Beta Analytic Comment

FAA-2023-1169-0003_attachment_1.pdf

Inflation Reduction Act - Fueling Aviation's Sustainable Transition Grant Program

Beta Analytic Comment

OMB: 2120-0817

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US Federal Aviation Administration (FAA)
Inflation Reduction Act (IRA) FAST-SAF Grant Program
This comment specifically regards the use of the carbon-14 testing method to determine the share of
biogenic carbon content in sustainable aviation fuels (SAF) produced by co-processing. Biogenic
content measurements under methods such as ASTM D6866 and BS EN 16640 are currently used to
quantify the biogenic carbon content in a wide variety of biofuels.
Included here you will find:
About Beta Analytic

1

Recommendations for the FAST-SAF Grant Program

2

What is Biogenic Testing (Carbon-14)?

2

ASTM D6866 Method B - The Most Reliable Method

3

ISO/IEC 17025:2017 laboratory

4

Required tracer-free facility for Carbon-14

5

About Beta Analytic
Beta Analytic was among the originators of the ASTM D6866 biobased / biogenic testing standard using
carbon-14 to distinguish renewable carbon sources from petroleum sources in solids, liquids, and gasses.
Renewable testing started in 2003 at the request of United States Department of Agriculture (USDA)
representatives who were interested in Beta’s Carbon-14 capabilities for their USDA BioPreferredⓇ
Program (www.biopreferred.gov). Carbon-14 third party testing is now standardized in a wide range of
international standards including ASTM D6866, CEN 16137, EN 16640, ISO 16620, ISO 19984, BS EN ISO
21644:2021, ISO 13833 and EN 16785. Beta Analytic continues involvement in ASTM D6866 revisions
with the current president, Ron Hatfield, serving as technical advisor and committee member to both the
ASTM D20.96 and USDA BioPreferred Programs.
Carbon-14 standardized testing is also incorporated in a variety of regulatory programs including the
California AB32 program, US EPA GHG Protocol, US EPA Renewable Fuels Standard, United Nations
Carbon Development Mechanism, Western Climate Initiative, Climate Registry’s Greenhouse Gas
Reporting Protocol and EU Emissions Trading Scheme.

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Recommendations for the FAST-SAF Grant Program
Our recommendation is that the FAST-SAF grant program includes biogenic content testing requirements
following the ASTM D6866 standard for any SAFs produced by co-processing.
Co-processing is a widely used method which is currently among the most common paths for producing
many biofuels, including renewable diesel. While HEFA is currently the method used to produce most SAF
available on the market today, many co-processing facilities designed for renewable diesel production are
currently shifting to SAF. Co-processing facilities currently producing renewable diesel require very little
modification to produce SAF.1 Even further, the US EPA’s recently published Renewable Fuel Standard
volumes for 2023-2025 have been widely criticized by the US biofuels industry for planning for volumes
far below the true production capacity for renewable diesel specifically.2 That pressure, combined with
the quick growing demand for SAFs led by new and proposed regulations around the world, will likely
lead to even more renewable diesel co-processing facilities making the transition to SAF production.
It is critical that co-processed fuels be required to submit biogenic content testing because these fuels
are particularly difficult to estimate using mass balance calculations. Biogenic content testing
requirements would be in line with other similar regulations’ treatment of co-processed fuels, including
those which allow mass balance calculations for other fuels. For example co-processed SAF is required to
submit biogenic content testing for the US RFS, California LCFS, Oregon CFS, Canada CFR and the EU RED
II, though for most of these programs SAF is not yet a mandatory obligated product, but can apply for tax
credits.3 It is common best practice for programs such as those listed to mandate third-party testing for
all analysis they require in order to guarantee accurate, properly obtained results.
International certification programs which specialize in SAF, such as the Roundtable on Sustainable
Biomaterials (RSB)’s guide for compliance with the International Civil Aviation Organization (ICAO)’s
Carbon Offsetting and Reduction Scheme for International Aviation (CORSIA) program, require carbon-14
testing following ASTM D6866 or an equivalent standard for biogenic content measurements as well.
What is Biogenic Testing (Carbon-14)?
Carbon-14 analysis is a reliable method used to distinguish the percentage of biobased carbon content in
a given material. The radioactive isotope carbon-14 is present in all living organisms and recently expired
material, whereas any fossil-based material that is more than 50,000 years old does not contain any
1

2022. “The Role of Co-Processing in Aviation’s Transition to a Low-Carbon Future” Air bp
2023. “Biofuels Groups Disappointed with EPA RFS Final Rule” AgWeb
3
2010. “40 CFR Part 80 Subpart M– Renewable Fuel Standard.” National Archives Code of Federal Regulations
2018. “Directive 2018/2001 of the European Parliament and the Council.” Official Journal of the European Union
2020. “Reporting Co-Processing and Renewable Gasoline Emissions Under MRR.” California Air Resources Board
2022. “Quantification Method for Co-Processing in Refineries.” Government of Canada
2

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carbon-14 content. Since Carbon-14 is radioactive, the amount of carbon-14 present in a given sample
begins to gradually decay after the death of an organism until there is no carbon-14 left. Therefore, a
radiocarbon dating laboratory can use carbon-14 analysis to quantify the carbon-14 content present in a
sample, determining whether the sample is biomass-based, fossil fuel-derived, or a combination. This
result is measured using an Accelerator Mass Spectrometer (AMS) instrument.
The analysis is based on standards such as ASTM D6866, ISO 13833 and EN 16640. ASTM D6866 is an
international standard developed for measuring the biobased carbon content of solid, liquid, and gaseous
samples using radiocarbon dating. ISO 16620 is an international standard that measures the biobased
carbon content of plastic products, polymers, and additives.
Carbon-14 analysis yields a result reported as % biobased carbon content. If the result is 100% biobased
carbon, this indicates that the sample tested is completely sourced from biomass material such as plant
or animal byproducts. A result of 0% biobased carbon means a sample is only fossil fuel-derived. A
sample that is a mix of both biomass sources and fossil fuel sources will yield a result that ranges
between 0% and 100% biobased carbon content. Carbon-14 testing has been incorporated into several
regulations as the recommended or required method to quantify the biobased content of a given
material.
ASTM D6866 Method B - The Most Reliable Method
Carbon-14 is a very well-established method which has been in use by many industries (including the
fossil fuel industry) and academic researchers for several decades.
Carbon-14 measurements done by commercial third party testing is robust, consistent, and with
quantifiable accuracy/precision of the carbon-14 amount under ASTM D6866 method B. The EN 16785 is
the only standard that allows a variant of the Mass Balance (MB) method of ‘carbon counting’ under EN
16785-2. The EN 16785-1 requires that the biocarbon fraction be determined by the carbon-14 method.
However, when incorporating this EN 16785 method, certification schemes like the “Single European
Bio-based Content Certification” only allow the use of EN 16785-1 due to its reliability and the value of a
third-party certification. http://www.biobasedcontent.eu/en/about-us/
It is very important that testing be required to follow ASTM D6866 Method B in particular. ASTM
D6866 Method B uses Accelerated Mass Spectrometry (AMS), while Method C uses Liquid
Scintillation Counting (LSC). In Method B, the AMS machine directly measures the 14C isotopes.
However, in Method C, scintillation molecules indirectly absorb the beta molecules that release
with the decay of 14C and convert the energy into photons which are measured proportionally to
the amount of 14C in the sample. Since Method B directly measures the 14C isotopes and Method
C measures them indirectly, Method B is significantly more precise and should be prioritized in

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regulations.4 LSC calculations, like those used in Method C, are commonly used as an internal
testing tool when samples are limited and accuracy does not need to be extremely high.
In ASTM D6866 method B, the carbon-14 result is provided as a single numerical result of carbon-14
activity, with graphical representation that is easily understood by regulators, policy makers, corporate
officers, and more importantly, the public. The overwhelming advantage of carbon-14 is that it is an
independent and standardized laboratory measurement of any carbon containing substance that
produces highly accurate and precise values. In that regard, it can stand alone as a quantitative indicator
of the presence of renewable vs. petroleum feedstocks. When carbon-14 test results are challenged,
samples can be rapidly remeasured to verify the original reported values (unlike mass balance).
Also of significant importance is that carbon-14 measurements are strictly third party generated under
ISO/IEC 17025:2017 Testing Accreditation with no contribution from the submitter, client, or
manufacturer.
Most international standards do not cite error limitations, however, the ASTM-D6866 method B
standard says that, “Instrumental error can be within 0.1-0.5 % (1 relative standard deviation (RSD),
but controlled studies identify an inter-laboratory total uncertainty up to +/- 3 % (absolute). This
error is exclusive of indeterminate sources of error in the origin of the biobased content.”5 This has
been applied across all industries and establishes a high degree of variability in indeterminate errors
likely to exist between different manufacturing processes. This approximation is well understood as
are any errors associated with the measurement.
ISO/IEC 17025:2017 Accredited Laboratory
To ensure the highest level of quality, laboratories performing ASTM D6866 testing should be ISO/IEC
17025:2017 accredited or higher. This accreditation is unbiased, third party awarded and supervised. It is
unique to laboratories that not only have a quality management program conformant to the ISO
9001:2008 standard, but more importantly, have demonstrated to an outside third-party laboratory
accreditation body that Beta Analytic has the technical competency necessary to consistently deliver
technically valid test results. The ISO 17025 accreditation is specifically for natural level radiocarbon
activity measurements including biobased analysis of consumer products and fuels, and for radiocarbon
dating.

4

2022. Testing the methods for determination of radiocarbon content in liquid fuels in the Gliwice Radiocarbon and Mass Spectrometry
Laboratory. Radiocarbon, 64(6), pp.1-10.
5
2021. Standard Test Methods for Determining the Biobased Content of Solid, Liquid, and Gaseous Samples Using Radiocarbon Analysis. ASTM
International (D6866-21). pp 1-19. doi: 10.1520/D6866-21.

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Required tracer-free facility for Carbon-14
For carbon-14 measurement to work, be accurate, and repeatable, the facility needs to be a tracer-free
facility, which means artificial/labeled carbon-14 is not and has never been handled in that lab. Facilities
that handle artificial carbon-14 use enormous levels relative to natural levels and it becomes ubiquitous
in the facility and cross contamination within the facility, equipment and chemistry lines is unavoidable.
Results from a facility that handles artificial carbon-14 would show elevated renewable contents (higher
pMC, % Biobased / Biogenic values), making those results invalid. Because of this, Federal contracts and
agency programs (such as the USDA BioPreferred Program) require that AMS laboratories must be 14C
tracer-free facilities in order to be considered for participation in solicitations.
To learn more about the risks associated with testing natural levels Carbon-14 samples in a facility
handling artificially enhanced isotopes please see the additional information provided after this
comment.

References
2010. “40 CFR Part 80 Subpart M– Renewable Fuel Standard.” National Archives Code of Federal Regulations
https://www.ecfr.gov/current/title-40/chapter-I/subchapter-C/part-80/subpart-M
2018. “Directive 2018/2001 of the European Parliament and the Council.” Official Journal of the European Union
https://eur-lex.europa.eu/legal-content/EN/TXT/HTML/?uri=CELEX:32018L2001
2020. “Reporting Co-Processing and Renewable Gasoline Emissions Under MRR.” California Air Resources Board
https://ww2.arb.ca.gov/sites/default/files/2020-09/MRR_coprocessing-slides_Sept_2020.pdf
2021. “Standard Test Methods for Determining the Biobased Content of Solid, Liquid, and Gaseous Samples Using
Radiocarbon Analysis.” ASTM International (D6866-21). pp 1-19. DOI: 10.1520/D6866-21.
2022.
“Quantification
Method
for
Co-Processing
in
Refineries.”
Government
of
Canada
https://www.canada.ca/en/environment-climate-change/services/managing-pollution/energy-production/fuel-regulati
ons/clean-fuel-regulations/compliance/quantification-methodco-processing-refineries.html
2022. “The Role of Co-Processing in Aviation’s Transition to a Low-Carbon Future” Air bp
https://www.bp.com/en/global/air-bp/news-and-views/views/the-role-of-co-processing-in-aviation-s-transition-to-a-l
ow-carb.html
2022. Testing the methods for determination of radiocarbon content in liquid fuels in the Gliwice Radiocarbon and
Mass Spectrometry Laboratory. Radiocarbon, 64(6), pp.1-10. DOI: 10.1017/RDC.2022.35
2023. “Biofuels Groups Disappointed with EPA RFS Final Rule” AgWeb
https://www.agweb.com/news/policy/politics/biofuels-groups-disappointed-epas-rfs-final-rule-volumes-dont-match-c
urrent

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Demand a Tracer-Free Laboratory
for Radiocarbon Dating
As part of its commitment to provide high-quality results to its clients, ISO/IEC
17025-accredited Beta Analytic does not accept pharmaceutical samples with
“tracer Carbon-14” or any other material containing artificial Carbon-14 (14C) to
eliminate the risk of cross-contamination. Moreover, the lab does not engage in
“satellite dating” – the practice of preparing individual sample graphite in a remote
chemistry lab and then subcontracting an AMS facility for the result.

High Risk of Cross-Contamination

Avoid the Risks

Pharmaceutical companies evaluate drug metabolism
by using a radiolabeled version of the drug under
investigation. AMS biomedical laboratories use 14C
as a tracer because it can easily substitute 12C atoms
in the drug molecule, and it is relatively safe to
handle. Tracer 14C is a well-known transmittable
contaminant to radiocarbon samples, both within the
AMS equipment and within the chemistry lab.

Find out from the lab that you are planning to use that
they have never in the past and will never in the
future:

Since the artificial 14C used in these studies is
phenomenally high (enormous) relative to natural
levels, once used in an AMS laboratory it becomes
ubiquitous. Cross-contamination within the AMS and
the chemistry lines cannot be avoided. Although the
levels of contamination are acceptable in a biomedical
AMS facility, it is not acceptable in a radiocarbon
dating facility.
Biomedical AMS facilities routinely measure
tracer-level, labeled (Hot) 14C samples that are
hundreds to tens of thousands of times above the
natural 14C levels found in archaeological, geological,
and hydrological samples. Because the 14C content
from the biomedical samples is so high, even sharing
personnel will pose a contamination risk; “Persons
from hot labs should not enter the natural labs and
vice versa” (Zermeño et al. 2004, pg. 294). These two
operations should be absolutely separate. Sharing
personnel, machines, or chemistry lines run the risk of
contaminating natural level 14C archaeological,
geological, and hydrological samples.

- accept, handle, graphitize or AMS count samples
containing Tracer or Labeled (Hot) 14C.
- share any laboratory space, equipment, or
personnel with anyone preparing (pretreating,
combusting, acidifying, or graphitizing) samples that
contain Tracer or Labeled (Hot) 14C.
- use AMS Counting Systems (including any and all
beam-line components) for the measurement of
samples that contain Tracer or Labeled (Hot) 14C.

Tracer-Free Lab Required
Recently, federal contracts are beginning to specify
that AMS laboratories must be 14C tracer-free
facilities in order to be considered for participation in
solicitations.
A solicitation for the National Oceanic and
Atmospheric Administration (NOAA) has indicated
that “the AMS Facility utilized by the Contractor for
the analysis of the micro-samples specified must be a
14C tracer-level-free facility.” (Solicitation Number:
WE-133F-14-RQ-0827 - Agency: Department of
Commerce)
As a natural level radiocarbon laboratory, we highly
recommend that researchers require the AMS lab
processing their samples to be Tracer-free.

No Exposure to Artificial Carbon-14

Useful Reference

According to ASTM International, the ASTM D6866
standard is applicable to laboratories working without
exposure to artificial carbon-14 routinely used in biomedical studies. Artificial carbon-14 can exist within the
laboratory at levels 1,000 times or more than 100 %
biobased materials and 100,000 times more than 1%
biobased materials. Once in the laboratory, artificial 14C
can become undetectably ubiquitous on materials and
other surfaces but which may randomly contaminate an
unknown sample producing inaccurately high biobased
results. Despite vigorous attempts to clean up contaminating artificial 14C from a laboratory, isolation has
proven to be the only successful method of avoidance.
Completely separate chemical laboratories and extreme
measures for detection validation are required from
laboratories exposed to artificial 14C. Accepted requirements are:

1. Memory effects in an AMS system: Catastrophe
and Recovery. J. S. Vogel, J.R. Southon, D.E.
Nelson. Radiocarbon, Vol 32, No. 1, 1990, p. 81-83
doi:10.2458/azu_js_rc.32.1252 (Open Access)

(1) disclosure to clients that the laboratory working with
their products and materials also works with artificial 14C
(2) chemical laboratories in separate buildings for the
handling of artificial 14C and biobased samples
(3) separate personnel who do not enter the buildings of
the other
(4) no sharing of common areas such as lunch rooms and
offices
(5) no sharing of supplies or chemicals between the two
(6) quasi-simultaneous quality assurance measurements
within the detector validating the absence of contamination within the detector itself.
ASTM D6866-22 – Standard Test Methods for Determining the Biobased Content of Solid, Liquid, and Gaseous
Samples Using Radiocarbon Analysis.

“... we certainly do not advocate processing both
labeled and natural samples in the same chemical
laboratory.” “The long term consequences are
likely to be disastrous.”
2. Recovery from tracer contamination in AMS
sample preparation. A. J. T. Jull, D. J. Donahue, L.
J. Toolin. Radiocarbon, Vol. 32, No.1, 1990, p.
84-85 doi:10.2458/azu_js_rc.32.1253 (Open
Access)
“... tracer 14C should not be allowed in a
radiocarbon laboratory.” “Despite vigorous recent
efforts to clean up the room, the “blanks” we
measured had 14C contents equivalent to modern
or even post ‐bomb levels.”
3. Prevention and removal of elevated radiocarbon
contamination in the LLNL/CAMS natural
radiocarbon sample preparation laboratory.
Zermeño, et. al. Nuclear Instruments and Methods
in Physics Research Section B: Beam Interactions
with Materials and Atoms
Vol. 223-224, 2004, p. 293-297
doi: 10.1016/j.nimb.2004.04.058
“The presence of elevated 14C contamination in a
laboratory preparing samples for natural
radiocarbon analysis is detrimental to the
laboratory workspace as well as the research
being conducted.”
4. High level 14C contamination and recovery at
XIʼAN AMS center. Zhou, et. al. Radiocarbon, Vol
54, No. 2, 2012, p. 187-193
doi:10.2458/azu_js_rc.54.16045
“Samples that contain high concentrations of
radiocarbon (“hot” samples) are a catastrophe for
low background AMS laboratories.” “In our case
the ion source system was seriously contaminated,
as were the preparation lines.”

www.radiocarbon.com


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