ASTM D6866-12
(Test Method)Standard Test Methods for Determining the Biobased Content of Solid, Liquid, and Gaseous Samples Using Radiocarbon Analysis
Standard Test Methods for Determining the Biobased Content of Solid, Liquid, and Gaseous Samples Using Radiocarbon Analysis
SIGNIFICANCE AND USE
Presidential (Executive) Orders 13101, 13123, 13134, Public Laws (106-224), AG ACT 2003 and other Legislative Actions all require Federal Agencies to develop procedures to identify, encourage and produce products derived from biobased, renewable, sustainable and low environmental impact resources so as to promote the Market Development Infrastructure necessary to induce greater use of such resources in commercial, non food, products. Section 1501 of the Energy Policy Act of 2005 (Public Law 109–58) and EPA 40 CFR Part 80 (Regulation of Fuels and Fuel Additives: Renewable Fuel Standard Requirements for 2006) require petroleum distributors to add renewable ethanol to domestically sold gasoline to promote the nation's growing renewable economy, with requirements to identify and trace origin.
Method B utilizes Accelerator Mass Spectrometry (AMS) along with Isotope Ratio Mass Spectrometry (IRMS) techniques to quantify the biobased content of a given product. Intsrumental error can be within 0.1-0.5 % (1 rsd), but empirical studies identify a total uncertainty up to ±3 % (absolute) inclusive of indeterminant sources of error in the final biobased content result. Sample preparation methods include the production of CO2 within a vacuum manifold system where it is ultimately distilled, quantified in a calibrated volume, transferred to a quartz tube, and torch sealed. Details are given in 8.7-8.10. The stored CO2 is then delivered to an AMS facility for final processing and analysis.
Method C uses LSC techniques to quantify the biobased content of a product using sample carbon that has been converted to benzene. This test method determines the biobased content of a sample with a maximum total error of ±3 % (absolute), as does Method B.
The test methods described here directly discriminate between product carbon resulting from contemporary carbon input and that derived from fossil-based input. A measurement of a product’s 14C/12C content is determined relative to the mod...
SCOPE
1.1 These test methods do not address environmental impact, product performance and functionality, determination of geographical origin, or assignment of required amounts of biobased carbon necessary for compliance with federal laws.
1.2 These test methods are applicable to any product containing carbon-based components that can be combusted in the presence of oxygen to produce carbon dioxide (CO2) gas. The overall analytical method is also applicable to gaseous samples, including flue gases from electrical utility boilers and waste incinerators.
1.3 These test methods make no attempt to teach the basic principles of the instrumentation used although minimum requirements for instrument selection are referenced in the References section. However, the preparation of samples for the above test methods is described. No details of instrument operation are included here. These are best obtained from the manufacturer of the specific instrument in use.
1.4 Currently, there are no ISO test methods that are equivalent to the test methods outlined in this 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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D6866 − 12
StandardTest Methods for
Determining the Biobased Content of Solid, Liquid, and
1
Gaseous Samples Using Radiocarbon Analysis
This standard is issued under the fixed designation D6866; 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* informationregardingthepracticeoftheartofisotopeanalysis
and to facilitate performance of these test methods.
1.1 These test methods do not address environmental
impact, product performance and functionality, determination
3.2 Terminology D883 should be referenced for terminol-
of geographical origin, or assignment of required amounts of
ogy relating to plastics. Although an attempt to list terms in a
biobased carbon necessary for compliance with federal laws.
logical manner (alphabetically) will be made as some terms
require definition of other terms to make sense.
1.2 These test methods are applicable to any product con-
taining carbon-based components that can be combusted in the
3.3 Definitions:
presence of oxygen to produce carbon dioxide (CO ) gas. The
2 3.3.1 dpm—disintegrations per minute. This is the quantity
overall analytical method is also applicable to gaseous
of radioactivity. The measure dpm is derived from cpm or
samples, including flue gases from electrical utility boilers and
counts per minute (dpm = cpm − bkgd / counting efficiency).
6 3
waste incinerators.
There are 2.2 by 10 dpm / uCi (14,17).
1.3 These test methods make no attempt to teach the basic
3.3.2 dps—disintegrationspersecond(ratherthanminuteas
principles of the instrumentation used although minimum
above) (14,17).
requirements for instrument selection are referenced in the
3.3.3 scintillation—the sum of all photons produced by a
References section. However, the preparation of samples for
radioactive decay event. Counters used to measure this as
the above test methods is described. No details of instrument
described in these test methods are Liquid Scintillation Coun-
operation are included here. These are best obtained from the
ters (LSC) (14,17).
manufacturer of the specific instrument in use.
3.3.4 specific activity (SA)—refers to the quantity of radio-
1.4 Currently, there are no ISO test methods that are
activitypermassunitofproduct,thatis,dpmpergram (14,17).
equivalent to the test methods outlined in this standard.
3.3.5 automated effıciency control (AEC)—a method used
1.5 This standard does not purport to address all of the
by scintillation counters to compensate for the effect of
safety concerns, if any, associated with its use. It is the
quenching on the sample spectrum (14).
responsibility of the user of this standard to establish appro-
3.3.6 AMS facility—a facility performing Accelerator Mass
priate safety and health practices and determine the applica-
Spectrometry.
bility of regulatory limitations prior to use.
3.3.7 accelerator mass spectrometry (AMS)—an ultra-
2. Referenced Documents
sensitive technique that can be used for measuring naturally
2
2.1 ASTM Standards:
occurring radio nuclides, in which sample atoms are ionized,
D883Terminology Relating to Plastics
accelerated to high energies, separated on basis of momentum,
charge, and mass, and individually counted in Faraday collec-
3. Terminology
tors. This high energy separation is extremely effective in
3.1 The definitions of terms used in these test methods are
filteringoutisobaricinterferences,suchthatAMSmaybeused
referenced in order that the practitioner may require further
14 12
to measure accurately the C/ C abundance to a level of 1 in
15
10 . At these levels, uncertainties are based on counting
1
These test methods are under the jurisdiction of ASTM Committee D20 on
statistics through the Poisson distribution (8,9).
Plastics and are the direct responsibility of Subcommittee D20.96 on Environmen-
tally Degradable Plastics and Biobased Products.
3.3.8 background radiation—the radiation in the natural
Current edition approved April 1, 2012. Published May 2012. Originally
environment; including cosmic radiation and radionuclides
approved in 2004. Last previous edition approved in 2011 as D6866-11. DOI:
10.1520/D6866-12.
2
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
3
Standards volume information, refer to the standard’s Document Summary page on Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof
the ASTM website. this standard.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, P
...
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:D6866–11 Designation:D6866–12
Standard Test Methods for
Determining the Biobased Content of Solid, Liquid, and
1
Gaseous Samples Using Radiocarbon Analysis
This standard is issued under the fixed designation D6866; 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*
1.1 These test methods do not address environmental impact, product performance and functionality, determination of
geographical origin, or assignment of required amounts of biobased carbon necessary for compliance with federal laws.
1.2 These test methods are applicable to any product containing carbon-based components that can be combusted in the
presence of oxygen to produce carbon dioxide (CO ) gas. The overall analytical method is also applicable to gaseous samples,
2
including flue gases from electrical utility boilers and waste incinerators.
1.3 These test methods make no attempt to teach the basic principles of the instrumentation used although minimum
requirements for instrument selection are referenced in the References section. However, the preparation of samples for the above
test methods is described. No details of instrument operation are included here. These are best obtained from the manufacturer of
the specific instrument in use.
1.4 Currently, there are no ISO test methods that are equivalent to the test methods outlined in this 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
3. Terminology
3.1 The definitions of terms used in these test methods are referenced in order that the practitioner may require further
information regarding the practice of the art of isotope analysis and to facilitate performance of these test methods.
3.2 Terminology D883 should be referenced for terminology relating to plastics.Although an attempt to list terms in a logical
manner (alphabetically) will be made as some terms require definition of other terms to make sense.
3.3 Definitions:
3.3.1 dpm—disintegrations per minute. This is the quantity of radioactivity. The measure dpm is derived from cpm or counts
6
3
per minute (dpm = cpm − bkgd / counting efficiency). There are 2.2 by 10 dpm / uCi (14,17).
3.3.2 dps—disintegrations per second (rather than minute as above) (14,17).
3.3.3 scintillation—the sum of all photons produced by a radioactive decay event. Counters used to measure this as described
in these test methods are Liquid Scintillation Counters (LSC) (14,17).
3.3.4 specific activity (SA)—refers to the quantity of radioactivity per mass unit of product, that is, dpm per gram (14,17).
3.3.5 automated effıciency control (AEC)—a method used by scintillation counters to compensate for the effect of quenching
on the sample spectrum (14).
3.3.6 AMS facility—a facility performing Accelerator Mass Spectrometry.
3.3.7 accelerator mass spectrometry (AMS)—an ultra-sensitive technique that can be used for measuring naturally occurring
radio nuclides, in which sample atoms are ionized, accelerated to high energies, separated on basis of momentum, charge, and
mass, and individually counted in Faraday collectors. This high energy separation is extremely effective in filtering out isobaric
14 12 15
interferences, such thatAMS may be used to measure accurately the C/ C abundance to a level of 1 in 10 .At these levels,
1
These test methods are under the jurisdiction of ASTM Committee D20 on Plastics and are the direct responsibility of Subcommittee D20.96 on Environmentally
Degradable Plastics and Biobased Products.
Current edition approvedApril 1, 2011.2012. PublishedApril 2011.May 2012. Originally approved in 2004. Last previous edition approved in 20102011 as D6866-101.
DOI: 10.1520/D6866-112.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
The boldface numbers in parentheses refer to the list of references at the end of this standard.
*A Summary of Changes sect
...
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