ASTM E1757-01(2007)
(Practice)Standard Practice for Preparation of Biomass for Compositional Analysis
Standard Practice for Preparation of Biomass for Compositional Analysis
SIGNIFICANCE AND USE
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 ¼ in.) or less and twigs not exceeding 0.6 cm (¼ in.) diameter. Herbaceous materials may be processed as whole straw. It is recommended that wastepaper should be shredded into pieces less then 1 cm (½ in.) wide. Furthermore, it is recommended that twigs, straw and wastepaper should not exceed 61 cm (24 in.) in length to facilitate handling.
Preparation Methods B and C—Test 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 (20 g). The drying step is done in a convection oven at 45°C (Test Method B) or by lyophilization (Test Method C).
This practice is not intended for materials that will already pass through a 20 mesh sieve or cannot be dried by the described methods to a total solids content of greater then 85 %, based on an oven dried weight.
This practice will separate the milled material into two fractions, a −20/+80 mesh fraction and a −80 mesh fraction.
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.
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), feedstocks pretreated to improve suitability for fermentation and fermentation residues into a uniform material suitable for compositional 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 the standard. The inch-pound units given in parentheses are for information only.
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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: E1757 − 01(Reapproved 2007)
Standard Practice for
Preparation of Biomass for Compositional Analysis
This standard is issued under the fixed designation E1757; 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 prepared biomass—biomass that has been prepared
according to this practice.
1.1 This practice covers a reproducible way to convert
hardwoods, softwoods, herbaceous materials (such as switch-
4. Significance and Use
grass and sericea), agricultural residues (such as corn stover,
4.1 Preparation Method A—Method suitable for the prepa-
wheat straw, and bagasse), wastepaper (such as office waste,
rationoflargequantities(>20g)offieldcollectedsamplesinto
boxboard, and newsprint), feedstocks pretreated to improve
a form appropriate for compositional analysis.Woody samples
suitability for fermentation and fermentation residues into a
must first be available as chips of a nominal 5 by 5 by 0.6 cm
uniform material suitable for compositional analysis.
1 1
(2 by 2 by ⁄4 in.) or less and twigs not exceeding 0.6 cm ( ⁄4
1.2 Milling and sieving actions both produce large amounts
in.)diameter.Herbaceousmaterialsmaybeprocessedaswhole
of dust. This dust can be a nuisance hazard and irritant. Use
straw. It is recommended that wastepaper should be shredded
appropriate respiratory protection as needed. If excessive 1
into pieces less then 1 cm ( ⁄2 in.) wide. Furthermore, it is
amounts of dust are allowed to become airborne a potential
recommended that twigs, straw and wastepaper should not
explosion hazard is possible. Provide appropriate dust control
exceed 61 cm (24 in.) in length to facilitate handling.
measures as needed.
4.2 Preparation Methods B and C—Test methods are suit-
1.3 The values stated in SI units are to be regarded as the
able for very moist feedstocks, samples that would not be
standard. The inch-pound units given in parentheses are for
stable during prolonged exposure to ambient conditions, or for
information only.
drying materials when room conditions deviate from the
1.4 This standard does not purport to address all of the ambient conditions described in 3.1.1. These test methods are
safety concerns, if any, associated with its use. It is the also suitable for handling small samples of biomass (<20 g).
responsibility of the user of this standard to establish appro- The drying step is done in a convection oven at 45°C (Test
priate safety and health practices and determine the applica- Method B) or by lyophilization (Test Method C).
bility of regulatory limitations prior to use.
4.3 This practice is not intended for materials that will
alreadypassthrougha20meshsieveorcannotbedriedbythe
2. Referenced Documents
described methods to a total solids content of greater then
2.1 ASTM Standards:
85%, based on an oven dried weight.
E11Specification forWovenWireTest Sieve Cloth andTest
4.4 This practice will separate the milled material into two
Sieves
fractions, a −20/+80 mesh fraction and a −80 mesh fraction.
4.4.1 Extraneous inorganic materials will accumulate in the
3. Terminology
-80 mesh fraction and it should be analyzed independently
3.1 Definitions of Terms Specific to This Standard: fromthe-20/+80meshfraction.Weightedresultsfromthetwo
3.1.1 ambient conditions—a temperature of 20 to 30°C (68 fractions can then be combined to obtain results for materials
to 85°F), less than 50% relative humidity. on an "as received" basis.
NOTE 1—During analysis, the very fine consistency of the -80 mesh
fractionmaycauseproblemsinfilteringoperationsandshouldbehandled
1 appropriately.
This practice is under the jurisdiction ofASTM Committee E48 on Bioenergy
and Industrial Chemicals from Biomass and is the direct responsibility of Subcom-
5. Apparatus
mittee E48.05 on Biomass Conversion.
Current edition approved Nov. 15, 2007. Published March 2008. Originally
5.1 Balance, sensitive to 0.1 g.
approved in 1995. Last previous edition approved in 2001 as E1757-01. DOI:
10.1520/E1757-01R07.
5.2 Riffle Sampler with Pans—Amanualsampledividerthat
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
splits the milled biomass into a number of alternate elements.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Riffledivisionsshouldbeintherangefrom6.4mmto12.7mm
Standards volume information, refer to the standard’s Document Summary page on
1 1
the ASTM website. ( ⁄4to ⁄2in.)withatleasttwenty-fourriffleopeningsacrossthe
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1757 − 01 (2007)
top. The feed chute and riffles should have a slope of at least 6.8 If multiple sieved samples were combined they must be
60°. Three pans are needed, one to pour the sample into the uniformlyblendedbacktogetherintoasinglesample.Pourthe
riffler, and two to collect the two subsamples. −20/+80 mesh fraction into the riffle sampler, and then recom-
bine the two subdivided samples in the bottom pans back
5.3 Sieve Set, No. 20 (850 µm), No. 80 (180 µm) stackable
together. Repeat this division and recombination an additional
sieves with lid and bottom pan. Sieves and bottom pan should
threetimes.Tocorrectlyusetherifflesampler,thesamplemust
be 8.9 cm (3 ⁄2 in.) in height. Sieves conform to Specification
be poured evenly onto all the riffle openings at the same time.
E11.
A pan, as wide as the riffle opening, should be used. Pour the
5.4 Sieve Shaker, provides motion in both horizontal and
sample evenly off the entire side of the pan and not from the
vertical axes.
end or the corner, nor from a container such as a jar.
5.5 Knife Mill, for grinding samples.
6.9 If the total sample needs to be subdivided into smaller
samples, use the riffler at this time to divide the main sample.
NOTE 2—AWiley Mill, size No. 4 with a 2-mm screen, is suitable for
samples >20 g, and the intermediate model, with 1-mm screen, is suitable
6.10 If the prepared sample is not analyzed immediately
for samples <20 g that will not be sieved.
after sieving and riffling, the sample should be stored in an
5.6 Drying Oven, 456 3° (Test Method B only).
air-tight container or sealable polyethylene bag and kept at
−20°C until needed.
5.7 Freeze-Drier—System with vacuum chamber and pump
capable of maintaining a pressure of <1 torr and a cold finger
7. Report: Preparation Method A
in the chamber capable of maintaining a temperature of −50°C
7.1 Calculate the percent of each fraction in the original,
(Test Method C only).
whole biomass:
fraction ,% 5 ~Wt 3100%!/~Wt 1Wt ! (1)
6. Preparation: Test Method A
20/80 20/80 20/80 80
6.1 This test method is suitable for larger quantities (>20 g) where:
of biomass as described in 4.1.
Wt = weight of −20/+80 mesh fraction, g, and
20/80
Wt = weight of fines fraction, g.
6.2 The raw biomass material should be spread out on a
suitable surface to air dry prior to any milling. Do not pile the fraction ,% 5 100%2fraction % (2)
80 20/80
material deeper then 15 cm. Turn the material at least daily to
7.2 The mass fraction is used to weigh analytical results
ensureevendryingandminimizemoldingofmaterialthatmay
whenthetwofractionsdifferincomposition,buttheresultsare
contain significant amounts of moisture. The material is
to be reported on the original, whole biomass.
considered dried whenthechangeinweightislessthan1%in
8. Procedure: Preparation Method B
24 h.
8.1 This test method is suitable for very wet biomass that is
6.3 The air-dried material is fed into the knife-mill and is
at risk for mold growth during drying, for wet pretreated
milledtopassthrougha2mmscreeninthebottomofthemill.
biomass or fermentation residues (sludges) that might degrade
Milled wastepaper does not need to be sieved and can be used
ifallowedtostandforprolongedperiods,orfordryingbiomass
directly for composition analysis. Milled biomass materials
when the prevailing conditions do not meet the ambient
should be sieved as foll
...
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:E1757–95 Designation: E 1757 – 01 (Reapproved 2007)
Standard Practice for
Preparation of Biomass for Compositional Analysis
This standard is issued under the fixed designation E1757; 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 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),feedstockspretreatedtoimprovesuitabilityforfermentationandfermentationresiduesintoauniformmaterialsuitable
for compositional 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 the standard. The inch-pound units given in parentheses are for
information only.
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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
E11Specification for Wire-Cloth Sieves for Testing Purposes Specification for Wire Cloth and Sieves for Testing Purposes
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 ambient conditions—a temperature of 20 to 30°C (68 to 85°F), less than 50% relative humidity.
3.1.2 prepared biomass—biomass that has been prepared according to this practice to reduce the moisture content to below
15%, based on an oven-dried solids weight. —biomass that has been prepared according to this practice.
4. Significance and Use
4.1 TestPreparation MethodA—PMethod 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
1 1
by2by ⁄4 in.) or less and twigs not exceeding 0.6 cm ( ⁄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 ( ⁄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 TestPreparation Methods B and C—Test methods that 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 (<20 g).The drying step
is done in a convection oven at 45°C (Test Method B) or by lyophilization (Test Method C).
4.3 Thispracticeisnotintendedformaterialsthatwillalreadypassthrougha20meshsieveorcannotbedriedbythedescribed
methods to a total solids content of greater then 85%, based on an oven dried weight.
4.4This practice will separate the milled material into two fractions, a −20/+80 mesh fraction and a −80 mesh fraction.
Extraneousinorganicmaterialswillaccumulateinthe−80meshfractionanditshouldbeanalyzedindependentlyfromthe−20/+80
mesh fraction.
4.4 This practice will separate the milled material into two fractions, a −20/+80 mesh fraction and a −80 mesh fraction.
This practice is under the jurisdiction of ASTM 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.
This practice is under the jurisdiction of ASTM Committee E48 on Biotechnology and is the direct responsibility of Subcommittee E48.05 on Biomass Conversion.
Current edition approved Nov. 15, 2007. Published March 2008. Originally approved in 1995. Last previous edition approved in 2001 as E1757-01.
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.ForAnnualBookofASTMStandards
, Vols 04.02 and 14.02.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.
E 1757 – 01 (2007)
4.4.1 Extraneousinorganicmaterialswillaccumulateinthe-80meshfractionanditshouldbeanalyzedindependentlyfromthe
-20/+80 mesh fraction. Weighted results from the two fractions can then be combined to obtain results for materials on an 9as
received9 basis.
NOTE1—During analysis, the very fine consistency of this fraction may cause problems in filtrating operations and should be handled appropriately.
4.4.1Weighted results from the two fractions can then be combined to obtain results for materials on an “as received” basis.
1—During analysis, the very fine consistency of the -80 mesh fraction may cause problems in filtering operations and should be
handled appropriately.
5. Apparatus
5.1 Balance, sensitive to 0.1 g.
5.2 RiffleSamplerwithPans—Amanualsampledividerthatsplitsthemilledbiomassintoanumberofalternateelements.Riffle
1 1
divisions should be in the range from 6.4 mm to 12.7 mm ( ⁄4 to ⁄2 in.) with at least twenty-four riffle openings across the top.
The feed chute and riffles should have a slope of at least 60°. Three pans are needed, one to pour the sample into the riffler, and
two to collect the two subsamples.
5.3 Sieve Set, No. 20 (850 µm), No. 80 (180 µm) stackable sieves with lid and bottom pan. Sieves and bottom pan should be
8.9 cm (3 ⁄2 in.) in height. Sieves conform to Specification E11.
5.4 Sieve Shaker, provides motion in both horizontal and vertical axes.
5.5 Knife Mill, for grinding samples.
NOTE 2—AWiley Mill, size No. 4 with a 2-mm screen, is suitable for samples >20 g, and the intermediate model, with 1-mm screen, is suitable for
samples <20 g that will not be sieved.
5.6 Drying Oven,456 3° (Test Method B only).
5.7 Freeze-Drier—System with vacuum chamber and pump capable of maintaining a pressure of <1 torr and a cold finger in
the chamber capable of maintaining a temperature of −50°C (Test Method C only).
6. Procedure: Test Method A
6.1This test method is suitable for larger quantities (>20 g) of biomass that are essentially still in a field collected state.
Preparation: Test Method A
6.1 This test method is suitable for larger quantities (>20 g) of biomass as described in 4.1.
6.2 The raw biomass material should be spread out on a suitable surface to air dry prior to any milling. Do not pile the material
deeper then 15 cm. Turn the material at least daily to ensure even drying and minimize molding of material that may contain
significant amounts of moisture. The material is considered dried when the change in weight is less than 1% in 24 h.
6.3 Theair-driedmaterialisfedintotheknife-millandismilledtopassthrougha2mmscreeninthebottomofthemill.Milled
wastepaperdoesnotneedtobesievedandcanbeuseddirectlyforcompositionanalysis.Milledbiomassmaterialsshouldbesieved
as follows.
6.4 The sieving is set up by stacking the sieves in the following order, starting at the bottom: start with the bottom pan, next
stack the 80 mesh sieve, followed by the 20 mesh sieve. Milled material is placed no more then 7 cm deep in the 20 mesh sieve.
6.5 Place the cover on the sieve stack and secure the stack in the sieve shaker.
6.6 The sieves need to be shaken for 15 6 1 min.At the end of the time period remove the sieves.The fraction retained on the
20 mesh sieve (+20 mesh fraction) should be remilled through the knife-mill.reprocessed beginning at step 6.3. The fraction
retained on the 80 mesh sieve (−20/+80 mesh fraction) should be retained for compositional analysis. The material in the bottom
pan is the fines (−80 mesh). Retain this material for ash analysis.
6.7 Repeat 6.3-6.6 until all of the milled material will pass through the 20 mesh sieve. Combine each of the appropriate sieve
fractions with the previously collected fraction. Weigh the −20/+80 mesh fraction and the fines to the nearest 0.1 g. Record the
−20/+80 mesh fraction weight as until all of the milled material will pass through the 20 mesh sieve. If necessary, combine all of
the -20/+80 mesh batches. If necessary, combine all of -80 mesh batches. Weigh the combined −20/+80 mesh fraction and the
combined fines to the nearest 0.1 g. Record the −20/+80 mesh fraction weight as Wt and the fines fraction weight as Wt .
...
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