ASTM E1690-08
(Test Method)Standard Test Method for Determination of Ethanol Extractives in Biomass
Standard Test Method for Determination of Ethanol Extractives in Biomass
SIGNIFICANCE AND USE
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.
This test method yields results comparable to Test Method D 1107.
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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: E1690 − 08
StandardTest Method for
1
Determination of Ethanol Extractives in Biomass
This standard is issued under the fixed designation E1690; 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.
1. Scope 3.1.2 oven-dried weight—the moisture-free corrected
weight of the prepared biomass sample. The correction factor
1.1 This test method covers the determination of ethanol
is determined in accordance with Test Method E1756.
solubleextractives,expressedasapercentageoftheoven-dried
biomass,ofhardandsoftwoods,herbaceousmaterials(suchas
3.1.3 prepared biomass—the biomass that has been pre-
switchgrass and sericea), agricultural residues (such as corn
pared in accordance with Practice E1757.
stover, wheat straw, and bagasse), and wastepaper (such as
office waste, boxboard, and newsprint).All results are reported
4. Significance and Use
relative to the oven-dried weight of the sample.
4.1 Ethanol extractives are any materials found in biomass
NOTE 1—This test method may not be suitable for hard and soft wood
that are soluble in ethanol. They are not considered to be part
samples that include bark or those with more than 10% extractable
of the structural components of biomass and should be re-
materials.
moved prior to any chemical analysis of the sample. The
1.2 The values stated in SI units are to be regarded as
prolonged extraction removes nonstructural materials that can
standard. No other units of measurement are included in this
includewaxes,fats,resins,tannins,gums,sugars,starches,and
standard.
pigments. Removing hydrophobic materials from the biomass
1.3 This standard does not purport to address all of the
makesiteasiertowetthematerialfortheanalysisofstructural
safety concerns, if any, associated with its use. It is the
components in the biomass.
responsibility of the user of this standard to establish appro-
4.2 This test method yields results comparable to Test
priate safety and health practices and determine the applica-
Method D1107.
bility of regulatory limitations prior to use.
5. Apparatus
2. Referenced Documents
2
2.1 ASTM Standards:
5.1 Soxhlet Extraction Apparatus, glass, of a size (100 mL)
D1107Test Method for Ethanol-Toluene Solubility ofWood
suitable for containing the sample and a 250-mL collection
E1756Test Method for Determination of Total Solids in
flask.
Biomass
5.2 Alundum Extraction Thimbles, medium porosity (10 to
E1757Practice for Preparation of Biomass for Composi-
15-µm pore), sized to fit the Soxhlet extractor.
tional Analysis
5.3 Analytical Balance, sensitive to 0.1 mg.
3. Terminology
5.4 Rotary Evaporator with Vacuum and Water Bath, con-
3.1 Definitions:
figured with a “bump” or safety trap, condenser, and receiving
3.1.1 ethanol extractives—the residue remaining after
vessel. A water aspirator will generally provide sufficient
evaporation of the ethanol solvent.These are materials that are
vacuum (<150 torr).
removed from the biomass by extraction with 190 proof
ethanol.
5.5 Vacuum Oven, controllable to 40 6 1°C and with
vacuum between 75 and 100 torr.
1
This test method is under the jurisdiction of ASTM Committee E48 on
BioenergyandIndustrialChemicalsfromBiomassandisthedirectresponsibilityof
6. Reagents and Materials
Subcommittee E48.05 on Biomass Conversion.
Current edition approved May 1, 2008. Published May 2008. Originally
6.1 Ethyl Alcohol, 190 proof, USP grade.
approved in 1995. Last previous edition approved in 2001 as E1690-01. DOI:
10.1520/E1690-08.
2 7. Sampling
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
7.1 The sample is milled material prepared in accordance
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. with Practice E1757.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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E1690 − 08
8. Procedure W 5 W 2 W 3 T/100% (1)
~ ! ~ !
s st t
8.1 Dry the Soxhlet extraction thimble in a drying oven at
where:
105°C overnight. Remove it and allow it to cool to room
W = weight of moisture-free solids in the prepared sample,
s
temperature in a desiccator.
g,
8.2 Weigh the Soxhlet extraction thimble to the nearest 0.1 W = weight of sample and thimble (8.2), g,
st
mg, and record the weight as W. Add a suitable quantity of W = tare weight of thimble (8.2), g, and
t t
T = percentageoftotalsolidsinthesample,asdetermined
sample to the extraction thimble. Do not over fill the thimble;
in accordance with
...
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:E1690–01 Designation:E1690–08
Standard Test Method for
1
Determination of Ethanol Extractives in Biomass
This standard is issued under the fixed designation E1690; 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. Scope
1.1 This test method covers the determination of ethanol soluble extractives, expressed as a percentage of the oven-dried
biomass,ofhardandsoftwoods,herbaceousmaterials(suchasswitchgrassandsericea),agriculturalresidues(suchascornstover,
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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D1107 Test Method for Alcohol-BenzeneEthanol-Toluene Solubility of Wood
E1756 Test Method for Determination of Total Solids in Biomass
E1757 Practice for Preparation of Biomass for Compositional Analysis
3. Terminology
3.1 Definitions:
3.1.1 ethanol extractives—the residue remaining after evaporation of the ethanol solvent.These are materials that are removed
from the biomass by extraction with 190 proof ethanol.
3.1.2 oven-dried weight—the moisture-free corrected weight of the prepared biomass sample. The correction factor is
determined in accordance with Test Method E1756.
3.1.3 prepared biomass—the biomass that has been prepared in accordance with Practice E1757.
4. 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.
4.2 This test method yields results comparable to Test Method D1107.
5. Apparatus
5.1 Soxhlet Extraction Apparatus , glass, of a size (100 mL) suitable for containing the sample and a 250-mL collection flask.
5.2 Alundum Extraction Thimbles , medium porosity (10 to 15-µm pore), sized to fit the Soxhlet extractor.
5.3 Analytical Balance, sensitive to 0.1 mg.
5.4 Rotary Evaporator with Vacuum and Water Bath, configured with a “bump” or safety trap, condenser, and receiving vessel.
A water aspirator will generally provide sufficient vacuum (<150 torr).
5.5 Vacuum Oven, controllable to 40 6 1°C and with vacuum between 75 and 100 torr.
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 November 10, 2001. Published February 2002. Originally published as E 1690-95. Last previous edition E 1690-95.
Current edition approved May 1, 2008. Published May 2008. Originally approved in 1995. Last previous edition approved in 2001 as E 1690-01.
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 ----------------------
E1690–08
6. Reagents and Materials
6.1 Ethyl Alcohol, 190 proof, USP grade.
7. Sampling
7.1 The sample is milled material prepared in accordance with Practice E1757.
8. Procedure
8.1 DrytheSoxhletextractionthimbleinadryingovenat105°Covernight.Removeitandallowittocooltoroomtemperature
in a desiccator.
8.2 Weigh the Soxhlet extraction thimble to the nearest 0.1 mg, and record th
...
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