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ASTM E1721-01

(Test Method)

Standard Test Method for Determination of Acid-Insoluble Residue in Biomass

Standard Test Method for Determination of Acid-Insoluble Residue in Biomass

SIGNIFICANCE AND USE
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 105C oven-dried weight of the sample.
1.2 The residue collected contains the acid-insoluble lignin and any condensed proteins from the original sample. An independent nitrogen analysis would be required to determine the acid-insoluble lignin content separate from the condensed protein fraction and is outside the scope of this test method.
1.3 A portion of the lignin in some biomass samples will remain soluble during this procedure. The total lignin in a biomass sample includes both acid-soluble lignin and lignin in the acid insoluble residue.
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 and health practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 8 and Note 2 and Note 4.

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 E1721-95 - Standard Test Method for Determination of Acid-Insoluble Residue in Biomass
Effective Date
10-Nov-2001
Replaced By
ASTM E1721-01(2009) - Standard Test Method for Determination of Acid-Insoluble Residue in Biomass
Effective Date
01-Nov-2009
Referred By
ASTM E1821-08(2020) - Standard Test Method for Determination of Carbohydrates in Biomass by Gas Chromatography
Effective Date
10-Nov-2001
Referred By
ASTM E1758-01(2020) - Standard Test Method for Determination of Carbohydrates in Biomass by High Performance Liquid Chromatography
Effective Date
10-Nov-2001

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ASTM E1721-01 - Standard Test Method for Determination of Acid-Insoluble Residue in BiomassASTM E1721-01 - Standard Test Method for Determination of Acid-Insoluble Residue in Biomass
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ASTM E1721-01 - Standard Test Method for Determination of Acid-Insoluble Residue in Biomass
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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:E1721–01
Standard Test Method for
1
Determination of Acid-Insoluble Residue in Biomass
This standard is issued under the fixed designation E1721; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
INTRODUCTION
Biomass is composed largely of the following: cellulose, a polymer of glucose; hemicellulose, a
complex polymer, the main chain of which consists of xylans or glucomannans; and lignin, a complex
phenolic polymer. The lignin is mostly insoluble in mineral acids, unlike the other cell wall
components of biomass. For this reason, lignin can be analyzed gravimetrically after hydrolyzing the
cellulose and hemicellulose fractions with sulfuric acid.
1. Scope 2. Referenced Documents
2
1.1 This test method covers determination of the acid- 2.1 ASTM Standards:
insoluble residue of hard and soft woods, herbaceous materials E1690 Test Method for Determination of Ethanol Extrac-
(suchasswitchgrassandsericea),agriculturalresidues(suchas tives in Biomass
corn stover, wheat straw, and bagasse), wastepaper (such as E1756 Test Method for Determination of Total Solids in
office waste, boxboard, and newsprint), acid and alkaline Biomass
pretreated biomass, and the solid fraction of fermentation E1757 Practice for Preparation of Biomass for Composi-
residues. All results are reported relative to the 105°C oven- tional Analysis
dried weight of the sample.
3. Terminology
1.2 The residue collected contains the acid-insoluble lignin
3.1 Definitions:
and any condensed proteins from the original sample. An
independent nitrogen analysis would be required to determine 3.1.1 acid-insoluble residue—the solid residue, corrected
for acid-insoluble ash, retained on a medium-porosity filter
the acid-insoluble lignin content separate from the condensed
protein fraction and is outside the scope of this test method. crucible after the primary 72 % and secondary 4 % H SO
2 4
hydrolysis described in this test method. This material is
1.3 A portion of the lignin in some biomass samples will
remain soluble during this procedure. The total lignin in a primarily acid-insoluble lignin and any condensed proteins.
3.1.2 prepared biomass—material that has been treated in
biomass sample includes both acid-soluble lignin and lignin in
the acid insoluble residue. accordancewithPracticeE1757inordertoraisethetotalsolids
content above 85 %, based on an oven-dried solids weight.
1.4 The values stated in SI units are to be regarded as the
standard.
4. Significance and Use
1.5 This standard does not purport to address all of the
4.1 The acid-insoluble residue content is used in conjunc-
safety concerns, if any, associated with its use. It is the
tion with other assays to determine the total composition of
responsibility of the user of this standard to establish appro-
biomass samples.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazards
5. Interferences
statements are given in Section 8 and Note 2 and Note 4.
5.1 The results of acid-insoluble residue analysis are af-
fected by the incomplete hydrolysis of biomass. The results
willbebiasedhighunlessthesampleishydrolyzedcompletely.
Take care to mix the acid/biomass slurry thoroughly during the
concentrated acid hydrolysis.
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. Orginally Standards volume information, refer to the standard’s Document Summary page on
published as E1721-95. Last previous edition E1721-95. DOI: 10.1520/E1721-01. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E1721–01
NOTE 1—In order to determine the absolute amounts of acid-insoluble
5.2 The results of acid-insoluble residue analysis are af-
residue and acid-insoluble ash, for quality control purposes, it is useful to
fected by the timing of the acid digestion steps. The insoluble
weigh and record the ignited crucible to the nearest 0.1 mg.
residue will dissolve slowly into solution in an irreproducible
10.2 Weigha0.3 60.01-gsampletothenearest0.1mg,and
fashion. The timing within this test method must be followed
place it in a test tube. Record the initial weight as W .
closely.
1
NO
...

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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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Standard Test Method for Determination of Acid-Insoluble Residue in Biomass

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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.  
1.2 The residue collected contains the acid-insoluble lignin and any condensed proteins from the original sample. An independent nitrogen analysis would be required to determine the acid-insoluble lignin content separate from the condensed protein fraction and is outside the scope of this test method.  
1.3 A portion of the lignin in some biomass samples will remain soluble during this procedure. The total lignin in a biomass sample includes both acid-soluble lignin and lignin in the acid insoluble residue.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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 hazards statements are given in Section 8 and Note 2 and Note 4.  
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ASTM E1755-01(2020)(Test Method)
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
1.1 This test method covers the determination of ash, expressed as the mass percent of residue remaining after dry oxidation (oxidation at 575 ± 25 °C), 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 mass of the sample. For particulate wood fuels, Test Method E1534 should be used.  
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Standard Test Method for Determination of Total Solids in Biomass

SIGNIFICANCE AND USE
4.1 Moisture is a ubiquitous and variable component of any biomass sample. Moisture is not considered a structural component of biomass and can change with storage and handling of biomass samples. The determination of the total solids content allows for the correction of biomass samples to an oven-dried solids mass that is constant for a particular sample.  
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.
SCOPE
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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SIGNIFICANCE AND USE
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.  
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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.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  See Section 8 for specific hazards statements.  
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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.
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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.
Note 1: This test method may not be suitable for hard and soft wood samples that include bark or those with more than 10% extractable materials.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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.  
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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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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ASTM E1721-01(2020)(Test Method)
Standard Test Method for Determination of Acid-Insoluble Residue in Biomass

SIGNIFICANCE AND USE
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.  
1.2 The residue collected contains the acid-insoluble lignin and any condensed proteins from the original sample. An independent nitrogen analysis would be required to determine the acid-insoluble lignin content separate from the condensed protein fraction and is outside the scope of this test method.  
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1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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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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