Standard Test Method for Determination of Carbohydrates in Biomass by High Performance Liquid Chromatography

SIGNIFICANCE AND USE
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 (%Text)—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 and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Note 3 and Note 4.

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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E1758 − 01(Reapproved 2007)
Standard Test Method for
Determination of Carbohydrates in Biomass by High
1
Performance Liquid Chromatography
This standard is issued under the fixed designation E1758; 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
The carbohydrates making up a major portion of biomass samples are polysaccharides constructed
primarilyofglucose,xylose,arabinose,galactose,andmannosesubunits.Thepolysaccharidespresent
in a biomass sample can be hydrolyzed to their component sugar monomers by sulfuric acid in a
two-stage hydrolysis process. These monosaccharides can then be quantified by ion-moderated
partition HPLC.
1. Scope 1.4 The values stated in SI units are to be regarded as the
standard.
1.1 This test method covers the determination of carbohy-
drates present in a biomass sample, expressed as the percent,
1.5 This standard does not purport to address all of the
by mass, of each sugar on a 105°C dried mass basis.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
NOTE 1—The percent sugar must be corrected for the water of
priate safety and health practices and determine the applica-
hydrolysis before calculating the actual mass percent of the polysaccha-
ride in the original biomass sample.
bility of regulatory limitations prior to use. Specific precau-
tionary statements are given in Note 3 and Note 4.
1.2 Sample materials suitable for this procedure include
hardandsoftwoods,herbaceousmaterials(suchasswitchgrass
2. Referenced Documents
and sericea), agricultural residues (such as corn stover, wheat
straw, and bagasse), wastepaper (such as office waste,
2
2.1 ASTM Standards:
boxboard, and newsprint), acid or alkaline-pretreated biomass
D1193Specification for Reagent Water
(washed free of any residual acid or alkali), and the solid
E1690Test Method for Determination of Ethanol Extrac-
fraction of fermentation residues. All results are reported
tives in Biomass
relative to the 105°C oven-dried mass of the sample.
E1721Test Method for Determination of Acid-Insoluble
1.3 The options for the types of samples to be analyzed in
Residue in Biomass
this test method are as follows:
E1756Test Method for Determination of Total Solids in
1.3.1 Prepared Biomass Samples:
Biomass
1.3.1.1 Air Dried (%T )—The percent, by mass, of total
E1757Practice for Preparation of Biomass for Composi-
ad
solids of the air-dried sample.
tional Analysis
1.3.1.2 45°C Dried (%T )—The percent, by mass, of total
45
solids of the 45°C dried sample.
3. Terminology
1.3.1.3 Freeze Dried (%T )—The percent, by mass, of total
fd
3.1 Definitions of Terms Specific to This Standard:
solids of the freeze dried sample.
3.1.1 as received biomass—the biomass material as it is
1.3.2 Extractives-Free Sample (%T )—The percent, by
ext
received in its field or process collected state.
mass, of total solids of the extracted sample determined at
105°C.
3.1.2 oven-dried mass—themoisture-freemassofabiomass
sample dried at 105°C as described in Test Method E1756.
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 Nov. 15, 2007. Published January 2008. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1995. Last previous edition approved in 2001 as 1758–01. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E1758-01R07. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E1758 − 01 (2007)
3.1.3 prepared biomass—material that has been treated 4. Significance and Use
according to Practice E1757 in order to raise the total solids
4.1 The percentage, by mass, of sugar content is used in
content above 85%, by mass, based on an oven-dried solids
conjunction with other assays to determine the total composi-
mass.
tion of biomass samples.
3.2 Abbreviations—Abbreviations of standards used in the
procedure, and definitions of terms used in the calculations are 5. Interferences
as follows:
5.1 Samples with high protein content may result in the
3.2.1 C —known concentration of sugar recovery standard
1 percentage, by mass, of sugar values being biased low, as a
before hydrolysis, in mg/mL.
consequence of protein b
...

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.
e1
Designation:E1758–95 Designation:E1758–01 (Reapproved 2007)
Standard Test Method for
Determination of Carbohydrates in Biomass by High
1
Performance Liquid Chromatography
This standard is issued under the fixed designation E1758; 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.
1
e NOTE—Paragraphs 11.4 and 11.7 were updated editorially in October 1996.
INTRODUCTION
The carbohydrates making up a major portion of biomass samples are polysaccharides constructed
primarilyofglucose,xylose,arabinose,galactose,andmannosesubunits.Thepolysaccharidespresent
in a biomass sample can be hydrolyzed to their component sugar monomers by sulfuric acid in a
two-stage hydrolysis process. These monosaccharides can then be quantitatedquantified by ion-
moderated partition HPLC.
1. Scope
1.1 Thistestmethodcoversthedeterminationofcarbohydratespresentinabiomasssample,expressedasthepercent,bymass,
of each sugar on a 105°C dried mass basis.
NOTE 1—Thepercentsugarmustbecorrectedforthewaterofhydrolysisbeforecalculatingtheactualmasspercentofthepolysaccharideintheoriginal
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 As Received SamplesPrepared Biomass Samples:
1.3.1.1 Air Dried (%T ) —The percent, by mass, of total solids of the air-dried sample.
ad
1.3.1.2 45°C Dried (%T )—The percent, by mass, of total solids of the 45°C dried sample.
45
1.3.1.3 Freeze Dried (%T ) —The percent, by mass, of total solids of the freeze dried sample.
fd
1.3.2 Extractives-Free Sample (%T )—The percent, by mass, of total solids of the extracted sample determined at 105°C.
ext
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 precautionary statements are given in Note 2 Note 3 and Note 4.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
E1690 Test Method for the Determination of Ethanol Extractives in Biomass
E1721 Test Method for the Determination of Acid-Insoluble Residue in Biomass
E1756 Test Method for the 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 E-48 on Biotechnology and is the direct responsibility of Subcommittee E48.05 on Biomass Conversion.
Current edition approved Oct. 10, 1995. Published December 1995.
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. Published January 2008. Originally approved in 1995. Last previous edition approved in 2001 as 1758–01.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book of ASTM Standards
, Vol 11.01.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 ----------------------
E1758–01 (2007)
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 as received biomass—the biomass material as it is received in its field or process collected state.
3.1.2 oven-dried mass—the moisture-free mass of a biomass sample dried at 105°C as described in Test Method E1756.
3.1.3 prepared biomass—material that has been treated according to Practice E1757 in order to raise the total solids content
above 85%, by mass, based on an oven
...

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