Standard Test Method for Ash in Biomass

SIGNIFICANCE AND USE
4.1 The ash content is an approximate measure of the mineral content and other inorganic matter in biomass.  
4.2 The ash 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 ash, expressed as the mass percent of residue remaining after dry oxidation (oxidation at 575 ± 25°C), of 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 and alkaline pretreated biomass, and the solid fraction of fermentation residues. All results are reported relative to the 105°C oven-dried mass of the sample. For particulate wood fuels, Test Method E1534 should be used.  
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E1755 − 01 (Reapproved 2015)
Standard Test Method for
Ash in Biomass
This standard is issued under the fixed designation E1755; 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.
1. Scope 4. Significance and Use
1.1 This test method covers the determination of ash, 4.1 The ash content is an approximate measure of the
expressed as the mass percent of residue remaining after dry mineral content and other inorganic matter in biomass.
oxidation (oxidation at 575 6 25°C), of hard and soft woods,
4.2 The ash content is used in conjunction with other assays
herbaceous materials (such as switchgrass and sericea), agri-
to determine the total composition of biomass samples.
cultural residues (such as corn stover, wheat straw, and
bagasse), wastepaper (such as office waste, boxboard, and
5. Apparatus
newsprint), acid and alkaline pretreated biomass, and the solid
5.1 Ashing Crucibles, 50 mL, platinum crucibles are
fraction of fermentation residues. All results are reported
preferred, but silica or porcelain crucibles may be used.
relative to the 105°C oven-dried mass of the sample. For
5.2 Muffle Furnace, an electric furnace is recommended for
particulate wood fuels, Test Method E1534 should be used.
igniting the sample. The furnace should be fitted with an
1.2 The values stated in SI units are to be regarded as the
indicating pyrometer or thermocouple, so that the required
standard.
temperature of 575 6 25°C can be maintained.
1.3 This standard does not purport to address all of the
5.3 Analytical Balance, sensitive to 0.1 mg.
safety concerns, if any, associated with its use. It is the
5.4 Desiccator, using anhydrous calcium sulfate.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5.5 Drying Oven, with temperature control of 105 6 2°C.
bility of regulatory limitations prior to use.
6. Test Specimen
2. Referenced Documents
6.1 Test specimens suitable for analysis by this test method
are as follows:
2.1 ASTM Standards:
6.1.1 Prepared biomass samples that have been prepared
E1534 Test Method for Determination of Ash Content of
according to Practice E1757.
Particulate Wood Fuels
6.1.2 Biomass feedstocks, dried at 105°C according to Test
E1756 Test Method for Determination of Total Solids in
Method E1756,
Biomass
6.1.3 Pretreated biomass, dried at 105°C according to Test
E1757 Practice for Preparation of Biomass for Composi-
Method E1756, and
tional Analysis
6.1.4 The solids fraction of fermentation residues, dried at
105°C according to Test Method E1756.
3. Terminology
6.2 The test specimen shall consist of approximately 0.5 to
3.1 Definitions of Terms Specific to This Standard:
1.0 g of sample obtained in such a manner to ensure that it is
3.1.1 ash—the inorganic residue left after ignition at 575 6
representative of the entire lot of material being tested.
25°C.
NOTE 1—All samples should be ground or milled to reduce the size of
the large pieces to less than 1 mm in diameter. The sample is then redried
at 105°C prior to testing. Prepared biomass can be used in place of 105°C
This test method is under the jurisdiction of ASTM Committee E48 on
dried material, but the mass of the material must be corrected for its
Bioenergy and Industrial Chemicals from Biomass and is the direct responsibility of
moisturecontentbyusingTestMethodE1756,priortocalculatingtheash.
Subcommittee E48.05 on Biomass Conversion.
CurrenteditionapprovedJune1,2015.PublishedJuly2015.Originallyapproved
7. Procedure
in 1995. Last previous edition approved in 2007 as E1755-01(2007)07. DOI:
10.1520/E1755-01R15.
7.1 Markapanorcruciblewithauniqueidentificationusing
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
a porcelain marker, place it in the muffle furnace at 575 6
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
25°C. Remove the pan or crucible from the furnace, cool to
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. room temperature in a desiccator, and weigh to the nearest 0.1
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1755 − 01 (2015)
mg. For an aluminum pan, two hours of heating at 575 6 25°C provided that the test specimen has already been analyzed for
will be sufficient to bring the pan to constant mass. With a mass percent total solids at 105°C using Test Method E1756.
crucible, however, the following procedure is used: place the
m 5 m 2 m 3T/100 (2)
~ !
s ar cont
crucible in the furnace at 575 6 25°C for 3 h. Remove the
where:
crucible and place in a desiccator.Allow the crucible to cool to
m = mass of moisture-free solids in the prepared biomass
room temperature and then weigh the crucible to the nearest
s
0.1 mg. Record this mass. After weighing, return the crucible sample, g,
m = initial mass of prepared biomass sample and
to the furnace for1hat575 6 25°C, cool again in the
ar
container, g,
desiccator, and reweigh. Repeat this step until the mass of the
m = tare mass of container, g, and
cruciblevariesbylessthan0.3mgfromthepreviousweighing. cont
T = mass percent of total solids in sample, as determined
Recordthisfinalmassasthecrucibletaremass, m .Keepthe
cont
by Test Method E1756.
pan or crucible in a desiccator until used.
% ash 5 @~m 2 m !/m # 3100 (3)
7.2 Weigh approximately 0.5 to 1.0 g, to the nearest 0.1 mg, ash cont s
of a test specimen into the tared pan or crucible. If the sample
where:
being analyzed is a test specimen dried at 105°C, the sample
% ash = mass percent of ash, based on 105°C oven-dried
should be stored in a desiccator until use. For a 105°C dried
mass of the sample,
test sample, record the mass (container plus sample mass) as
m = mass of ash and container, g,
ash
the initial mass, m . For prepared biomass samples prepped
od
m = tare mass of container, g, and
cont
according to Practice E1757, record the mass (container plus
m = mass of moisture-free solids in the prepared bio-
s
sample mass) as the initial mass, m .
ar mass sample, g.
NOTE 2—For prepared biomass samples, it is recommend that samples
9. Report
for moisture determination should be weighed out at the same time as the
samples for the ash determination. If this is done at a later time it can
9.1 Report the result to two decimal places, as a mass
introduce an error in the calculation because ground biomass can rapidly
percent of the sample’s 105°C dried mass, and cite the basis
gain or lose moisture when exposed to the atmosphere.
used in the calculation.
7.3 Place the container and contents in the muff
...


This document is not an ASTM standard and is intended only to provide the user of an ASTM 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: E1755 − 01 (Reapproved 2007) E1755 − 01 (Reapproved 2015)
Standard Test Method for
Ash in Biomass
This standard is issued under the fixed designation E1755; 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.
1. Scope
1.1 This test method covers the determination of ash, expressed as the mass percent of residue remaining after dry oxidation
(oxidation at 575 6 25°C), of 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 and alkaline
pretreated biomass, and the solid fraction of fermentation residues. All results are reported relative to the 105°C oven-dried mass
of the sample. For particulate wood fuels, Test Method E1534 should be used.
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.
2. Referenced Documents
2.1 ASTM Standards:
E1534 Test Method for Determination of Ash Content of Particulate Wood Fuels
E1756 Test Method for Determination of Total Solids in Biomass
E1757 Practice for Preparation of Biomass for Compositional Analysis
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 ash—the inorganic residue left after ignition at 575 6 25°C.
4. Significance and Use
4.1 The ash content is an approximate measure of the mineral content and other inorganic matter in biomass.
4.2 The ash content is used in conjunction with other assays to determine the total composition of biomass samples.
5. Apparatus
5.1 Ashing Crucibles, 50 mL, platinum crucibles are preferred, but silica or porcelain crucibles may be used.
5.2 Muffle Furnace, an electric furnace is recommended for igniting the sample. The furnace should be fitted with an indicating
pyrometer or thermocouple, so that the required temperature of 575 6 25°C can be maintained.
5.3 Analytical Balance, sensitive to 0.1 mg.
5.4 Desiccator, using anhydrous calcium sulfate.
5.5 Drying Oven, with temperature control of 105 6 2°C.
6. Test Specimen
6.1 Test specimens suitable for analysis by this test method are as follows:
6.1.1 Prepared biomass samples that have been prepared according to Practice E1757.
This test method is under the jurisdiction of ASTM Committee E48 on Bioenergy and Industrial Chemicals from Biomass and is the direct responsibility of Subcommittee
E48.05 on Biomass Conversion.
Current edition approved Nov. 15, 2007June 1, 2015. Published January 2008July 2015. Originally approved in 1995. Last previous edition approved in 20012007 as
E1755E1755-01(2007)-01.07. DOI: 10.1520/E1755-01R07.10.1520/E1755-01R15.
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 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
E1755 − 01 (2015)
6.1.2 Biomass feedstocks, dried at 105°C according to Test Method E1756,
6.1.3 Pretreated biomass, dried at 105°C according to Test Method E1756, and
6.1.4 The solids fraction of fermentation residues, dried at 105°C according to Test Method E1756.
6.2 The test specimen shall consist of approximately 0.5 to 1.0 g of sample obtained in such a manner to ensure that it is
representative of the entire lot of material being tested.
NOTE 1—All samples should be ground or milled to reduce the size of the large pieces to less than 1 mm in diameter. The sample is then redried at
105°C prior to testing. Prepared biomass can be used in place of 105°C dried material, but the mass of the material must be corrected for its moisture
content by using Test Method E1756, prior to calculating the ash.
7. Procedure
7.1 Mark a pan or crucible with a unique identification using a porcelain marker, place it in the muffle furnace at 575 6 25°C.
Remove the pan or crucible from the furnace, cool to room temperature in a desiccator, and weigh to the nearest 0.1 mg. For an
aluminum pan, two hours of heating at 575 6 25°C will be sufficient to bring the pan to constant mass. With a crucible, however,
the following procedure is used: place the crucible in the furnace at 575 6 25°C for 3 h. Remove the crucible and place in a
desiccator. Allow the crucible to cool to room temperature and then weigh the crucible to the nearest 0.1 mg. Record this mass.
After weighing, return the crucible to the furnace for 1 h at 575 6 25°C, cool again in the desiccator, and reweigh. Repeat this
step until the mass of the crucible varies by less than 0.3 mg from the previous weighing. Record this final mass as the crucible
tare mass, m . Keep the pan or crucible in a desiccator until used.
cont
7.2 Weigh approximately 0.5 to 1.0 g, to the nearest 0.1 mg, of a test specimen into the tared pan or crucible. If the sample being
analyzed is a test specimen dried at 105°C, the sample should be stored in a desiccator until use. For a 105°C dried test sample,
record the mass (container plus sample mass) as the initial mass, m . For prepared biomass samples prepped according to Practice
od
E1757, record the mass (container plus sample mass) as the initial mass, m .
ar
NOTE 2—For prepared biomass samples, it is recommend that samples for moisture determination should be weighed out at the same time as the
samples for the ash determination. If this is done at a later time it can introduce an error in the calculation because ground biomass can rapidly gain or
lose moisture when exposed to the atmosphere.
7.3 Place the container and contents in the muffle furnace and ignite at 575 6 25°C for a minimum of 3 h, or until all the carbon
is eliminated. To avoid flaming, initially heat the sample to 250°C at a rate of 10 K/min and hold for 30 min before increasing the
temperature to 575 6 25°C. Avoid heating above the maximum stated temperature.
NOTE 3—For test specimens containing high amounts of ash (greater than 5 % by mass), it will be necessary to increase the time in the furnace to
overnight to ensure complete elimination of the carbon. This ignition time period should not exceed 24 h.
7.4 Taking care to protect the test container from strong drafts to avoid mechanical loss of test specimen, remove the pan or
crucible with its contents t
...

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