ASTM E3146-18a
(Test Method)Standard Test Method for Determination of Carbonyls in Pyrolysis Bio-Oils by Potentiometric Titration
Standard Test Method for Determination of Carbonyls in Pyrolysis Bio-Oils by Potentiometric Titration
SIGNIFICANCE AND USE
5.1 While pyrolysis bio-oils are comprised of a large variety of compounds and chemical functional groups, quantification of carbonyl groups is especially important. Carbonyls are known to be responsible for the instability of bio-oil during both storage and processing. This method can be used to quantify the total carbonyl content of bio-oils.
SCOPE
1.1 This test method covers the determination of the carbonyl content of bio-oils derived from thermochemical decomposition of lignocellulosic biomass and their deoxygenated products. This method is used for determination of carbonyls between 0.5 and 8 mol/kg.
1.2 Review the current and appropriate Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid procedures, and safety precautions and proper personal protective equipment.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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.
1.5 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.
General Information
Relations
Buy Standard
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E3146 − 18a
Standard Test Method for
Determination of Carbonyls in Pyrolysis Bio-Oils by
1
Potentiometric Titration
This standard is issued under the fixed designation E3146; 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 2.2 Other Standards
CEN/TR 17103:2017 Petroleum and related products - Fast
1.1 This test method covers the determination of the carbo-
pyrolysis bio-oils for stationary internal combustion en-
nyl content of bio-oils derived from thermochemical decom-
2
gines - quality determination
position of lignocellulosic biomass and their deoxygenated
EN 16900:2017 Fast Pyrolysis bio-oils for industrial
products. This method is used for determination of carbonyls
3
boilers—Requirement and test methods
between 0.5 and 8 mol/kg.
1.2 Review the current and appropriate Safety Data Sheets 3. Terminology
(SDS) for detailed information concerning toxicity, first aid
3.1 Definitions:
procedures, and safety precautions and proper personal protec-
3.1.1 Bio-Oil, n—The crude liquid product of converting
tive equipment.
solid biomass into a liquid via fast pyrolysis or other thermo-
chemical conversion process.
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 3.1.2 Carbonyl, n—The chemical functional group consist-
standard.
ing of a carbon-oxygen double bond, C=O. For this method,
this includes all aldehydes and ketones; carboxylic acids,
1.4 This standard does not purport to address all of the
esters, and lactone groups are not measured by this method.
safety concerns, if any, associated with its use. It is the
3.1.3 fast pyrolysis, n—Pyrolysis conducted with rapid heat-
responsibility of the user of this standard to establish appro-
ing and short residence time; typically less than 10 seconds.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
3.1.3.1 Discussion—– Other definitions for fast pyrolysis
4
1.5 This international standard was developed in accor-
state residence times of typically less than 10 seconds (1), 5
dance with internationally recognized principles on standard-
seconds(CENstandards,EN16900:2017),and1second (2, 3).
ization established in the Decision on Principles for the
3.1.4 pyrolysis, n—Chemical decomposition of organic ma-
Development of International Standards, Guides and Recom-
terials by heating in the absence of oxygen.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
4. Summary of Test Method
4.1 A bio-oil sample is dissolved in dimethylsulfoxide
2. Referenced Documents
(DMSO) and solutions are added containing hydroxylamine
2.1 ASTM Standards: hydrochloride (NH OH·HCl) and triethanolamine (TEA). The
2
D664 Test Method for Acid Number of Petroleum Products mixture is sealed, stirred, and heated to 80 °C for 2 hours.
by Potentiometric Titration Carbonyl compounds (aldehydes and ketones) react with
D1193 Specification for Reagent Water NH OH·HCl forming the corresponding oxime and liberating
2
D6299 Practice for Applying Statistical Quality Assurance HCl. Liberated HCl is consumed by TEA, which drives the
and Control Charting Techniques to Evaluate Analytical reaction forward. After the reaction, unconsumed TEA is
Measurement System Performance
titrated with a standardized HCl titrant to determine the molar
concentration of carbonyls in the sample.
1
This test method is under the jurisdiction of ASTM Committee E48 on
2
Bioenergy and Industrial Chemicals from Biomass and is the direct responsibility of Available from European Committee for Standardization (CEN), Avenue
Subcommittee E48.05 on Biomass Conversion. Marnix 17, B-1000, Brussels, Belgium, http://www.cen.eu.
3
Current edition approved June 1, 2018. Published January 2018. Originally Available from British Standards Institution (BSI), 389 Chiswick High Rd.,
approved in 2018. Last previous edition approved in 2018 as E3146–18. DOI: London W4 4AL, U.K., http://www.bsigroup.com.
10.1520/E3146–18A.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E3146 − 18a
5. Significance and Use
5.1 While pyrolysis bio-oils are comprised of a large variety
of compounds and chemical functional groups, quantification
of carbonyl groups is especially important. Carbonyls are
known to be responsible for the instability of bio-oil during
both storage and processing. This method can be used to
quantify the total ca
...
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: E3146 − 18 E3146 − 18a
Standard Test Method for
Determination of Carbonyls in Pyrolysis Bio-Oils by
1
Potentiometric Titration
This standard is issued under the fixed designation E3146; 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 the carbonyl content of bio-oils derived from thermochemical decomposition
of lignocellulosic biomass and their deoxygenated products. This method is used for determination of carbonyls between 0.5 and
8 mol/kg.
1.2 Review the current and appropriate Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid
procedures, and safety precautions and proper personal protective equipment.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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.
1.5 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.
2. Referenced Documents
2.1 ASTM Standards:
D664 Test Method for Acid Number of Petroleum Products by Potentiometric Titration
D1193 Specification for Reagent Water
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
2.2 Other Standards
CEN/TR 17103:2017 Petroleum and related products - Fast pyrolysis bio-oils for stationary internal combustion engines -
2
quality determination
3
EN 16900:2017 Fast Pyrolysis bio-oils for industrial boilers—Requirement and test methods
3. Terminology
3.1 Definitions:
3.1.1 Bio-Oil, n—The crude liquid product of converting solid biomass into a liquid via fast pyrolysis or other thermochemical
conversion process.
3.1.2 Carbonyl, n—The chemical functional group consisting of a carbon-oxygen double bond, C=O. For this method, this
includes all aldehydes and ketones; carboxylic acids, esters, and lactone groups are not measured by this method.
3.1.3 fast pyrolysis, n—Pyrolysis conducted with rapid heating and short reaction time; within approximately 2 residence time;
typically less than 10 seconds.
3.1.3.1 Discussion—
1
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 Jan. 1, 2018June 1, 2018. Published January 2018. Originally approved in 2018. Last previous edition approved in 2018 as E3146–18. DOI:
10.1520/E3146–18.10.1520/E3146–18A.
2
Available from European Committee for Standardization (CEN), Avenue Marnix 17, B-1000, Brussels, Belgium, http://www.cen.eu.
3
Available from British Standards Institution (BSI), 389 Chiswick High Rd., London W4 4AL, U.K., http://www.bsigroup.com.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E3146 − 18a
4
– Other definitions for fast pyrolysis state residence times of typically less than 10 seconds (1), 5 seconds (CEN standards, EN
16900:2017), and 1 second (2, 3).
3.1.4 pyrolysis, n—Chemical decomposition of organic materials by heating in the absence of oxygen.
4. Summary of Test Method
4.1 A bio-oil sample is dissolved in dimethylsulfoxide (DMSO) and solutions are added containing hydroxylamine
hydrochloride (NH OH·HCl) and triethanolamine (TEA). The mixture is sealed, stirred, and heated to 80 °C for 2 hours. Carbonyl
2
compounds (aldehydes and ketones) react with NH OH·HCl forming the corresponding oxime and liberating HCl. Liberated HCl
2
is consumed by TEA, which drives the reaction forward. After the reaction, unconsumed TEA is titrated with a standardized HCl
titrant to determine the molar concentration of carbonyls in the sample.
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.