)
Standard Practice for Preparation of Biomass for Compositional Analysis

SIGNIFICANCE AND USE
4.1 Preparation Method A—Method suitable for the preparation of large quantities (>20 g) of field collected samples into a form appropriate for compositional analysis. Woody samples must first be available as chips of a nominal 5 by 5 by 0.6 cm (2 by 2 by 1/4 in.) or less and twigs not exceeding 0.6 cm (1/4 in.) diameter. Herbaceous materials may be processed as whole straw. It is recommended that wastepaper should be shredded into pieces less then 1 cm (1/2 in.) wide. Furthermore, it is recommended that twigs, straw, and wastepaper should not exceed 61 cm (24 in.) in length to facilitate handling.  
4.2 Preparation Methods B and C—Methods are suitable for very moist feedstocks, samples that would not be stable during prolonged exposure to ambient conditions, or for drying materials when room conditions deviate from the ambient conditions described in 3.1.1. These test methods are also suitable for handling small samples of biomass (  
4.3 Preparation Methods A, B, and C are not intended for materials that will already pass through a 20 mesh sieve or that cannot be dried by the described methods to a total solids content of greater than 85 %, based on an oven dried weight.  
4.4 Preparation Method A will separate the milled material into two fractions, a −20/+80 mesh fraction and a −80 mesh fraction.  
4.4.1 Extraneous inorganic materials will accumulate in the −80 mesh fraction and it should be analyzed independently from the −20/+80 mesh fraction. Weighted results from the two fractions can then be combined to obtain results for materials on an "as received" basis.
Note 1: During analysis, the very fine consistency of the −80 mesh fraction may cause problems in filtering operations and should be handled appropriately.  
4.5 Preparation Method D—Method suitable for cereal grains, cereal grain fermentation mash, cereal grain fermentation beer, and cereal grain fermentation residues that are generally stable.  
4.6 Preparation Method E—Method suitable for ce...
SCOPE
1.1 This practice covers a reproducible way to convert hardwoods, softwoods, herbaceous materials (such as switchgrass and sericea), agricultural residues (such as corn stover, wheat straw, and bagasse), wastepaper (such as office waste, boxboard, and newsprint), cellulosic feedstocks pretreated to improve suitability for fermentation, cereal grains, cereal grain fermentation mash, cereal grain fermentation beer, and fermentation residues into a uniform material suitable for compositional analysis. This practice is intended for samples that need to be dried prior to analysis.  
1.2 Milling and sieving actions both produce large amounts of dust. This dust can be a nuisance hazard and irritant. Use appropriate respiratory protection as needed. If excessive amounts of dust are allowed to become airborne a potential explosion hazard is possible. Provide appropriate dust control measures as needed.  
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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Standard Test Method for Determination of Ethanol Extractives in Biomass

SIGNIFICANCE AND USE
4.1 Ethanol extractives are any materials found in biomass that are soluble in ethanol. They are not considered to be part of the structural components of biomass and should be removed prior to any chemical analysis of the sample. The prolonged extraction removes nonstructural materials that can include waxes, fats, resins, tannins, gums, sugars, starches, and pigments. Removing hydrophobic materials from the biomass makes it easier to wet the material for the analysis of structural components in the biomass.  
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SCOPE
1.1 This test method covers the determination of ethanol soluble extractives, expressed as a percentage of the oven-dried biomass, of hard and soft woods, herbaceous materials (such as switchgrass and sericea), agricultural residues (such as corn stover, wheat straw, and bagasse), and wastepaper (such as office waste, boxboard, and newsprint). All results are reported relative to the oven-dried weight of the sample.
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1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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ASTM E1758-01(2020)(Test Method)
Standard Test Method for Determination of Carbohydrates in Biomass by High Performance Liquid Chromatography

SIGNIFICANCE AND USE
4.1 The percentage, by mass, of sugar content is used in conjunction with other assays to determine the total composition of biomass samples.
SCOPE
1.1 This test method covers the determination of carbohydrates present in a biomass sample, expressed as the percent, by mass, of each sugar on a 105 °C dried mass basis.
Note 1: The percent sugar must be corrected for the water of hydrolysis before calculating the actual mass percent of the polysaccharide in the original biomass sample.  
1.2 Sample materials suitable for this procedure include hard and soft woods, herbaceous materials (such as switchgrass and sericea), agricultural residues (such as corn stover, wheat straw, and bagasse), wastepaper (such as office waste, boxboard, and newsprint), acid or alkaline-pretreated biomass (washed free of any residual acid or alkali), and the solid fraction of fermentation residues. All results are reported relative to the 105 °C oven-dried mass of the sample.  
1.3 The options for the types of samples to be analyzed in this test method are as follows:  
1.3.1 Prepared Biomass Samples:  
1.3.1.1 Air Dried (%Tad)—The percent, by mass, of total solids of the air-dried sample.
1.3.1.2 45 °C Dried (%T45)—The percent, by mass, of total solids of the 45 °C dried sample.
1.3.1.3 Freeze Dried (%Tfd)—The percent, by mass, of total solids of the freeze dried sample.  
1.3.2 Extractives-Free Sample (%T ext)—The percent, by mass, of total solids of the extracted sample determined at 105°C.  
1.4 The values stated in SI units are to be regarded as the standard.  
1.5 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Note 3 and Note 4.  
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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Standard Test Method for Ash in Biomass

SIGNIFICANCE AND USE
4.1 The ash content is an approximate measure of the mineral content and other inorganic matter in biomass.  
4.2 The ash content is used in conjunction with other assays to determine the total composition of biomass samples.
SCOPE
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