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ASTM E3417-24

(Test Method)

Standard Test Method for Determination of Cellulose/Hemicellulose-Derived Glucan and Galactan Content in Solid Corn Biomass Samples

Standard Test Method for Determination of Cellulose/Hemicellulose-Derived Glucan and Galactan Content in Solid Corn Biomass Samples

SIGNIFICANCE AND USE
4.1 The procedure, in brief, consists of solubilization of biomass using cold caustic extraction, an enzymatic removal of starch and yeast glucan followed by precipitation of hemicellulosic material, and acid hydrolysis of the residual carbohydrate pellet before measurement of glucose and galactose derived from cellulose and hemicellulose.  
4.2 The starch removal procedure is identical to that employed in the NREL assay2 which was itself adapted from the Megazyme-published starch analysis procedure: RTS-NaOH, 2019.5,6  
4.3 The cellulosic pellet hydrolysis and monosaccharide measurements are identical to those described in the NREL laboratory analytical procedure “Determination of Structural Carbohydrates and Lignin in Biomass,” NREL/TP-5100-42618 and “Determination of Cellulosic Glucan Content in Starch Containing Feedstocks,” NREL/TP-2800-76724.7  
4.4 This test method references Practices E1757 and E3181.  
4.5 This test method is intended for use in the measurement of the fermentable portion of cellulosic content in pre- and post-fermentation corn biomass specifically for the apportionment of a percentage of the total ethanol produced in a fermentation as cellulosic.
SCOPE
1.1 This procedure can be used to quantify the cellulose/hemicellulose-derived glucan and galactan (CHDGG) content in corn biomass samples that also contain varying levels of starch-derived and yeast-derived glucan. The method has been shown to provide accurate values for samples with cellulose content up to 40 % w/w.3  
1.2 Units—The values stated in SI units are to be regarded as the standard. No other units of 34 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.

General Information

Status
Published
Publication Date
31-Dec-2023
Technical Committee
E48 - Bioenergy and Industrial Chemicals from Biomass
Drafting Committee
E48.05 - Biomass Conversion
Current Stage
Ref Project

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ASTM E3417-24 - Standard Test Method for Determination of Cellulose/Hemicellulose-Derived Glucan and Galactan Content in Solid Corn Biomass SamplesASTM E3417-24 - Standard Test Method for Determination of Cellulose/Hemicellulose-Derived Glucan and Galactan Content in Solid Corn Biomass Samples
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ASTM E3417-24 - Standard Test Method for Determination of Cellulose/Hemicellulose-Derived Glucan and Galactan Content in Solid Corn Biomass Samples
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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.
Designation: E3417 − 24
Standard Test Method for
Determination of Cellulose/Hemicellulose-Derived Glucan
1
and Galactan Content in Solid Corn Biomass Samples
This standard is issued under the fixed designation E3417; 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
The US biofuel industry generates ~15 billion gal of bioethanol annually. Most of this bioethanol
is produced using processes that convert the starch content of corn biomass to glucose through
enzymatic degradation and subsequently to ethanol via yeast fermentation. Starch [a branched
polymer of α-(1-4)-D-glucose units] is the source of the majority of the glucose content present in
corn. A tiny proportion of bioethanol is generated using processes that convert cellulosic feedstock to
glucose before yeast fermentation. The emergence of in-situ corn kernel fiber (CKF) conversion
processes that allow the simultaneous conversion of starch and cellulosic content in biomass presents
an excellent opportunity for the sector. While starch measurement methodology has been well
described in literature, the analytical methodology required to accurately measure cellulosic content
in corn biomass has not been published to date despite the urgent requirement for the same to be used
in the assignment of a small but valuable percentage of total ethanol produced during such a
fermentation as cellulosic.
The procedure outlined herein seeks to address this need by modifying the assay described in the
2
seminal 2021 work of Sluiter et al.
1. Scope 1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This procedure can be used to quantify the cellulose/
ization established in the Decision on Principles for the
hemicellulose-derived glucan and galactan (CHDGG) content
Development of International Standards, Guides and Recom-
in corn biomass samples that also contain varying levels of
mendations issued by the World Trade Organization Technical
starch-derived and yeast-derived glucan. The method has been
Barriers to Trade (TBT) Committee.
shown to provide accurate values for samples with cellulose
3
content up to 40 % w/w.
2. Referenced Documents
4
1.2 Units—The values stated in SI units are to be regarded
2.1 ASTM Standards:
as the standard. No other units of 34 measurement are included
E1757 Practice for Preparation of Biomass for Composi-
in this standard.
tional Analysis
E3181 Practice for Determination of the Converted Fraction
1.3 This standard does not purport to address all of the
of Starch and Cellulosic Content From a Fuel Ethanol
safety concerns, if any, associated with its use. It is the
Production Facility
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
3. Terminology
mine the applicability of regulatory limitations prior to use.
3.1 Definitions:
3.1.1 biomass, n—substance wholly comprised of living or
recently living (non-fossil) material.
1
This test method is under the jurisdiction of ASTM Committee E48 on
3.1.1.1 Discussion—This method is selective for corn bio-
Bioenergy and Industrial Chemicals from Biomass and is the direct responsibility of
Subcommittee E48.05 on Biomass Conversion.
mass which is defined as the biomass from large kernels set in
Current edition approved Jan. 1, 2024. Published January 2024. DOI: 10.1520/
rows on a cob from a cereal plant.
E3417-24.
2
Sluiter, J. B. et al., “Direct Determination of Cellulosic Glucan Content in
4
Starch-Containing Samples,” Cellulose, 2021, https://doi.org/10.1007/s10570-020- For referenced ASTM standards, visit the ASTM website, www.astm.org, or
03652-2. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
See Supporting data document - Determination of cellulosic carbohydrate Standards volume information, refer to the standard’s Document Summary page on
content in corn biomass samples the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E3417 − 24
3.1.2 calibration verification standard, CVS, n—standards 3.2.4 SRS—Sugar Recovery Standard
used in determining the quality of the calibration curve as well
3.2.5 YDC—Yeast Degrading Cocktail
as the quality of the standard reagents used in preparing the
calibration standards.
4. S
...

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