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ASTM E1756-01

(Test Method)

Standard Test Method for Determination of Total Solids in Biomass

Standard Test Method for Determination of Total Solids in Biomass

SIGNIFICANCE AND USE
Moisture is a ubiquitous and variable component of any biomass sample. Moisture is not considered a structural component of biomass and can change with storage and handling of biomass samples. The determination of the total solids content allows for the correction of biomass samples to an oven-dried solids mass that is constant for a particular sample.
This procedure is not suitable for biomass samples that visibly change on heating to 105°C, for example, unwashed acid-pretreated biomass still containing free acid.
Some materials that contain large amount of free sugars or proteins will caramelize or brown under direct infrared heating elements used in Test Method B. Total solids in these materials should be done by Test Method A.
SCOPE
1.1 This test method covers the determination of the amount of total solids remaining after drying a sample. Materials suitable for this procedure include samples prepared in accordance with Practice E 1757 and extractive-free material prepared in accordance with Test Method E 1690. For particulate wood fuels, Test Method E 871 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.

General Information

Status
Historical
Publication Date
09-Nov-2001
ICS
65.040.20 - Buildings and installations for processing and storage of agricultural produce
Technical Committee
E48 - Bioenergy and Industrial Chemicals from Biomass
Drafting Committee
E48.05 - Biomass Conversion
Current Stage
Ref Project

Relations

Replaces
ASTM E1756-95 - Standard Test Method for Determination of Total Solids in Biomass
Effective Date
10-Nov-2001
Replaced By
ASTM E1756-08 - Standard Test Method for Determination of Total Solids in Biomass
Effective Date
01-May-2008
Referred By
ASTM E1721-01(2020) - Standard Test Method for Determination of Acid-Insoluble Residue in Biomass
Effective Date
10-Nov-2001
Referred By
ASTM E1821-08(2020) - Standard Test Method for Determination of Carbohydrates in Biomass by Gas Chromatography
Effective Date
10-Nov-2001
Referred By
ASTM E1758-01(2020) - Standard Test Method for Determination of Carbohydrates in Biomass by High Performance Liquid Chromatography
Effective Date
10-Nov-2001
Referred By
ASTM E1690-08(2021) - Standard Test Method for Determination of Ethanol Extractives in Biomass
Effective Date
10-Nov-2001
Referred By
ASTM E1755-01(2020) - Standard Test Method for Ash in Biomass
Effective Date
10-Nov-2001

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ASTM E1756-01 - Standard Test Method for Determination of Total Solids in Biomass
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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: E 1756 – 01
Standard Test Method for
1
Determination of Total Solids in Biomass
This standard is issued under the fixed designation E 1756; 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.
INTRODUCTION
The total solids content is used to adjust the mass of the biomass so that all analytical results may
be reported on a moisture-free basis. Total solids content may be determined by overnight drying at
105°C in a convection oven or with a loss-on-drying moisture analyzer.
1. Scope purposes of this procedure, the moisture content of a biomass
sample is considered to be the amount of mass lost during the
1.1 This test method covers the determination of the amount
drying of the sample at 105°C to constant mass. An inherent
of total solids remaining after drying a sample. Materials
error of this and any oven-drying procedure is that volatile
suitable for this procedure include samples prepared in accor-
substances other than water are removed from the sample
dance with Practice E 1757 and extractive-free material pre-
during drying.
pared in accordance with Test Method E 1690. For particulate
3.1.2 prepared biomass—the biomass that has been pro-
wood fuels, Test Method E 871 should be used.
cessed according to Practice E 1757.
1.2 The values stated in SI units are to be regarded as the
standard.
4. Significance and Use
1.3 This standard does not purport to address all of the
4.1 Moisture is a ubiquitous and variable component of any
safety concerns, if any, associated with its use. It is the
biomass sample. Moisture is not considered a structural com-
responsibility of the user of this standard to establish appro-
ponentofbiomassandcanchangewithstorageandhandlingof
priate safety and health practices and determine the applica-
biomass samples. The determination of the total solids content
bility of regulatory limitations prior to use.
allows for the correction of biomass samples to an oven-dried
2. Referenced Documents solids mass that is constant for a particular sample.
2
4.2 This procedure is not suitable for biomass samples that
2.1 ASTM Standards:
visibly change on heating to 105°C, for example, unwashed
E 871 Method for Moisture Analysis of Particulate Wood
acid-pretreated biomass still containing free acid.
Fuels
4.3 Some materials that contain large amount of free sugars
E 1690 Test Method for Determination of Ethanol Extrac-
or proteins will caramelize or brown under direct infrared
tives in Biomass
heating elements used in Test Method B. Total solids in these
E 1757 Practice for Preparation of Biomass for Composi-
materials should be done by Test Method A.
tional Analysis
5. Apparatus and Materials
3. Terminology
5.1 Analytical Balance, sensitive to 0.1 mg.
3.1 Descriptions of Terms Specific to This Standard:
5.2 Drying Oven, 105 6 3°C (Test Method A only).
3.1.1 oven-dried solids—the solids remaining after heating
5.3 Desiccator, containing anhydrous calcium sulfate (Test
the prepared biomass at 105°C to constant mass. For the
Method A only).
3
5.4 MoistureAnalyzer, infraredheated,20gcapacity,1mg
1
This test method is under the jurisdiction of ASTM Committee E48 on resolution (Test Method B only).
Biotechnology and is the direct responsibility of Subcommittee E48.05 on Biomass
5.5 Drying Pans, disposable, aluminum, 10 cm diameter,
Conversion.
suitable for moisture analyzer (Test Method B only).
Current edition approved November 10, 2001. Published February 2002.
Originally published as E1756-95. Last previous edition E1756-95.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM A Denver Instruments, Model IR-100, available from Denver Instrument
Standards volume information, refer to the standard’s Document Summary page on Company,6542FigSt.,Arvada,CO80004,hasbeenfoundtobesatisfactoryforthis
the ASTM website. purpose.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E1756–01
TABLE 1 Critical Difference, Percent of Grand Average, For the
8. Calculation: Test Method A
A,B
Conditions Noted
8.1 Calculate the mass percent of the total solids obtained
Number of
by drying at 105°C as
Observations Single Operator
Test Conditions
in Precision
%T 5 ~m 2 m !/~m 2 m ! 3 100 % (1)
105 f1 t i1 t
Each Average
Test Method A, hybrid poplar 1 0.55 where:
2 0.39
%T = mass percent of total solids based on 105°C dry
105
Test Method A, fermentation residue 1 1.35
mass,
2 0.95
m = tar
...

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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.  
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4.1 The ash content is an approximate measure of the mineral content and other inorganic matter in biomass.  
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4.1 The structural carbohydrate content is used in conjunction with other assays to determine the total composition of biomass samples.
SCOPE
1.1 This test method describes the determination of structural carbohydrates present in a biomass sample, expressed as the percent mass of an oven-dried sample basis of each anhydrosugar.  
1.2 Sample materials suitable for this procedure include hard and softwoods, herbaceous materials, such as sericea and switchgrass, agricultural residues, such as corn stover, wheat straw, and bagasse, wastepaper, such as boxboard, office waste, and newsprint, acid or alkaline-pretreated biomass, washed free of any residual acid or alkali, and the solid fraction of fermentation residues.  
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1.1 This test method covers determination of the acid-insoluble residue 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 weight of the sample.  
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4.3 Some materials that contain large amount of free sugars or proteins will caramelize or brown under direct infrared heating elements used in Test Method B. Total solids in these materials should be done by Test Method A.
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1.1 This test method covers the determination of the amount of total solids remaining after drying a sample. Materials suitable for this procedure include samples prepared in accordance with Practice E1757 and extractive-free material prepared in accordance with Test Method E1690. For particulate wood fuels, Test Method E871 should be used.  
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SIGNIFICANCE AND USE
4.1 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 1/4 in.) or less and twigs not exceeding 0.6 cm (1/4 in.) diameter. Herbaceous materials may be processed as whole straw. It is recommended that wastepaper should be shredded into pieces less then 1 cm (1/2 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 Preparation Methods B and C—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 (  
4.3 Preparation Methods A, B, and C are not intended for materials that will already pass through a 20 mesh sieve or that cannot be dried by the described methods to a total solids content of greater than 85 %, based on an oven dried weight.  
4.4 Preparation Method A will separate the milled material into two fractions, a −20/+80 mesh fraction and a −80 mesh fraction.  
4.4.1 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.  
4.5 Preparation Method D—Method suitable for cereal grains, cereal grain fermentation mash, cereal grain fermentation beer, and cereal grain fermentation residues that are generally stable.  
4.6 Preparation Method E—Method suitable for ce...
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), cellulosic feedstocks pretreated to improve suitability for fermentation, cereal grains, cereal grain fermentation mash, cereal grain fermentation beer, and fermentation residues into a uniform material suitable for compositional analysis. This practice is intended for samples that need to be dried prior to 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 standard. The values given in parentheses after SI units are provided for information only and are not considered standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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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.  
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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.
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Standard Test Method for Determination of Carbohydrates in Biomass by High Performance Liquid Chromatography

SIGNIFICANCE AND USE
4.1 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 (%T ext)—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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Note 3 and Note 4.  
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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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
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