ASTM D6866-10
(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 A utilizes Liquid Scintillation Counting (LSC) radiocarbon (14C) techniques to quantify the biobased content of a given product with maximum total error of 15 % count, which is associated with sample preparation and actual counting. This test method is based on LSC analysis of CO2 cocktails after collecting the CO2 in a suitable absorbing solution.
Method B utilizes Accelerator Mass Spectrometry (AMS) and Isotope Ratio Mass Spectrometry (IRMS) techniques to quantify the biobased content of a given product with possible uncertainties of 1 to 2 % and 0.1 to 0.5 %, respectively. Sample preparation methods are identical to Method A, 8.2–8.5. Method B diverges after 8.5 and rather than LSC analysis the sample CO2 remains within the vacuum manifold and is distilled, quantified in a calibrated volume, transferred to a quartz tube, torch sealed. Details are given in 12.7-12.10. 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. However, whereas Method A uses LSC analysis of CO2 cocktails, Method C uses LSC analysis of sample carbon that has been converted to benzene....
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:D6866–10
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 informationregardingthepracticeoftheartofisotopeanalysis
and to facilitate performance of these test methods.
1.1 These test methods do not address environmental im-
3.2 Terminology D883 should be referenced for terminol-
pact, product performance and functionality, determination of
ogy relating to plastics. Although an attempt to list terms in a
geographical origin, or assignment of required amounts of
logical manner (alphabetically) will be made as some terms
biobased carbon necessary for compliance with federal laws.
require definition of other terms to make sense.
1.2 These test methods are applicable to any product con-
3.3 Definitions:
tainingcarbon-basedcomponentsthatcanbecombustedinthe
3.3.1 dpm—disintegrations per minute. This is the quantity
presence of oxygen to produce carbon dioxide (CO ) gas. The
2
of radioactivity. The measure dpm is derived from cpm or
overall analytical method is also applicable to gaseous
counts per minute (dpm = cpm − bkgd / counting efficiency).
samples, including flue gases from electrical utility boilers and
6
3
There are 2.2 by 10 dpm / uCi (14,17).
waste incinerators.
3.3.2 dps—disintegrationspersecond(ratherthanminuteas
1.3 These test methods make no attempt to teach the basic
above) (14,17).
principles of the instrumentation used although minimum
3.3.3 scintillation—the sum of all photons produced by a
requirements for instrument selection are referenced in the
radioactive decay event. Counters used to measure this as
References section. However, the preparation of samples for
described in these test methods are Liquid Scintillation
the above test methods is described. No details of instrument
Counters (LSC) (14,17).
operation are included here. These are best obtained from the
3.3.4 specific activity (SA)—refers to the quantity of radio-
manufacturer of the specific instrument in use.
activitypermassunitofproduct,thatis,dpmpergram(14,17).
1.4 Currently, there are no ISO test methods that are
3.3.5 automated effıciency control (AEC)—a method used
equivalent to the test methods outlined in this standard.
by scintillation counters to compensate for the effect of
1.5 This standard does not purport to address all of the
quenching on the sample spectrum (14).
safety concerns, if any, associated with its use. It is the
3.3.6 AMS facility—a facility performingAccelerator Mass
responsibility of the user of this standard to establish appro-
Spectrometry.
priate safety and health practices and determine the applica-
3.3.7 accelerator mass spectrometry (AMS)—an ultra-
bility of regulatory limitations prior to use.
sensitive technique that can be used for measuring naturally
2. Referenced Documents occurring radio nuclides, in which sample atoms are ionized,
2
accelerated to high energies, separated on basis of momentum,
2.1 ASTM Standards:
charge, and mass, and individually counted in Faraday collec-
D883 Terminology Relating to Plastics
tors. This high energy separation is extremely effective in
3. Terminology
filteringoutisobaricinterferences,suchthatAMSmaybeused
14 12
to measure accurately the C/ C abundance to a level of 1 in
3.1 The definitions of terms used in these test methods are
15
10 . At these levels, uncertainties are based on counting
referenced in order that the practitioner may require further
statistics through the Poisson distribution (8,9).
3.3.8 background radiation—the radiation in the natural
1
These test methods are under the jurisdiction of ASTM Committee D20 on
environment; including cosmic radiation and radionuclides
Plastics and are the direct responsibility of Subcommittee D20.96 on Environmen-
present in the local environment, for example, materials of
tally Degradable Plastics and Biobased Products.
CurrenteditionapprovedJuly1,2010.PublishedJuly2010.Originallyapproved construction, metals, glass, concrete (2,4,7,8,14-19).
in 2004. Last previous edition approved in 2008 as D6866-08. DOI: 10.1520/
D6866-10.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Bo
...
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:D6866–08 Designation:D6866–10
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 approved Aug.July 1, 2008.2010. Published September 2008.July 2010. Originally approved in 2004. Last previous edition approved in 20062008 as
D6866-06a.D6866-08. DOI: 10.1520/D6866-108.
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.
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...
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