ASTM E1690-95
(Test Method)Standard Test Method for Determination of Ethanol Extractives in Biomass
Standard Test Method for Determination of Ethanol Extractives in Biomass
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 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 the 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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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
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Designation: E 1690 – 95
Standard Test Method for
Determination of Ethanol Extractives in Biomass
This standard is issued under the fixed designation E 1690; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope soluble in ethanol. They are not considered to be part of the
structural components of biomass and should be removed prior
1.1 This test method covers the determination of ethanol
to any chemical analysis of the sample. The prolonged extrac-
soluble extractives, expressed as a percentage of the oven-dried
tion removes nonstructural materials that can include waxes,
biomass, of hard and soft woods, herbaceous materials (such as
fats, resins, tannins, gums, sugars, starches, and pigments.
switchgrass and sericea), agricultural residues (such as corn
Removing hydrophobic materials from the biomass makes it
stover, wheat straw, and bagasse), and wastepaper (such as
easier to wet the material for the analysis of structural
office waste, boxboard, and newsprint). All results are reported
components in the biomass.
relative to the oven-dried weight of the sample.
4.2 This test method yields results comparable to Test
1.2 The values stated in SI units are to be regarded as the
Method D 1107.
standard.
1.3 This standard does not purport to address all of the
5. Apparatus
safety concerns, if any, associated with its use. It is the
5.1 Soxhlet Extraction Apparatus, glass, of a size (100 mL)
responsibility of the user of this standard to establish appro-
suitable for containing the sample and a 250-mL collection
priate safety and health practices and determine the applica-
flask.
bility of regulatory limitations prior to use.
5.2 Alundum Extraction Thimbles, medium porosity (10 to
2. Referenced Documents 15-μm pore), sized to fit the Soxhlet extractor.
5.3 Analytical Balance, sensitive to 0.1 mg.
2.1 ASTM Standards:
5.4 Rotary Evaporator with Vacuum and Water Bath, con-
D 1107 Test Method for Alcohol-Benzene Solubility of
figured with a “bump” or safety trap, condenser, and receiving
Wood
vessel. A water aspirator will generally provide sufficient
E 1756 Test Method for Determination of Total Solids in
3 vacuum (<150 torr).
Biomass
5.5 Vacuum Oven, controllable to 40 6 1°C and with
E 1757 Practice for Preparation of Biomass for Composi-
3 vacuum between 75 and 100 torr.
tional Analysis
6. Reagents and Materials
3. Terminology
6.1 Ethyl Alcohol, 190 proof, USP grade.
3.1 Definitions:
3.1.1 ethanol extractives—the residue remaining after
7. Sampling
evaporation of the ethanol solvent. These are materials that are
7.1 The sample is milled material prepared in accordance
removed from the biomass by extraction with 190 proof
with Practice E 1757.
ethanol.
3.1.2 oven-dried weight—the moisture-free corrected
8. Procedure
weight of the prepared biomass sample. The correction factor
8.1 Dry the Soxhlet extraction thimble in a drying oven at
is determined in accordance with Test Method E 1756.
105°C overnight. Remove it and allow it to cool to room
3.1.3 prepared biomass—the biomass that has been pre-
temperature in a desiccator.
pared in accordance with Practice E 1757.
8.2 Weigh the Soxhlet extraction thimble to the nearest 0.1
4. Significance and Use mg, and record the weight as W . Add a suitable quantity of
st
sample to the extraction thimble. Do not over fill the thimble;
4.1 Extractives are any materials found in biomass that are
the largest sample should still leave approximately 1 cm of free
space in the top of the thimble. Weigh to the nearest 0.1 mg,
This test method is under the jurisdiction of ASTM Committee E-48 on and record this weight as W .
st
Biotechnology and is the direct responsibility of Subcommittee E48.05 on Biomass
NOTE 1—The precision for quantitation of the extractives weight is
Conversion.
Current edition approved Oct 10, 1995. Published December 1995. based on a nominal 7-g prepared sample weight. Smaller samples will
Annual Book of ASTM Standards, Vol 04.10.
introduce a larger relative error.
Annual Book of ASTM Standards, Vol 11.05.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
E 1690
NOTE 2—The samples for total solids determination should be weighed
W 5 tare weight of thimble (8.2), g, and
t
out at the same time as those for extractives determination. If this is
T 5 percentage of total solids in the sample, as deter-
performed at a later tim
...
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